Interface Vol. 30, No. 1, Spring 2021 by The Electrochemical Society

VOL. 30, NO. 1, S p r i n g 2 0 2 1

Solid State Aspects of Energy Conversion

8 26

2020 Year in Review

Free Radicals: Winner Takes All

239th ECS Meeting Highlights

A Vision for Sustainable Energy

Future eCS MeetingS 239th eCS Meeting with the 18th international Meeting on Chemical Sensors DIGITAL MEETING May 30-June 3, 2021

240th eCS Meeting OrLANDO, FL October 10-14, 2021

Orange County Convention Center

241st eCS Meeting VANcOuVEr, Bc May 29-June 2, 2022

Vancouver Convention Center

242nd eCS Meeting ATLANTA, GA Oct. 9-13, 2022 Atlanta Hilton

2021 2021 2022 2022

www.electrochem.org/meetings

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

FROM THE EDITOR

The New Leisure Class

oon after I started as a faculty member in 1990, there was an opinion article in The Wall Street Journal. It described faculty members (at least in the U.S.) as the “New Leisure Class,” riffing off the book by Thorstein Veblen in which he coined the term conspicuous consumption. This topic has been revisited many times since, with statistics on the number of hours the average faculty member has contact with students in class and office hours used as evidence of a pretty cushy existence. The fact that the scholarly productivity of some is weak, to say the least, is often alluded to as well. The irony that the op-eds are often authored by employees of free-market think tanks has not been lost on me. Every time such assessments appear and are linked to the high cost of college education, I have to admit that they get under my skin. Every time I am told (often by in-laws for some reason) how nice it must be to have the summers off, I explain through slightly gritted teeth that if I actually took my summers off, my paycheck would do the same. It is tempting to offer a full-throated defense of my chosen profession, citing the long hours worked and important contributions that many of my colleagues make. Being a contrarian, I will instead describe why I think it is the best job on earth (spoiler alert: it is not because of the low workload). Possibly supporting the talking points of the critics, I can attest that I have never worked a day in my adult life. I can also say that I often work my rear end off. (Although it apparently regenerates like a salamander tail.) Being a faculty member means having the best job and the worst boss. The job is great because it involves interacting with some of the smartest people— students, staff, and other faculty—in the pursuit of (a) a better understanding of our natural world, (b) creation of means to improve the human condition, and (c) guiding the development of the next generation of leaders—both technical and otherwise. I have been lucky to have my best friends as my colleagues, so going to work (when allowed to do so) is more like a playdate. My students become family, and I have as much joy in having a front seat at their development as I do with my actual kids. The boss is a jerk because you are the boss. Teaching in class reminds me of why I love science. It also requires me to learn what I thought I already knew because you realize how little you know about a subject when it comes time to teach it to very bright people who tend to ask very good questions. Standing in front of a class with a dumb look on your face is not great fun (something for which I have a lot of personally collected empirical evidence). So you dig into the topic both out of a desire to avoid embarrassment and hope to help the students see the beauty as you do. The job requirement that one provides service to the technical community allows you to pay back what those before you provided, such as opportunities to present your work at conferences and in journals that will be read by many for years to come. Some even get to spout off four times a year in editorials. So, is being a faculty member all mai tais and shuffleboard? Well, not really. It is one of those jobs in which you feel you are always on. You are essentially a small business owner in a research park (your department). Students have truly urgent needs that arise well outside normal working hours that need immediate attention. Sponsors seem to wait until your busiest time to reach out with their own needs. Here the Golden Rule applies—he who has the gold makes the rules. As a friend of mine once said, every request of a faculty member’s time is reasonable—there is just an infinite number of them. Most of us are terrible at saying no, so we get overloaded, then complain to our friends and family about the unfairness of it all. Showing saint-like restraint, they commiserate. All that said, being a professor is like being a kid in a candy store. You decide what research topics interest you. You have captive audiences several times a week, so you get to enjoy the sound of your own voice. You decide how best to serve. It sure beats working for a living. Until next time, be safe and happy.

Rob Kelly Editor rgk6y@virginia.edu https://orcid.org/0000-0002-7354-0978

Published by: The Electrochemical Society (ECS) 65 South Main Street Pennington, NJ 08534-2839, USA Tel 609.737.1902, Fax 609.737.2743 www.electrochem.org Editor: Rob Kelly, rgk6y@virginia.edu Guest Editor: Paul A. Maggard, paul_maggard@ncsu.edu Contributing Editors: Donald Pile, Donald.Pile@gmail. com; Alice Suroviec, asuroviec@berry.edu Production Editor: Mary Beth Schwartz, MaryBeth.Schwartz@electrochem.org Print Production Manager: Dinia Agrawala, interface@electrochem.org Staff Contributors: Frances Chaves, Beth Craanen, Genevieve Goldy, Mary Hojlo, Christopher J. Jannuzzi, John Lewis, Anna Olsen, Jennifer Ortiz, Shannon Reed, Beth Schademann, Mary Beth Schwartz, Francesca Spagnuolo, Keerthana Varadhan Advisory Board: Brett Lucht (Battery), Dev Chidambaram (Corrosion), Durga Misra (Dielectric Science and Technology), Philippe Vereecken (Electrodeposition), Jennifer Hite (Electronics and Photonics), Mani Manivannan (Energy Technology), Cortney Kreller (High-Temperature Energy, Materials, & Processes), John Weidner (Industrial Electrochemistry and Electrochemical Engineering), Jakoah Brgoch (Luminescence and Display Materials), Hiroshi Imahori (Nanocarbons), Jim Burgess (Organic and Biological Electrochemistry), Andrew Hillier (Physical and Analytical Electrochemistry), Ajit Khosla (Sensor) Publications Subcommittee Chair: Turgut Gür Society Officers: Stefan De Gendt, President; Eric Wachsman, Senior Vice President; Turgut Gür, 2nd Vice President; Gerardine Gabriela Botte, 3rd Vice President; Marca Doeff, Secretary; Gessie Brisard, Treasurer; Christopher J. Jannuzzi, Executive Director & CEO Statements and opinions given in The Electrochemical Society Interface are those of the contributors, and ECS assumes no responsibility for them. Authorization to photocopy any article for internal or personal use beyond the fair use provisions of the Copyright Act of 1976 is granted by The Electrochemical Society to libraries and other users registered with the Copyright Clearance Center (CCC). Copying for other than internal or personal use without express permission of ECS is prohibited. The CCC Code for The Electrochemical Society Interface is 1064-8208/92. Canada Post: Publications Mail Agreement #40612608 Canada Returns to be sent to: Pitney Bowes International, P.O. Box 25542, London, ON N6C 6B2 ISSN : Print: 1064-8208

Online: 1944-8783

The Electrochemical Society Interface is published quarterly by The Electrochemical Society (ECS), at 65 South Main Street, Pennington, NJ 08534-2839 USA. Subscription to members is part of membership service; subscription to nonmembers is available; see the ECS website. Single copies $10.00 to members; $19.00 to nonmembers. © Copyright 2021 by The Electrochemical Society. *“Save as otherwise expressly stated.” Periodicals postage paid at Pennington, New Jersey, and at additional mailing offices. POSTMASTER: Send address changes to The Electrochemical Society, 65 South Main Street, Pennington, NJ 08534-2839. The Electrochemical Society is an educational, nonprofit 501(c)(3) organization with more than 8,500 scientists and engineers in over 75 countries worldwide who hold individual membership. Founded in 1902, the Society has a long tradition in advancing the theory and practice of electrochemical and solid state science by dissemination of information through its publications and international meetings. Cummings Printing uses 100% recyclable low-density polyethylene (#4) film in the production of Interface.

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

3 All recycled paper. Printed in USA.

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The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Solid State Aspects of Energy Conversion by Paul A. Maggard

In Search of the ‟Perfectˮ Inorganic Semiconductor/Liquid Interface for Solar Water Splitting by Krishnan Rajeshwar, Paul A. Maggard, and Shaun O’Donnell

Synthesis as a Design Variable for Oxide Materials by Jack Vaughey, Steve Trask, and Ken Poeppelmeier Electrodeposition as a Powerful Tool for the Fabrication and Characterization of NextGeneration Anodes for Sodium Ion Rechargeable Batteries by Nathan J. Gimble,* Kelly Nieto,* and Amy L. Prieto A Vision for Sustainable Energy: The Center for Hybrid Approaches in Solar Energy to Liquid Fuels (CHASE) by Jillian L. Dempsey, Catherine M. Heyer, and Gerald J. Meyer

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Vol. 30, No. 1 Spring 2021

the Editor: 3 From The New Leisure Class Corner: 7 Pennington Adapting–and Advancing– Through Unforeseen Circumstances

8 2020 Year in Review and Balsara on 11 Newman Electrochemical Systems Fourth Edition

ECS Community on 13 The Adapting, Advancing, and

Overcoming the Pandemic

15 Society News ECS Meeting with 26 239th IMCS 18 32 Free Radicals 35 People News 37 Looking at Patent Law 43 Tech Highlights 69 Section News 74 Awards Program 80 New Members 83 Student News ECS Meeting 89 240th Call for Papers On the Cover: For the spring cover, we consulted guest editor Paul A. Maggard. To visualize energy conversion, he suggested using a caterpillar turning into a butterfly, a growing flower, or fire burning. We combined fire and the butterfly to capture the transformation. Cover design by Dinia Agrawala.

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The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

PENNINGTON CORNER

Adapting–and Advancing–Through Unforeseen Circumstances

omeone much wiser than I once said, “Sometimes, the situation is the boss.” I was reminded of this sobering fact as I was writing my 2020 annual work review and setting my goals for the year to come. Looking back at all that happened in 2020, and trying, as best I could, to peer forward into 2021, the inescapable truth of this axiom hit me head-on. I realized that while we may be in charge, we are by no means in control. Some might say that is a fatalistic, somewhat helpless point of view, but I beg to differ. There is a certain liberation in recognizing the limitations of what we can control. To me, it is the same sort of liberation that comes from accepting the Socratic notion that true knowledge exists in first knowing that we know nothing. Acceding to these truths is not just liberating—it is also inspiring. As CEO of an organization, it is a vital strategy for guiding the work of the Society and navigating the very tricky waters in which we are currently sailing. Every January, I provide the ECS Executive Committee (ExCom) a list of goals and deliverables for the year ahead that aligns with major long-term strategic initiatives defined by the ExCom and the Board. Each goal includes dates and timelines, costs and resources needed, and the ultimate benefit to the Society. However, in addition to these targeted, specific goals, and in recognition of the limitations to our true span of control, I always include one open-ended goal called “Issues Management.” The description is simple but vague: allot time to manage unforeseen circumstances that arise through the year, which although unplanned, require significant time and effort to address. Some years, there is not much in the Issues Management column—a troubling IT challenge, an unexpected employee departure, or a policy or regulation change. These are not trivial matters, however looking at them in the rear-view mirror several years hence, they do not loom so large. In fact, they seem minor. But then there are years when Issues Management is pretty much all I contend with: the September 11, 2001, attacks; for those like me who live and work along the New Jersey coastline, Hurricane Sandy in 2012; and for all of us around the globe, 2020 and the COVID-19 pandemic.

When I drafted my goals for 2020, chief among them was to produce two major in-person events. One, PRiME 2020, sponsored in cooperation with our friends at The Electrochemical Society of Japan and The Korean Electrochemical Society, promised to be the largest gathering in ECS’s storied history. Another major goal was to greatly enhance the educational and professional development offerings at our in-person meetings. But, like so much in 2020, nothing went according to plan. There was little—if anything—we could do to change that. Clearly, the situation was the boss. Our goal became to leverage our collective resources and capabilities to ensure that we could serve our community despite the pandemic. Looking back, I am truly proud of what ECS, the volunteer leaders, and staff accomplished in 2020. Together, we: • Created our first fully digital meeting, providing an entirely new way to convene our community; • Hosted the largest single ECS event in our history, with nearly 7,000 people registering for PRiME 2020; • Launched the ECS Webinar Program; • Experienced record-breaking downloads for the ECS Digital Library, over 4 million for the first time! Through all this change, uncertainty, and innovation, we also provided measured, prudent financial stewardship to protect the Society’s investments and real estate holdings, ensuring we have the financial resources necessary to keep ECS’s vital operations moving forward despite the challenges faced. And that is precisely what we will continue to do in 2021. Yes, we have goals for 2021. Yes, we have the game plan, the passion, and the drive to achieve those goals. But we know that the future is always uncertain, this year more than most, and so we will adapt as needed to continue to serve the ECS community and advance our science for the benefit of all.

Christopher J. Jannuzzi ECS Executive Director/Chief Executive Officer Chris.Jannuzzi@electrochem.org https://orcid.org/0000-0002-7293-7404

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

2020 Year in Review ECS Adapts and Advances

The new decade started with compounding crises: a global health pandemic; faltering economies; the devastating effects of climate change; and in the U.S., social unrest and science denial on an unprecedented scale. As COVID-19 changed everything about how we live and work, ECS adapted and innovated to continue to support, convene, and advocate for our world-wide community. We developed new ways to engage with a broader range of people, holding the largest single gathering in our 118year history, PRiME 2020. A new series of webinars brought electrochemical education into homes around the globe. Through disciplined, prudent fiscal stewardship, we maintained our strong financial position and launched a new partnership with IOPscience, leading to dramatic increases in the dissemination of our digital content worldwide. Our top priority is, and will always be, the well-being of our community. We wish you and your family peace and good health. Thank you for your support in these uncertain times.

Membership

Decrease in student memberships

Student members

2,872

Total members Decrease in membership

8.3%

8,046

Overall retention rate

56%

new ECS Student Chapters totaling 107

Fellowships and Awards Toyota Fellowship

• Money awarded: $150,000 • Number of recipients: 3 recipients at $50,000 each

Biannual Meeting Travel Grants

• 237th ECS Meeting o No travel grants awarded as the 237th ECS Meeting was cancelled. • PRiME 2020 meeting o Money awarded: $11,290 o Number of recipients: 86

ECS Fellows

• 2020 Class inducted 14 fellows

ECS Summer Fellowships

• Money awarded: $20,000 • Recipients: 4 recipients at $5,000 each

Society, Section, Division prizes

• General Student Poster winners: $3,000 o Three General Student Poster winners  1st prize: $1,500; 2nd prize: $1,000; 3rd prize: $500 • Society, Division, and Section: $67,000 o Total: 38  Society: 6; Division: 25; Section: 7 The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Meetings 237th ECS Meeting with International Meeting on Chemical Sensors (IMCS) (cancelled)

2,950 total abstracts

PRiME 2020 (digital) joint meeting of ECS,The Electrochemical Society of Japan (ECSJ), and The Korean Electrochemical Society (KECS)

countries represented

6,891 attendees

3,900 abstracts

PRiME 2020 Special Events • Legends of Battery Science: A Celebration in Honor of Nobel Laureates M. Stanley Whittingham and Isamu Akasaki • Honorary symposia and sessions for Hideaki Takahashi, Philippe Marcus, Ken Nobe, Junichi Yoshida, and Mogens Mogensen • Electrochemical Energy Summit 2020 • Symposium on 4D Materials and Systems + Soft Robotics

$$$$

symposia

exhibitors

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Symposium speaker funding

• Total dollars in registration waivers: $88,115 • Total dollars in travel reimbursement: $12,370* *As PRiME was digital, travel grants were allocated to symposium award winners ($4,015) and memberships ($8,265). 9

Publications Germany Japan China

992

total of open access papers published

ers publ ishe p a di sp s e

Canada

71 83 355 96 132 255

published in the 2020 volume year

Open ac c

country)

47%

(by 20 20

of all journal content published since 2014 as open access

of articles published in 2020 as open access

2,096 journal articles

Other

35%

institutions published open access at no cost

178

number of papers published by subscribing institutions

USA

270 subscribing

4,000,000+ articles and abstracts downloaded from the ECS Digital Library

New Ventures • • • •

Single Sign On implemented with ORCID iD integration Partnership with IOP Publishing IOPscience hosts the ECS Digital Library ECS Pacific Northwest Section chartered

ECS WEBINAR SERIES launches

3,968 registered participants

sessions

2,151

live participants

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Newman and Balsara on Electrochemical Systems Fourth Edition

by Frances Chaves

he long-awaited fourth edition of Electrochemical Systems by John Newman and Nitash P. Balsara is now available. This classic serves as a textbook and dependable resource for students and seasoned scientists alike. The authors update all of the chapters, add content on lithium battery electrolyte characterization and polymer electrolytes, and include a new chapter on impedance spectroscopy. Make room on your bookshelf for the fourth edition.

The Fourth Edition

The fourth edition covers topics including electrochemical theories as they relate to the understanding of electrochemical systems; the foundations of thermodynamics; chemical kinetics; transport phenomena including the electrical potential and charged specials; and how to apply electrochemical principles to systems analysis and mathematical modeling. The fourth edition is presented in four sections: • Thermodynamics of Electrochemical Cells • Electrode Kinetics and Other Interfacial Phenomena • Transport Processes in Electrolytic Solutions • Current Distribution and Mass Transfer in Electrochemical Systems Three appendices include information on partial molar volumes; vectors and tensors; and numerical solution of coupled, ordinary differential equations. ECS thanks Drs. John Newman and Nitash P. Balsara, authors of Electrochemical Systems Fourth Edition, for generously taking time in December 2020 to speak with us. Q: Why a fourth edition? Dr. Newman: This is the first time that many topics have been covered. Also, there’s more emphasis on physics, impedance, oxygen electrode, and turbulence. Dr. Balsara: A lot had happened in the battery space since 2004, when the third edition was released. Lithium-ion batteries have dominated and continue to dominate the energy landscape in an increasingly important way, from the point of view of transportation and other energy needs. It has been a joy for me to work on the fourth edition and see it in the context of new developments. Dr. Newman: The book can be used to model and understand a variety of electrochemical systems, first: batteries, second: hydrogenand oxygen-based fuel cells, third: corrosion, fourth: production of aluminum and chlorine (electrochemical synthesis), fifth: biological systems, sixth: electroplating and electrofinishing, and lastly, renewable energy. Q: How has the book stood the test of time? Dr. Balsara: John’s book has increased in importance over the years. In the first edition (1973), John created a framework to understand what happens inside all the electrochemical systems that John enumerated above. Some applications like batteries are now described by elaborate models due to the need to understand exactly when they will run out of charge. His framework has stood the test of time.

Dr. Newman: The book has Electrochemical Systems, 4th been relevant throughout this Edition (The ECS Series of Texts entire period. What’s changed and Monographs) by John Newman is that people are increasingly and Nitash P. Balsara. ISBN: 978-1-119-51460-2. 608 pages. understanding its relevance and Hardcover copy. Price: $175. importance. Recently, I was Publisher: Wiley (www.wiley.com) speaking with people at Ohio University who are interested in removing pollutants from water. I published a paper about that in 1971. An important problem in modeling these systems is turbulence. This was the subject I talked about at two universities in the last week, a subject that has challenged scientists for over a century. In the talks, I referred to Heisenberg’s dissertation (published in 1924) on turbulence.1 He is one of the fathers of quantum mechanics. Many subjects worked on in the past 100 years fit nicely together. I see these all as timeless topics. Q: Can the book apply to emerging problems? Dr. Balsara: John teaches us how to model complete electrochemical systems. Sensors are electrochemical systems. Increasingly people want to power them for a long time and not have to worry about them. Many of the principles used to design these systems were laid out in John’s first edition. How do you modify your system to accommodate new requirements? When it first came out, the Prius needed a battery that charged and discharged 50,000 times. This is an example of a system that was modeled using John’s framework but in a way that had not been used before. Q: How does The Electrochemical Society foster innovation? Dr. Newman: I am an Honorary Member of ECS and attended Society meetings in 2016, 2017, and 2019. It is an institution that values scholarship. The three scientists who won the Nobel Prize for lithium-ion batteries are ECS members. The Society encourages young people: student membership is not prohibitively expensive, and students are encouraged to speak at meetings (whereas I know of at least one other society where students “should be seen but not heard,” as they say). The Electrochemical Society has a balance between the academic side, represented by members and universities, and the industrial side, where I have done extensive consulting. ECS covers what we call the wet and dry sides, all the photoelectrochemical things and the transistor things. ECS is in the middle of the technology as it is developing. Dr. Balsara: John began his career early on in electrochemistry. He built and made the field what it is today. I entered the field when I was about 10 years into my academic career; I began my academic career working in the general area of polymer science. The Electrochemical Society is where I learned what it takes to transition from just knowing what plastics do, into thinking about what polymers (continued on next page)

Werner Heisenberg, “Über Stabilität und Turbulenz von Flüssigkeitsströmen,” Annalen der Physik, Band 74, No, 15, pp. 577-627, 1924. English translation: Washington: National Advisory Committee on Aeronautics, Technical Memorandum 1291, June, 1951. Translated by Mary L. Mahler.

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

(continued from previous page)

might do in electrochemical systems. I didn’t understand anything in the talks I attended the first few meetings! However, it was a great education; I stuck with it, and slowly, I started learning the language and the concepts. The wisdom of the field became apparent to me through attending ECS meetings. They are where my students go to get educated. ECS meetings are extremely relevant. It’s the go-to meeting if you really want to get on top of the field. Q: What does your work look like today? Dr. Newman: I have been officially retired for 10 years. I moved to North Carolina and work with this laptop. Last week I gave two talks, one at the University of Illinois; the other at Ohio University. I went to Illinois and Ohio from my home. And we had productive times in both of these places! I don’t like to travel, yet I can work with people in India, in Russia, and around the world. I tried to involve a friend in Russia and told him all he needed was a computer and a library. He corrected me, “No, you also need time.” He is at a stage in his career where he has young people working for him, so he has to work for them, too, and find funding for their work. He doesn’t have the freedom that I have. Dr. Balsara: I run the lab from home as instructed by the university and the national lab where I work; I have a joint appointment. There are extreme limits on the number of people who can occupy a lab. My presence there may be a liability because I take a spot from a student who’s trying to finish their thesis or project. I’m amazed by the Berkeley students and their resiliency. They produce results at a rate that is fun to watch. We are doing our best. I would say we are at 80 percent productivity at this point.

Q: Do you believe that mentorship is a two-way street? Dr. Newman: We’re mentoring students who are going to take over and do important things. Everybody thought that my career was brilliant because I kept doing interesting things. The truth is that I had students. The students came and went and started different things. Everybody thought that was because of my excellent leadership. But really, it was because students come up with new ideas all the time and keep doing all kinds of interesting things. They benefit from a little guidance. It’s more efficient to start with people who already know something. The students at Berkeley are really good! Dr. Balsara: It has been a privilege to work with John on the book. He is very much a mentor to me. John underplays his role as a mentor. His students flourish because instead of having us start from scratch, he shows us the way that takes us to our destination. And he does it in a way that brings us joy. Sometimes I asked the same question five times because I didn’t understand the answer. He’s very, very patient. That comes through in the book, in my view. Q: Is there going to be a fifth edition of Electrochemical Systems? Dr. Balsara: John refers to the issue of the current that flows through the human nervous system; however it has not been addressed directly yet. Perhaps in the fifth edition, we will make that connection more directly. There is a lot of work to be done in electrochemical systems. It’s an exciting place to be! When asked when he thought a fifth edition would be needed, Newman replied, “When Nitash can get on it!” © The Electrochemical Society. DOI: 10.1149.2/2.F01211IF.

About the Authors

Nitash P. Balsara, PhD, holds the Charles W. Tobias Chair in Electrochemistry at the Department of Chemical and Biomolecular Engineering, University of California, Berkeley, where he has been a professor since 2000. A Fellow of the American Physical Society, he received the Charles M. A. Stine Award for Materials Engineering and Science from the American Institute of Chemical Engineers (2005), and the John H. Dillon Medal for Polymer Physics from the American Physical Society (1997). He may be reached at nbalsara@berkeley.edu. https://orcid.org/0000-0002-0106-5565 Photo: www.rickchapman.com

John Newman, PhD, lead author on all editions of Electrochemical Systems, has been a Professor of Chemical Engineering at the University of California, Berkeley, since 1963. He is a Fellow of The Electrochemical Society and a member of the National Academy of Engineering. Newman received the ECS Edward Goodrich Acheson Award (2010), ECS Olin Palladium Medal (1991), ECS Henry B. Linford Award for Distinguished Teaching (1990), ECS Physical Electrochemistry Division David C. Grahame Award (1985), and ECS Young Authors’ Prizes in 1969 and 1966. He may be reached at newman@newman.cchem.berkeley.edu.

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

THE ECS COMMUNITY ON ADAPTING, ADVANCING, AND OVERCOMING THE PANDEMIC

by Frances Chaves ere we are, over a year into a global pandemic, the likes of which has not been seen in a century. The Society continues to actively monitor the pandemic to prepare for potential impact on programming—and to support our community. When we spoke with members last spring about COVID-19’s impact on their lives and work, it was clear that engagement with an active community was vital to maintain mental health. Everyone was convinced that electrochemistry and solid state science would play a critical role in overcoming the current crisis. Today we see that research, collaboration, teaching, and learning are continuing in new ways. The ECS community is responding to the pandemic with resilience and creativity rather than despondence. Here’s how.

Reinventing the Wheel

The Society completely reinvented its meeting format after the unfortunate but warranted cancellation of the 237th ECS Meeting. For the first time in its history, ECS presented a meeting—PRiME 2020—entirely from a digital platform. Presentations were reimagined, as was the fee structure. Participation was 100 percent free; only presenters paid a fee that was less than regular registration. Response to the meeting was overwhelmingly positive, with a record participation of 6,891 people from 78 countries. Virtual connecting continued with the launch of a new ECS webinar series. In 2020, 3,968 people registered for 12 different webinars, with 2,151 attending the live sessions presented by distinguished ECS members.

On the Science Frontier Joe Stetter—inventor, entrepreneur, and owner of KWJ Engineering and Spec Sensors—shared his desire last spring to “help the frontline people who keep this country moving.” His niece, a nurse, got one mask a week that she kept in a paper bag. Joe’s solution: build a small, portable, inexpensive sterilizer. “The project is called S4PPE. We developed prototypes, computer-controlled, Joe Stetter performed several in-lab demonstrations, and are looking for partners interested in field testing the system,” Joe said recently. “We can make and supply critical parts of the Joseph R. Stetter- jrstetter@kwjengineering.com

Initial validation of a compact ozone sterilization chamber prototype using an E. coli bacteriophage D. Ebeling1, J. Werner1, J. Erbe1, S. Ebeling1, Q. Miao1, A. Ebeling1, L. Sanford1, D. Peaslee2, L. Ploense3, R. Ploense3, E. Stetter3, M. Findlay3, B. Meulendyk3, M. Lee3, V. Patel3, J. Stetter3; 1 Wisconsin Lutheran College, Milwaukee, WI, 2 Spec Sensors LLC, Newark, CA, 3 KWJ Engineering Inc., Newark, CA

Abstract

Advances in Ozone Sterilization Chamber

Results and Discussion

The rapid spread of the COVID-19 pandemic worldwide has taxed the availability of N95 masks and other personal protective equipment (PPE). Widespread ability to sterilize and re-use N95 masks will help relieve this critical issue in the short-term. It is also clear that additional long-term benefits of sterilization and reuse will include lowering operating cost, improving material supply chain logistics, and reducing waste. KWJ Engineering is leading development of an inexpensive modular sterilizer design which requires no toxic chemical consumables, generating the ozone (O3) on demand as needed in precisely controlled concentrations and cycle times. The unit will be inexpensive and portable enough to provide sterilization of PPE to virtually all types of healthcare facilities, clinics, and emergency response teams, regardless of size or location. Additionally, this capability to sterilize N95 and medical masks will allow other non-emergency care users to sterilize and reuse masks and PPE rather than disposing of them. This will reduce the demand, allowing more ready access to new PPE for emergency healthcare workers.

The phase 2 S4PPE system of containers with O3 in-situ generation as a schematic (Figure 3) and picture (Figure 4). The top is removable so the bottom container can be transported with the sterile material to the worksite. The next container of soiled PPE can be transported to the S4PPE in the 5-gal container and its lid removed and replaced with the lid with the ozone capability. After mounting the S4PPE lid, the sterilization occurs at the push of a button, and the readout monitors the [O3], time, T, RH and reports the compete cycle at the end. The S4PPE lid has a safety O3 sensor to shut down O3 generation if any leaks occur. The lid also contains an O3 destruct filter that destroys the O3 at the end of the cycle before the lid is opened and the sterile PPE can be removed. There is a possibility to have many transport containers for one S4PPE since the cycle only takes about one hour. Thus, one S4PPE can support multiple field operations. The power supply is a simple charger such as is used for a PC or other portable electronics and the entire system can run on 12V DC and is powered by an AI algorithm on an Arduino microcontroller. The system is designed to be inexpensive and easy to operate for even small operations like clinics, emergency rooms, or small companies and universities providing confidence that reused Figure 3. Schematic of phase 2 S4PPE concept. PPE is safe [not to mention

BB A Considering that viruses, when mixed in a ~300 ppm O3 with phage on 3M mask material liquid aerosol droplet, could land and 1.0E+08 remain on the surface of some materials or 1.0E+07 soak into other materials, the ozone 1.0E+06 chamber was tested for its ability to 1.0E+05 decrease bacteriophage concentration on two substrates, mask material and filter 1.0E+04 paper disks. When tested by pipetting 2.5 1.0E+03 and 25 microliters of LB broth on mask 1.0E+02 material, the liquid did not soak into the material but instead remained as a droplet 1.0E+01 on the surface until it eventually dried. 1.0E+00 15 min 30 min 60 min However, the filter paper disk allowed both O3 treated Not treated 2.5 and 25 microliters of LB broth to soak into the filter disk completely. Figure 6. (A)TLS-soaked filter disks and (B) 3M mask material, treated with approximately 300 ppm ozone. The results for the 60 minute ozone-treated As shown in Figures 6A and 6B, there was samples, also 30 minute in (B), is more accurately <100 PFU, as there were nearly zero plaques on the least dilute plates. This experiment was greater than a four log reduction in active performed at room temperature with high RH. Only one trial (with three technical replicates each) was performed under these conditions. TLS concentration on mask material and filter disks after one hour of maximal ozone treatment compared to untreated samples. However, there was a marked difference in TLS inactivation levels between the two substrates at the 30 and 15 minute time points. This could be due to the different materials or the fact that the LB broth containing TLS is able to soak into the filter disk thus potentially making it more challenging for the ozone to reach and inactivate the phage.

While viral particles may be transmitted via liquid aerosol droplets, it is possible these droplets may dry on surfaces after they land. This leaves the possibility that viruses in liquid (wet) samples and dried samples may react differently to ozone treatment. From Figure 7, it can be seen that allowing the sample to dry before treatment resulted in less inactivation. Low humidity also furthered that effect. Additionally, while ozone is demonstrated to be effective at inactivating viruses (Hiroshi, 2009; Hudson 2007), relative humidity appears to play a role in the effectiveness of ozone for inactivation (Dubuis, 2020). It is likely that ozone reacts with water to generate reactive oxygen species which is harmful to living organisms and viruses. These preliminary experiments helped focus experiments to investigate of the effect of RH on dried-on samples for one-hour treatments. Determining the effective concentration of ozone at high and low RH

Figure 4. Phase 2 sterilization chamber side view (A), and lid with all assemblies mounted to it (B).

Validation Materials and Methods Preliminary tests of the effect of ozone on TLS bacteriophage on the were done to investigate some of the major variables. Tests were done with high ozone concentrations (~300 ppm) for 15, 30, and 60 minutes on filter paper discs (Remel) (Figure 6A), clear vinyl from microscope cover slips (Fisherbrand), and N95 mask material (VFlex, 3M) (Figure 6B). Each piece was approximately 0.5 cm2. Variations of tests on the mask material included allowing the TLS solution to dry on the substrate vs. immediately placing the it into the chamber and also 100% RH (high) vs. 50% RH (low) in the chamber (Figure 7). Based on the preliminary results, the variables of concentration and RH were investigated further with applications to mask material. On ten separate days, 5 trials of low RH (47-55%) and 5 trials of high RH (>95%) were carried out. Each trial had 3 replicates. Concentrations of 0, 25, 50, 100, and 200 ppm ozone were applied for one hour. Each data point on the graphs is an average of the 5 trials, normalizing the inactivation to the one hour 0 ppm trials (Figures 8A and B).

After establishing several important factors for effective inactivation of TLS, the final condition tested in this study was ozone concentration. The difference in TLS inactivation between no ozone treatment and each ozone concentration is plotted in Figure 8. In high RH conditions, an increase in TLS inactivation is observed from 25 to 200 ppm. There is nearly a 3 log reduction at 50 ppm, 3-4 at 100 ppm, and 4-5 at 200 ppm. Even at the 25 ppm ozone concentration close to a 2 log reduction in TLS activity was observed. However, when this experiment was repeated with ambient RH, there was little to no inactivation of TLS. This is consistent with the results in Figure 7 and further confirms that RH is an important factor to consider when using ozone to inactivate viruses. AA 0.6 0.5 0.4 0.3 0.2 0.1 0

100

Sample preparation and plaque assay

Figure 1. Phase 1 sterilization chamber used for data collection, left (A); and under side of the lid with fans and sensor, right (B). B A Figure 2. Holders for stacking masks or other PPE inside the chamber, maintaining space between each item. (A) Stacked brackets and (B) laser cut and rolled plastic.

TLS bacteriophage was diluted to approximately 109 plaque-forming units (PFU)/ml. To the mask material, 2.5 microliters of TLS dilution was added. To the filter disks, 25 microliters of a 108 PFU/ml TLS dilution was added. After treatment in the ozone chamber, samples were removed, placed in LB broth, and shaken vigorously for 30 seconds. Serial dilutions (1:10) of these samples were then prepared. A 100 microliter sample of each sample dilution, 250 microliters of overnight-grown E. coli culture in LB broth, and four milliliters of top agar were mixed in a sterile culture tube and spread on an LB agar plate. Plates were incubated overnight at 37°C. TLS plaques were counted the following day. Figure 5. Schematic of procedure and plaque assay.

150

200

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Figure 7. Comparing RH levels on different samples with vinyl and mask substrates in a 30 min treatment. The “dry” samples air-dried for 1 hour before treatment. The ”non-treated” control was in 0 ppm ozone for 30 min.

High RH log-scale phage inactivation 1 hour 5.0 4.5

ppm ozone 0

4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5 0.0 0

ppm ozone

Growth media and organisms Luria Broth – Miller’s (Research Products International) and Luria Agar – Miller’s (Research Products International) were prepared as instructed on the container. Top agar was a 50/50 mixture of Luria Broth and Luria agar. The strain of Escherichia coli used in this study was the laboratory strain, MC4100 (Casadaban, 1976). The bacteriophage used in this study was TLS (German and Misra, 2001). Both MC4100 and the TLS bacteriophage were obtained from Dr. Rajeev Misra at Arizona State University.

Low RH log-scale phage inactivation 1 hour

Log of inactivation vs. 0 ppm control

The chamber is closed with the material to be sterilized inside. Ozonated air is forced into the chamber at 1.5 L/min, and the concentration in the chamber increases to the desired concentration at a rate of 25 ppm/min. The ozone concentration, relative humidity (RH), and temperature are monitored and logged inside and outside of the chamber with a DGS-O3 (Spec Sensors, Newark, CA). In addition, in these experiments, the ozone concentration inside the chamber was monitored with a UV-100 ozone analyzer (EcoSensors, Newark, CA) to confirm the accuracy and stability of the inexpensive printed amperometric O3 sensor’s feedback control of ozone concentration.

Plaque-forming units

Comparison of wet versus dry samples and effects of relative humidity on inactivation of TLS B

Plaque-forming units

reducing cost and waste].

Ozone Sterilization Chamber [PATENTS PENDING 2020] KWJ Engineering and Wisconsin Lutheran College have collaborated in ozone sterilization projects, and have developed instruments with applications for water disinfection and sterilization of medical equipment (Shirke, 2014; Stetter, 2012). The construction of this chamber uses similar technologies with simpler construction. The S4PPE [Sterilization for Personal Protective Equipment] chamber was constructed using two nesting 5-gallon FDA-approved plastic polypropylene containers, one of which the bottom 3” was cut off horizontally to be nested in the other (Figure 1A). The lid of the top bucket holds the gas connections, sensors, and fans (Figure 1B); the top side of the lid has the control electronics [optional]. Ozone was generated with an Ozotech Poseidon 200 [or equivalent source, several successfully used in prototypes], and air was pumped with a Whisper AP300 or similar inexpensive air pump. Air leaving the chamber passed through an ozone destruct filter. In one preferred source design, the ozone is generated in-situ and recirculated. Inserts, such as the mask rack (Figure 2), can be used to keep air space between the PPE material to be sterilized.

Log of inactivation vs. 0 ppm control

Using off-the-shelf components, KWJ fabricated a benchtop sterilization chamber with controlled relative humidity (RH) and ozone to develop and validate the ozone sterilization protocol for deactivation of surrogate viruses on N95 masks. Preliminary experiments have been performed using TLS, an E. coli bacteriophage (bacteria-infecting virus), to provide initial estimates of effectiveness for variables such as time, ozone and viral concentrations, temperature, relative humidity, and virus-contaminated substrate. Initial experiments have confirmed previous reports that bacteriophages are susceptible to inactivation by ozone treatment. We have demonstrated that the effectiveness of ozone treatment is relative to the amount of water either in the sample or in the air. Wet samples of TLS bacteriophage on cellulose disks, FFP3 N95 mask material, or on vinyl sheets showed a 2-3 log reduction in active bacteriophage when treated with greater than 200 ppm ozone and ambient RH (47-55%) but less than one log reduction in activity if the bacteriophage sample is dried on the material before ozone treatment. However, if the experiments are repeated with close to 100% RH in the chamber, there is a greater than 4-5 log reduction in active bacteriophage within one hour, regardless of material and whether the initial sample was wet or dried. This demonstrates that this ozone sterilization chamber is capable of inactivating TLS bacteriophage as designed, but it is necessary for ozone to be combined with high RH to effectively work in a variety of conditions.

Comparison of substrates

100

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phage inactivation 0.000%

99.245%

99.831%

100

99.961%

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Figure 8. (A) Relative humidity in the chamber was ambient (47-55%). (B) Humidity was high (>95%). The error bars are standard error; n=5. In (C) the high RH data from (B) is shown in a table.

References Casadaban, M J. “Transposition and fusion of the lac genes to selected promoters in Escherichia coli using bacteriophage lambda and Mu.” Journal of molecular biology vol. 104,3 (1976): 541-55. Dubuis, Marie-Eve et al. “Ozone efficacy for the control of airborne viruses: Bacteriophage and norovirus models.” PloS one vol. 15,4 e0231164. 10 Apr. 2020. German, G. and R. Misra. “The TolC protein of Escherichia coli serves as a cell-surface receptor for the newly characterized TLS bacteriophage.” Journal of molecular biology 308 4 (2001): 579-85. Hiroshi, Tanaka et al. “Inactivation of Influenza Virus by Ozone Gas.” IHI engineering review 42 (2009): 108-111. Hudson, J B et al. “Inactivation of Norovirus by ozone gas in conditions relevant to healthcare.” The Journal of hospital infection vol. 66,1 (2007): 40-5. Shirke, A, Li, S, Ebeling, D, Carter, M, Stetter, J. “Integrated Ozone Microreactor Technology for Water Treatment” ECS Transactions 58(35): 11-20 (2014). Stetter, J. Principle Investigator; National Institute of Health SBIR Grant; “A New Low Power Low Cost Ozone Sterilizer for Medical Equipment” (2012).

CONCLUSION An affordable PPE sterilizer has been developed, validated, and shown to repeatedly inactivate more than 99% of bacterial virus on N95 mask material at conditions between 25 and 200 ppm, one hour, and high RH. Future work will also demonstrate the efficacy on other organisms including mammalian viruses and pathogens, further showing the utility of this sterilizer in protecting individuals from COVID-19 and other transmissible diseases.

system like the ozone generator and circulator, safety sensors for control, and the ozone safety destruct filter system. Each of these parts is low cost, run on 12 VDC (battery or a simple computer power supply), and the entire device plans are available now. We published a poster paper on the efficacy of a surrogate virus that is harder to kill than COVID-19, and if possible, want to move forward with a partner to get to widespread use.” A year ago, Netz Arroyo-Currás, Assistant Professor at Johns Hopkins School of Medicine, described how his lab shifted gears to develop a highly specific, sensitive device to rapidly identify people infected with the SARS-CoV-2 virus. He briefed us on recent developments. “We are continuing the development of this platform. Unfortunately, some of the approaches we pursued initially Netz Arroyodidn’t provide the robust response we were Currás hoping to achieve in the assay. In response, we have been doing substantial protein engineering to address this issue. Our hope is to successfully develop the electrochemical sensing strategy in the next few months.”

An Industry Perspective Before 2020, Alex Peroff, Electroanalytical Scientist at Pine Research, traveled extensively for conferences and customer visits. He has worked from home since spring 2020. While not ideal, Peroff keeps a positive outlook, using this period as a gift to reflect and develop great new ideas. Lab access is minimal and strictly regulated. New product development continues, but significant supply Alex Peroff chain disruptions impact production. There Photo: Pine are “big rippling effects” if anyone tests Research positive for COVID-19, he says. International inquiries for products and technical assistance continue, but the U.S. is comparatively slow. “In the past, digital marketing complemented ‘outbound’ or ‘boots on the ground’ efforts. Now it’s the only way to reach our customers. We have redoubled our digital marketing efforts. For example, to support our customer base, I’m improving our YouTube videos’ quantity and quality.” Although digital communication “is never quite the same as face-to-face,” Peroff uses Zoom, Skype, Facebook, Twitter, telephone—whatever works to maintain communication. “I love hearing from professors who just got their publications out or won grants.

International Society of Exposure Science Virtual Meeting – September 21-22, 2020

Poster presenting Joe Stetter’s compact ozone sterilization chamber prototype. The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

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They’ll say, ‘I finished this proposal while my kids were yelling at me!’ I hear noise and dogs barking in the background. I help them by providing support and encouragement.” “Everything is moving digitally, which creates new opportunities to engage with our customers,” Peroff says. “I’m part of the social media conversation. When someone tweets a weird-looking cyclic voltammogram and puts a little dot and smiley face on it, people respond, ‘It’s a duck’ or ‘It’s a giraffe.’ It’s fun; it’s part of the community; it keeps people’s spirits up. Chemists and electrochemists are people too. We have emotions and feelings, and yes, these are not just clients to us!”

Time Well Spent Rather than spending his sabbatical in the Czech Republic, France, and China—with additional trips to Chile, Italy, and Norway in the planning stages—Mark Orazem, Distinguished Professor in the Department of Chemical Engineering at the University of Florida, was home—where he still is. The pandemic provided the opportunity to finish a project Orazem had been working on for the last 30 years, Mark Orazem the groundbreaking EIS: Measurement Model Program. The impedance spectrometry-measuring tool that he wrote with students in the 1990s was used in-house and not available to the general community. Orazem’s student, William Watson, provided the final key—using Python—to make the distribution of the program viable. (EIS is available at no cost [for noncommercial use] on ECSarXiv, the Society’s free online preprint service.) “I have had more time to work on papers and other endeavors such as the EIS: Measurement Model Program. Of course, this would not have been possible without William! The pandemic also gave me more time to spend with my wife. In some ways, it will be hard to go back to the fast-paced life where I William Watson traveled so much,” Orazem said.

Still Not Your Usual Academic Year When we spoke with Carolyn Graverson last spring, she was completing her senior year at Lewis University. Now she is a first-year chemistry graduate student at Rice University, venturing into unchartered territory in an unparalleled time: living alone off campus for the first time, choosing a lab specialty while being socially distant. Graverson attended different lab groups’ virtual meetings. As there were fewer Carolyn in-person meetings, it wasn’t the same as preGraverson pandemic. Nonetheless, Carolyn is happy with her decision to join the Matthew R. Jones Lab, focusing on nanoparticle assembly and ligand design. “It’s been a little strange. Rice is known for its close-knit (chemistry) department, but we haven’t had that as much (this year). Parts of orientation were in person, but mostly, everything was virtual.

ORCID

Connecting research and researchers

We had department Zoom happy hours where we shared a drink and some laughs. We can’t meet at Valhalla, the on-campus grad student bar, which is the hub of graduate life. (In the past) talking about your project there with other chemistry graduate students led to many collaborations. It’s hard not getting to know people that way. But the department, and especially some of the older graduate students, reached out and did their best under the circumstances to help us adjust,” said Graverson.

Setting the Stage for Solutions

At the 239th ECS Meeting, a joint symposium of the Society and the 18th International Meeting on Chemical Sensors (IMCS) focuses on COVID-19 and Pathogen Related Research, Development, and Engineering in Sensors and Systems. “The ability to respond to such challenges, both related to SARS-CoV-2 virus as well as other biothreats, is highly dependent upon the actionable and timely understanding of the fundamental scientific Peter Hesketh aspects of the problem, from the level of a single patient to a community and beyond,” said lead organizers Peter Hesketh, Professor of Micro and Nano Engineering at The George W. Woodruff School of Mechanical Engineering at Georgia Tech, and Joe Stetter (page 13). All aspects of the COVID-19 situation and the global response and recovery will be covered in the seminar, especially those involving disease detection, surveillance, mitigation, and prevention by using sensors and systems. A second symposium, organized by Sadagopan Krishnan and Hiroshi Imahori, is planned for the 240th ECS Meeting. “Electrochemical and Solid State Science and Engineering Applied to COVID Issues” broadens the discussion to the most recent results related Sadagopan to emergent viral diseases. It covers the science Krishnan and engineering of diagnostics of SARS-CoV-2, Photo: Oklahoma methods of its deactivation, therapeutics, State University surveillance, health care devices, PPE, and other approaches to mitigate the COVID-19 pandemic and its consequences. Bringing together the most active electrochemistry and solid state science and technology researchers in academia, government, and industry to engage, discuss, and collaborate on solutions to the pandemic is sure to have a global impact. Hiroshi Imahori

A Brighter Outlook

Without exception, everyone we spoke with is looking forward to reconnecting face-to-face with their community at the next in-person ECS meeting. In the meantime, digital meetings, webinars, and group and one-on-one online communication keep the community together and supported—and critical scientific research moving forward. © The Electrochemical Society. DOI: 10.1149.2/2.F02211IF.

Visit www.orcid.org . to register.

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ECS Announces Brand Guide The ECS Brand Guide has been posted online to empower unified and consistent use of The Electrochemical Society brand. Following the guidelines ensures that the brand—a critical asset that expresses the ECS persona, culture, and values—is known, respected, and esteemed throughout the world. The ECS global community shares the responsibility for, and integrity of, the Society’s brand. “Welcome to the ECS Brand” is the gateway to the ECS Brand Guide. It includes links to the ECS Brand Assets & Templates page and access to downloadable files. The ECS Brand Guide contains the Society’s brand components and rules for how each element is used when creating branded communications. It includes the following. • ECS master brand logo, font, and colors • ECS sub brands, partnered meeting brands, and alignment groups • Use guidelines for images, video, and social media • Usage directions for formats, website, and voice and tone • Templates and assets are attached, such as the official ECS boilerplate statement in three different lengths, and links to downloadable logos and templates for creating standardized PowerPoint presentations and web content.

ECS Brand Guide

The Electrochemical Society

December 2020, Version 1

65 South Main Street, Building D Pennington, New Jersey 08534-2839, USA Tel: 609.737.1902 l Fax: 609.737.2743 customerservice@electrochem.org www.electrochem.org

The glossary contains explanations and definitions of terms that are not commonly used by ECS Brand Guide users who are not professional graphic designers or writers. Use of the ECS logo, brand elements, and assets requires prior approval by ECS staff. Please address your requests and questions or concerns to customerservice@ electrochem.org.

Introducing the ECS Institutional Engagement Committee The ECS Board of Directors recently approved the proposal to change the name of the ECS Sponsorship Committee to the ECS Institutional Engagement Committee. “We felt that the word sponsorship did not clearly define the purpose of our committee. Our goal is to engage the broader electrochemical community. By defining our committee as the ECS Institutional Engagement Committee, we will reach both the academic and Marion Jones, Chair, ECS industrial members of our society,” said Committee Institutional Chair Marion Jones, Director of Marketing at Engagement Scribner Associates, Inc. Committee The committee’s goals have been evolving over the last several years. “One of the main focuses is to ensure closer, more mutually beneficial relationships between the research community and our industry partners. Research requires industry to move forward and industry needs research to move

a free preprint service for electrochemistry and solid state science and technology

forward! Together, we can do so much to help the global community address critical issues.” Expanding institutional support for ECS is still an important goal. One new initiative has been hosting an industry lunch at ECS meetings. “We’ve had people from Tesla, Apple, GE, and other big institutions come together with our smaller members. Through talking and sharing, we discover common ground. This reinforces the importance of ECS meetings, which are fertile ground for collaboration.” Jones looks forward to the resumption of face-to-face ECS meetings and seeing her fellow committee members. “COVID has slowed down our momentum but not our enthusiasm! We are working at finding ways to keep our academic and industry members engaged—and to support ECS.” For more information about the ECS Institutional Engagement Committee, please contact Staff Liaison Anna Olsen at Anna.Olsen@ electrochem.org.

www.electrochem.org/ecsarxiv

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

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ECS Members in the 2020 Class of Highly Cited Researchers

Husam N. Alshareef

Peter G. Bruce*

Gerbrand Ceder**

Jaephil Cho

IB Chorkendorff

Yi Cui

Sheng Dai

Hubert Gasteiger*

Yury Gogotsi

John Goodenough

Michael Gräetzel

Liangbing Hu

Yu Huang

Joseph T. Hupp*

Thomas F. Jaramillo

Prashant V. Kamat

Marc T. M. Koper*

Hong Li

Yuehe Lin

Jun Lu

Arumugam Manthiram*

Chad A. Mirkin*

Jens K. Norskov

Nam-Gyu Park*

Jan Rossmeisl

Rodney S. Ruoff*

Yuyan Shao

Yang Shao-Horn*

Peter Strasser**

Yang-Kook Sun

Chunsheng Wang

Hailiang Wang

Joseph Wang**

Gang Wu

Nianqiang “Nick” Wu*

Jie Xiao

Guihua Yu

Ji-Guang Zhang

Jiujun Zhang

Qiang Zhang

(Photo: UNIST)

(Photo: Stanford University)

(Photo: University of Maryland)

(Photo: Eric de Vries)

he Electrochemical Society is proud to announce the Society’s distinguished members recognized as 2020 Highly Cited Researchers.1 The prestigious list, published by the Web of Science Group at Clarivate Analytics, identifies scientists and social scientists who produced multiple papers ranking in the top 1% by citations for their field and year of publication, demonstrating significant research influence among their peers.

Only 0.2 percent or nine out of 3,896 Highly Cited researchers appear in three or more Institute for Scientific Information™ (ISI) fields. ECS Fellow Yi Cui and ECS Awarded Life Member Michael Gräetzel were recognized for chemistry, engineering, and materials science. ECS Fellows Yuri Gogotsi, Arumugam Manthiram,* and Yang-Kook Sun are among the 5.2% of all Highly Cited Researchers appearing in two fields—in their case, Chemistry and Materials Science. ECS members Rodney S. Ruoff* and Qiang Zhang are 16

also recognized in these two fields, while Ji-Guang Zhang was included in both the Materials Science and Engineering lists. Highly Cited Researchers (in a single field) include Nobel laureate and ECS Honorary Member and Fellow, John Goodenough. ECS Fellows Hubert Gasteiger*, Prashant V. Kamat, Yuehe Lin, Yang Shao-Horn*, Joseph Wang**, Nianqiang “Nick” Wu*, and Jie Xiao are also on the Highly Cited Researchers list. Below is a list of ECS members whose research on electrochemistry and solid state science and technology is shaping the scientific discourse. If we missed your name, please let us know and we will update accordingly. The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

SOCIE T Y NE WS The Society has an impressive number of student chapters at institutions (universities, government agencies, or other entities) with 24 or more Highly Cited Researchers—including two universities in the top 10: University of California, Berkeley (#6) and Tsinghua University (#9). ECS has student chapters at the following academic institutions included on the list:

ECS Member Highly Cited Researchers in Chemistry Peter G. Bruce* IB Chorkendorff Joseph T. Hupp* Marc T. M. Koper* Jens K. Norskov Jan Rossmeisl Hailiang Wang

Gerbrand Ceder** Sheng Dai Thomas F. Jaramillo Chad A. Mirkin* Nam-Gyu Park* Peter Strasser** Jiujun Zhang

• • • • • • • • •

ECS Member Highly Cited Researchers in Materials Science Husam N. Alshareef Liangbing Hu Hong Li Yuyan Shao Gang Wu

University of Oxford (12) University of Cambridge (16) University of Pennsylvania (17) University of California, Los Angeles (24) University of Washington (31) University of British Columbia, British Columbia (47) Imperial College London (50) University of Toronto (51) Ghent University, Belgium (54)

Congratulations to all!

Jaephil Cho Yu Huang Jun Lu Chunsheng Wang GuihuaYu

Nanoscale Electrochemistry Study using Scanning Electrochemical Cell Microscopy (SECCM) Park SECCM operates under atmospheric conditions, without the need to completely immerse the sample in fluid. SECCM uses a glass nanopipette integrated with a quasi-reference electrode and filled with an electrolyte solution / redox buffer. A tiny droplet formed at the pipette end acts as a mobile nano-sized electrochemical cell that can be scanned across a surface. When the droplet meniscus is in contact with the substrate, a sudden current signal can be detected. Our SECCM system provides researchers full access to control all electrochemical parameters featuring fast and simple setup and reliable operation.

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*ECS Awarded Life Member **Emeritus Member 1 https://recognition.webofscience.com/awards/highly-cited/2020/?campaignname=Highly_Cited_Researchers_Parent_SAR_ Global_2020&campaignid=7014N000001r&utm_campaign=Highly_Cited_Researchers_Parent_SAR_Global_2020&utm_source=earned_coverage&utm_ medium=press The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

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Publications Update

Editorial Board Appointments for ECS Journals

Graphical Abstracts Coming to ECS Journals The Electrochemical Society journals now accept graphical abstracts for inclusion with the online publication of papers. The goal is to facilitate browsing within the tables of contents and to encourage interdisciplinary research among the topical interest areas. Submitted graphics should present an easy-tocomprehend synopsis of the work reported in the article, allowing readers to easily identify papers relevant to their particular research interests, without providing the specific results or any conclusions reached. Ideally, the image should be a single snapshot of the research presented, which allows an expert in the field to understand the significance of the work while simultaneously encouraging the non-expert to read the paper. Graphical abstracts should be unique and designed for the purpose, rather than duplicating one of the images used within the paper itself. Submission of a graphical abstract is not required but is strongly encouraged. All submitted images are considered for inclusion during the peer-review process. Feedback is provided to the authors as required at the revision stage. For more information on submission of graphical abstracts, please visit the journals’ author instructions on the ECS site.

Journal of The Electrochemical Society Technical Editor Doron Aurbach has received a three-year reappointment as a technical editor for the Journal of The Electrochemical Society. Aurbach handles manuscripts related to batteries and energy storage. Aurbach is a professor at Bar-Ilan University (BIU), Department of Chemistry. He is also a member of the BIU Senate and director of the Energy Center at the Bar-Ilan University Institute of Nanotechnology and Advanced Materials (BINA). In addition, Aurbach is a leader of the Israel National Research Center for Electrochemical Propulsion (INREP). His research includes passivation phenomena, intercalation processes, and complex solution chemistry and the development of new analytical avenues, such as in situ spectroelectrochemical tools and hydrodynamic spectroscopy of composite surfaces on electrodes. His term will end on December 31, 2023.

Journal of The Electrochemical Society Associate Editor

ECS Transactions Celebrates Volume 100

UPCOMING

ECS Transactions (ECST), the official conference proceedings publication of The Electrochemical Society, recently celebrated its 100th volume. “IV Congreso Colombiano de Electroquímica (IVCCEQ2020)” takes the honor of Volume 100, Issue 1. Every volume of ECS Transactions features full-text content of proceedings from ECS meetings and ECS-sponsored meetings. ECST is a highquality venue for authors and an excellent resource for researchers. The papers appearing in ECST are reviewed to ensure that submissions meet generally accepted scientific standards. ECS Transactions volumes are available online through the ECS Digital Library. End users also can purchase instantly downloadable electronic (PDF) editions through the ECS Online Store.

April 7

Photo: North Carolina State University

Rajeev Kumar Gupta has received a two-year reappointment as an associate editor for the Journal of The Electrochemical Society. Gupta handles manuscripts related to corrosion science and technology. He is an associate professor at North Carolina State University, Department of Materials Science and Engineering. Gupta’s research group focuses on understanding corrosion initiation and propagation mechanisms, hightemperature oxidation, and structure-processingproperty-performance relationships. His term will end on December 31, 2022.

ECS WEBINAR SERIES

Physics of Dopant Emission to Harness the Rainbow Emission of Nanocrystals

Dr. Ranjani Viswanatha, Jawaharlal Nehru Centre for Advanced Scientific Research, India

April 21 The Development of New Ionic Electrolytes for Energy Storage Devices

Prof. Jenny Pringle, Deakin University, Australia

May 5

Dr. Kelsey Bridget Hatzell, Vanderbilt University, U.S.

Insight into Interfaces and Interphases in All Solid State Batteries

Visit electrochem.org/webinars to register 18

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

SOCIE T Y NE WS In the

Next Issue of

DID

YOU

KNOW?

• Summer 2021 Interface will spotlight the Corrosion Division. The issue will focus on High-Temperature Corrosion. According to Dev Chidambaram, the guest editor, high-temperature corrosion is an area attracting more interest due to increased durability demands for materials, especially due to the rapidly growing sustainable energy sector. Dev is a professor at the University of Nevada, Reno, Department of Materials Science and Engineering.

• Summer 2021 Interface also will include exclusive election coverage, 239th Meeting highlights, Free the Science Week results, and the recipients of ECS 2021 Summer Fellowships.

Summer 2021 Interface is scheduled to publish on June 25, 2021.

You can belong to more than one primary division! Join Additional Primary Divisions!

www.electrochem.org/divisions

Explore our PAT system for battery material research Strain, force and pressure measurements

3-electrode testing Battery test cells

Optical and XRD characterization

Long-term measurements

Potentiostats

Modular cell design

EIS

Control software

High throughput testing Adapters for third party cells

Cableless cell connection

+49 (0) 40 79012 734

Gas analysis

Electronic cell ID

sales@el-cell.com

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

www.el-cell.com 19

ECS Journals Current and Upcoming Focus Issues Journal of The Electrochemical Society (JES)

READ ONLINE International Meeting on Chemical Sensors (IMCS) 2020 – Volume One Technical Editor: Ajit Khosla Guest Editors: Peter Hesketh, Steve Semancik, Udo Weimar, Yasuhiro Shimizu, Joseph Stetter, Gary Hunter, Joseph Wang, Xiangqun Zeng, Sheikh Akbar, Muthukumaran Packirisamy, Rudra Pratap

NOW IN PRODUCTION Selected Papers of Invited Speakers to IMLB 2020 Technical Editor: Doron Aurbach Associate Editors: Thierry Brousse, Scott Donne, Brett Lucht, Venkat Srinivasan, Nae-Lih (Nick) Wu

Proton Exchange Membrane Fuel Cell & Proton Exchange Membrane Water Electrolyzer Durability Technical Editor: Xiao-Dong Zhou Guest Editors: Jean St-Pierre, Deborah Myers, Rodney Borup, Katherine Ayers

UPCOMING Solid Oxide Fuel Cells (SOFCs) and Electrolysis Cells (SOECs)

Characterization of Corrosion Processes in Honor of Philippe Marcus

Technical Editor: Xiao-Dong Zhou Guest Editors: Eric Wachsman, Subash Singhal Submissions Open: April 8, 2021 Deadline: July 29, 2021

Technical Editor: Gerald S. Frankel Guest Editors: Dev Chidambaram, Koji Fushimi, Vincent Maurice, Vincent Vivier

Molten Salts and Ionic Liquids II

18th International Meeting on Chemical Sensors (IMCS) – Volume Two

Technical Editor: Ajit Khosla Guest Editors: Peter Hesketh, Steve Semancik, Udo Weimar, Yasuhiro Shimizu, Joseph Stetter, Gary Hunter, Joseph Wang, Xiangqun Zeng, Sheikh Akbar, Muthukumaran Packirisamy, Rudra Pratap Submissions Open: May 6, 2021 Deadline: August 4, 2021

Modern Electroanalytical Research in the Society for Electroanalytical Chemistry (SEAC) Technical Editor: David Cliffel Guest Editors: Lane Baker, Lanqun Mao, Frank Zamborini, Bo Zhang Submissions Open: June 3, 2021 Deadline: September 1, 2021

Technical Editor: David Cliffel Guest Editors: David P. Durkin, Paul C. Trulove, Robert A. Mantz

Recent Advances in Chemical and Biological Sensors & Micro-Nanofabricated Sensors and Systems

Technical Editor: Ajit Khosla Guest Editors: Michael Adachi, Netz Arroyo, Thomas Thundat

Future of Intercalation Chemistry for Energy Storage and Conversion in Honor of M. Stanley Whittingham Technical Editor: Doron Aurbach Guest Editors: Brett Lucht, Louis Piper, Shirley Meng

Visit

www.electrochem.org/focusissues • Calls for upcoming JES and JSS focus issue papers • Links to published issues • Future focus issue proposals

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

ECS Journals Current and Upcoming Focus Issues ECS Journal of Solid State Science and Technology (JSS)

READ ONLINE

NOW IN PRODUCTION

Photovoltaics for the 21st Century

Solid State Reviews

Technical Editor: Ajit Khosla Contributing Technical Editors: Jennifer Bardwell, Francis D’Souza, Peter Mascher, Kailash C. Mishra, Fan Ren Associate Editors: Michael Adachi, Netz Arroyo, Thomas Thundat, Meng Tao Guest Editors: Sheng-Joue Young, Zhenhuan Zhao, Sandeep Arya, Sajjad Husain Mir, Kumkum Ahmed, MD Nahin Islam Shiblee

Technical Editor: Fan Ren Associate Editor: Meng Tao Guest Editors: Hiroki Hamada, Thad Druffel, Jae-Joon Lee

4D Materials and Systems + Soft Robotics

Technical Editor: Ajit Khosla Associate Editors: Michael Adachi, Netz Arroyo Guest Editors: Hidetmisu Furukawa, Koh Hosoda, Sheng-Joue Young, Zhenhuan Zhao, Tsukasa Yoshida, Yoon Hwa, Sathish K. Sukumaran, Masahiro Shimizu, Jessica E. Koehne

ACCEPTING SUBMISSIONS Solid State Electronic Devices and Materials

Photovoltaics for the 21st Century II

Selected Papers from the International Conference on Nanoscience and Nanotechnology 2021 (ICONN-2021)

Semiconductor Wafer Bonding: Science, Technology, and Applications

Technical Editor: Fan Ren Associate Editor: Meng Tao Guest Editors: Jae-Joon Lee, Doo-Hyun Ko, Yoonmook Kang, Hyeok Kim

Technical Editor: Fan Ren Guest Editors: Chao-Sung Lai, Chia-Ming Yang, Yu-Lin Wang Deadline: April 28, 2021

Technical Editor: Jennifer Bardwell Guest Editors: Roy Knechtel, Chuan Seng Tan, Tadatomo Suga, Helmut Baumgart, Frank Fournel, Mark Goorsky, Karl D. Hobart

Technical Editor: Francis D'Souza Guest Editors: Senthil Kumar Eswaran, S. Yuvaraj, M. S. Ramachandra Rao, Masaru Shimomura Deadline: May 5, 2021

UPCOMING

Molecular Electronics

Dedicated to the Memory of Professor George Blasse: Recent Developments in Theory, Materials and Applications of Luminescence

Technical Editor: Krishnan Rajeshwar Guest Editor: Jean Christophe Lacroix Deadline: June 2, 2021

Technical Editor: Kailash Mishra Guest Editors: John Collins, Jakoah Brgoch, Ron-Jun Xie, Eugeniusz Zych, Tetsuhiko Isobe, Ramchandra Pode, Andries Meijerink Deadline: July 28, 2021

Visit

www.electrochem.org/submit • JES manuscript submissions • JSS manuscript submissions

www.electrochem.org/focusissues The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

SOCIE T Y NE WS

New Division Officer Slates ECS Thanks 2020 Reviewers The Electrochemical Society relies upon the technical expertise and judgement of the many individuals who, as reviewers, help to maintain the high standards characteristic of the Society’s peerreviewed journals. In 2020, 3,523 individuals supported the Society’s long-standing commitment to ensuring both the technical quality of the works published, as well as the integrity and validity of the peer review the community provides. ECS greatly appreciates the time and effort put forth by these individuals, and the Society would like to express a sincere thank you for their hard work and support.

For a complete list of the 2020 viewers, visit the ECS Blog.

INSTITUTIONAL MEMBERSHIP PROGRAM

Institutional membership provides organizations the opportunity to support and advance the dissemination of electrochemical and solid state science research. Member organizations save 15-20% in spending through discounts on ECS subscriptions, meeting registrations, marketing opportunities, and are able to provide ECS membership benefits to their employees.

New division officers for the spring 2021-spring 2023 term have been nominated for the following divisions. All election results will be reported in the summer 2021 issue of Interface. Electronics and Photonics

Chair Jennifer Hite, Naval Research Laboratory Vice-Chair Qiliang Li, George Mason University 2nd Vice-Chair Vidhya Chakrapani, Rensselaer Polytechnic Institute Secretary Zia Karim, Yield Engineering Systems Treasurer Erica A. Douglas, Sandia National Laboratories Energy Technology

Chair William Mustain, University of South Carolina Vice-Chair Katherine Ayers, Nel Hydrogen Secretary Minhua Shao, The Hong Kong University of Science and Technology Treasurer Ahmet Kusoglu, Lawrence Berkeley National Laboratory Hui Xu, Giner, Inc. Iryna Zenyuk, University of California at Irvine Organic and Biological Electrochemistry

Chair Sadagopan Krishnan, Oklahoma State University Vice-Chair Song Lin, Cornell University Secretary/Treasurer Jeffrey M. Halpern, University of New Hampshire Physical and Analytical Electrochemistry

Chair Andrew Hillier, Iowa State University Vice-Chair Stephen Paddison, University of Tennessee Knoxville Secretary Anne Co, Ohio State University Treasurer Svitlana Pylypenko, Colorado School of Mines

Contact Anna.Olsen@electrochem.org to learn more about institutional membership benefits.

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

SOCIE T Y NE WS

ECS Division Contacts High-Temperature Energy, Materials, & Processes

Battery

Y. Shirley Meng, Chair University of California San Diego shirleymeng@ucsd.edu • 858.822.4247 (U.S.)

Paul Gannon, Chair Montana State University pgannon@montana.edu • 406.994.7380 (U.S.)

Brett Lucht, Vice-Chair Jie Xiao, Secretary Jagjit Nanda, Treasurer Doron Aurbach, Journals Editorial Board Representative

Sean Bishop, Sr. Vice-Chair Cortney Kreller, Jr. Vice-Chair Xingbo Liu, Secretary/Treasurer Raymond Gorte, Journals Editorial Board Representative

Corrosion

James Noël, Chair University of Western Ontario jjnoel@uwo.ca • 519.661.2111, ext. 88029 (CA) Dev Chidambaram, Vice-Chair Eiji Tada, Secretary/Treasurer Gerald Frankel, Journals Editorial Board Representative Dielectric Science and Technology

Peter Mascher, Chair McMaster University mascher@mcmaster.ca • 905.525.9140, ext. 24963 (U.S.) Uros Cvelbar, Vice-Chair Sreeram Vaddiraju, Secretary Zhi David Chen, Treasurer Peter Mascher, Journals Editorial Board Representative Electrodeposition

Industrial Electrochemistry and Electrochemical Engineering

Shrisudersan Jayaraman, Chair Corning Incorporated jayaramas@corning.com • 607.974.9643 (U.S.) Maria Inman, Vice-Chair Paul Kenis, Secretary/Treasurer John Harb, Journals Editorial Board Representative Luminescence and Display Materials

Jakoah Brgoch, Chair University of Houston jbrgoch@central.uh.edu • 713.743.6233 (U.S.) Rong-Jun Xie, Vice-Chair Eugeniusz Zych, Secretary/Treasurer Kailash Mishra, Journals Editorial Board Representative Nanocarbons

Philippe Vereecken, Chair IMED philippe.vereecken@imec.be • +32.4.741.73.110 (BE)

Hiroshi Imahori, Chair Kyoto University imahori@scl.kyoto-u.ac.jp • +81.75.383.2566 (JP)

Vasiljevic Natasa R., Vice-Chair Luca Magagnin, Secretary Andreas Bund, Treasurer Takayuki Homma, Journals Editorial Board Representative

Jeffrey Blackburn, Vice-Chair Ardemis Boghossian, Secretary Slava V. Rotkin, Treasurer Francis D’Souza, Journals Editorial Board Representative

Electronics and Photonics

Organic and Biological Electrochemistry

Junichi Murota, Chair Tohoku University murota@riec.tohoku.ac.jp • +81.22.217.3913 (JP)

Diane Smith, Chair San Diego State University dksmith@mail.sdsu.edu • 619.594.4839 (U.S.)

Yu-Lin Wang, Vice-Chair Jennifer Hite, 2nd Vice-Chair Qiliang Li, Secretary Robert Lynch, Treasurer Fan Ren, Journals Editorial Board Representative Jennifer Bardwell, Journals Editorial Board Representative

Sadagopan Krishnan, Vice-Chair Song Lin, Secretary/Treasurer Janine Mauzeroll, Journals Editorial Board Representative

Energy Technology

Vaidyanathan Subramanian, Chair University of Nevada Reno ravisv@unr.edu • 775.784.4686 (U.S.) William Mustain, Vice-Chair Katherine Ayers, Secretary Minhua Shao, Treasurer Xiao-Dong Zhou, Journals Editorial Board Representative

Physical and Analytical Electrochemistry

Petr Vanýsek, Chair Northern Illinois University pvanysek@gmail.com • 815.753.1131 (U.S.) Andrew Hillier, Vice-Chair Stephen Paddison, Secretary Anne Co, Treasurer David Cliffel, Journals Editorial Board Representative Sensor

Jessica Koehne, Chair NASA Ames Research Center jessica.e.koehne@nasa.gov • 650.604.6818 (U.S.) Larry Nagahara, Vice-Chair Praveen Kumar Sekhar, Secretary Dong-Joo Kim, Treasurer Ajit Khosla, Journals Editorial Board Representative

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

SOCIE T Y NE WS

Staff News Early this year, ECS said goodbye to a respected, cherished colleague, Beth Craanen. After six outstanding years with the Society, Beth has moved on to an exciting new position. In her time with ECS, Beth had an enormous impact, beginning in Membership, and for the past few years in Publications. Most notably, Beth was instrumental in ensuring the smooth transition of our digital library and subscription sales to IOP, an effort upon which much of our current and future success is poised. While Beth will no longer be with us, and she will undoubtedly be missed, her work will have value lasting far beyond her tenure. Congratulations and best wishes for your continued success, Beth!

Be the Next Leader Contact Anna.Olsen@electrochem.org to inquire about the benefits of institutional membership for your organization.

For more information you also can visit:

www.electrochem.org/leadership-circle

Publisher’s Notes In the summer 2020 issue of Interface, the authors (Suzanne Witt, Nick Rancis, Mary Ensch, and Vanessa Maldonado) would like to point out errors in the feature “Electrochemical Destruction of ‘Forever Chemicals’: The Right Solution at the Right Time.” The acronym PFBA is incorrectly defined as pentafluorobenzoic acid in the caption for Fig. 5 (p. 74) and in the Conclusions and Outlook section (p. 75). It should be noted that the correct chemical name for PFBA is perfluorobutanoic acid. In the winter 2020 issue of Interface, the authors (Wuxiang Feng, Wei Wu, Congrui Jin, and Dong Ding) would like to point out a missing acknowledgement in the feature “Manufacturing Techniques of Thin Electrolyte for Planar Solid Oxide Electrochemical Cells.” The text should read: “This work is supported by the U.S. Department of Energy (USDOE), Office of Energy Efficiency and Renewable Energy (EERE), Hydrogen and Fuel Cell Technologies Office (FCTO), Technology Acceleration under DOE Idaho Operations Office under contract DE-AC07-05ID14517. Congrui Jin would like to acknowledge a subcontract from Idaho National Laboratory.” ECS regrets these errors.

INTERESTED IN PUBLISHING WITH ECS? Visit the ECS website to learn more about the book publishing process, information on preparing a proposal, and helpful advice on how to get your book published. Questions? If you have questions or are ready to take the next step, reach out to ECS staff at publications@electrochem.org.

UPCOMING ECS SPONSORED MEETINGS In addition to the ECS biannual meetings and ECS satellite conferences, ECS, its divisions, and sections sponsor meetings and symposia of interest to the technical audience ECS serves. The following is a partial list of upcoming sponsored meetings. Please visit the ECS website (www.electrochem.org/upcoming-meetings) for a list of all sponsored meetings.

2021 • 18th International Meeting on Chemical Sensors (IMCS), with the 239th ECS Meeting May 30-June 3, 2021, Digital Meeting https://imcs2021.gatech.edu • The 17th International Symposium on Solid Oxide Fuel Cells (SOFC-XVII) July 18-23, 2021, Digital Meeting www.electrochem.org/sofc-xvii

To learn more about what an ECS sponsorship could do for your meeting, including information on publishing proceeding volumes for sponsored meetings, or to request an ECS sponsorship of your technical event, please contact ecs@electrochem.org.

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

SOCIE T Y NE WS

Websites of Note Suggested for you by Alice Suroviec.

Open Textbook Library

MERLOT

Host: University of Minnesota Site: https://open.umn.edu/opentextbooks

Host: California State University Site: https://www.merlot.org

The Open Textbook Library is part of the Open Education Network, located at the University of Minnesota. These are textbooks written by authors with open licenses. This means that textbooks can be downloaded and edited by endusers. There are many peer-reviewed engineering textbooks available. This is an excellent starting point for those looking to learn more about introductory topics.

Multimedia Educational Resource for Learning and Online Training (MERLOT) is a community working together to provide users with open educational resources (OER) teaching and learning materials. The system features video tutorials, a website building platform, and a content builder. MERLOT’s peer-reviewed content is free for all users.

BCcampus Open Ed

OpenStax

Host: BCcampus Site: https://open.bccampus.ca/

Host: Rice University Site: https://openstax.org/

The focus of BCcampus Open Ed is to support the postsecondary institutions of British Columbia as they adopt, adapt, and evolve their teaching and learning practices to create a better experience for students. These resources are available to access, develop, research, and explore opportunities to improve the learning experience for all students. These resources are available to those not just in British Columbia but are truly open access. This website has access to many textbooks on the subjects of engineering, chemistry, and physics.

OpenStax is part of Rice University, which is a 501(c)(3) nonprofit charitable corporation. As such, through partnerships with philanthropic foundations and alliances with other educational companies, they are able to provide free, opensource, peer-reviewed textbooks that are available in a variety of formats (online, PDF, print.) There are several excellent introductory books on engineering topics, as well as many other subjects. For those looking for a textbook on a subject, this is a great place to start.

Alice Suroviec is a professor of bioanalytical chemistry and dean of the College of Mathematical and Natural Sciences at Berry College. She earned a BS in chemistry from Allegheny College in 2000. She received her PhD from Virginia Tech in 2005 under the direction of Dr. Mark R. Anderson. Her research focuses on enzymatically modified electrodes for use as biosensors. She is currently associate editor of the PAE Technical Division for the Journal of The Electrochemical Society. She can be reached at asuroviec@berry.edu and is always looking for new app/website suggestions. https://orcid.org/0000-0002-9252-2468 The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

239th ECS Meeting 239TH ECS MEETING WITH IMCS 18 • May 30-June 3, 2021

DIGITAL MEETING May 30-June 3, 2021

oin us at this international meeting and share electrochemistry- and solid state science-related research and issues with academic, industry, and government scientists, engineers, and researchers. Absorb and exchange information on the latest scientific developments across a variety of interdisciplinary areas in a forum of peers sharing a unique knowledge base and experience. In light of the COVID-19 pandemic, this year’s spring meeting with over 2,000 technical talks across 53 symposia—including the 18th International Meeting on Chemical Sensors (IMCS)—is completely digital. Presenters have been asked to submit digital presentation files for viewing as part of the digital meeting. To further our vision of open access to science, the Society is pleased to again offer our global community no-cost registration. Everyone is welcome to participate!

Registration Access to technical presentations is available to the entire global community, greatly expanding the potential audience who can see, hear, and experience the meeting’s outstanding content. Registration, which is required to participate, is complimentary.

Technical Presentations Presenting authors submit digital presentation files (video, and/or slide deck or poster) in advance of the meeting. These materials are available on-demand from May 30-June 26, 2021.

Live Symposia Sessions These sessions showcase live technical talks by invited and contributing speakers offering opportunities for participants to ask questions.

Special Events In addition to the robust on-demand technical program and live symposia sessions, join us for live broadcast special talks and events including the Opening Ceremony, ECS Plenary Lecture, award ceremonies, and more.

Exhibitors and Sponsors The digital meeting allows participants to interact with important partners including exhibitors. During your online meeting experience, visit the Digital Exhibit and Vendor (DEV) Guide. Thank you to the generous support from our meeting sponsors, digital exhibitors, and symposium sponsors!

Proceedings Publication and ECS Journals The Society publishes proceeding papers from selected symposia in ECS Transactions. To purchase or download the content, visit www.electrochem.org/239/transactions. All presenters are invited and encouraged to submit their publication to ECS’s prestigious journals—the Journal of The Electrochemical Society or the Journal of Solid State Science and Technology.

18th International Meeting on Chemical Sensors (IMCS) ECS appreciates the 18th IMCS meeting joining us for this shared meeting! As a special bonus, participants of the ECS and IMCS meetings can attend both meetings’ sessions. See page 30 for more information on IMCS.

The ECS Lecture Monday, May 31

“Carbon Material”

Rodney S. Ruoff, Ulsan National Institute of Science & Technology (UNIST) Rodney S. Ruoff is a Distinguished Professor in the Departments of Chemistry and Materials Photo: UNIST Science, and the School of Energy Science and Chemical Engineering, at the Ulsan National Institute of Science and Technology (UNIST), South Korea. He serves as Director of the Center for Multidimensional Carbon Materials (CMCM), an Institute for Basic Science at UNIST. From 2007 until he joined UNIST in 2014, Prof. Ruoff was the Cockrell Family Regents Endowed Chair Professor at the University of Texas at Austin, U.S. He earned his PhD in Chemical Physics from the University of Illinois-Urbana, U.S., in 1988, and was a Fulbright Fellow in 19881989 at the Max-Planck-Institut für Strömungsforschung, Germany. At Northwestern University, U.S., in 2007, Prof. Ruoff was the John Evans Professor of Nanoengineering and Director of the Biologically Inspired Materials Institute. The Electrochemical Society Fullerenes Group—now known as the Nanocarbons Division—was founded in 1993 with Prof. Ruoff as Chairman and Karl M. Kadish as Vice-Chair. Prof. Ruoff is a Fellow of the Materials Research Society, American Physical Society, American Association for the Advancement of Science, and Royal Society of Chemistry. He received the American Physics Society’s James C. McGroddy Prize for New Materials (2018), American Carbon Society SGL Skakel Award (2016), and Materials Research Society Turnbull Prize (2014). Prof. Ruoff has authored or coauthored some 500 peer-reviewed publications related to chemistry, physics, materials science, mechanics, and biomedical science. Clarivate Analytics named Prof. Ruoff a Citation Laureate for many years. He has been a Highly Cited Researcher in Chemistry, Physics, and Materials Science since such statistics have been reported.

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Award-Winning Speakers

(Check the online program for further information.)

239TH ECS MEETING WITH IMCS 18 • May 30-June 3, 2021

SOCIETY AWARD WINNING SPEAKERS Hiroshi Iwai, Tokyo Institute of Technology Gordon E. Moore Award

Marc Koper, Leiden University Allen J. Bard Award

DIVISION AWARD WINNING SPEAKERS Bryan Pivovar, National Renewable Energy Laboratory Energy Technology Division Research Award Lisa Housel, Stony Brook University Energy Technology Division Graduate Student Award Sponsored by BioLogic Charles Wan, Massachusetts Institute of Technology Energy Technology Division Graduate Student Award Sponsored by BioLogic Iryna Zenyuk, University of California, Irvine Energy Technology Division Supramaniam Srinivasan Young Investigator Award

Andreas Hirsch, Friedrich-Alexander-Universität Erlangen-Nürnberg Nanocarbons Division Robert C. Haddon Research Award Markita Landry, University of California at Berkeley Nanocarbons Division SES Young Investigator Award Siegfried R. Waldvogel, Johannes Gutenberg Universität Mainz Organic and Biological Electrochemistry Division Manuel M. Baizer Award Bruce Parkinson, University of Wyoming Physical and Analytical Electrochemistry Division David C. Grahame Award

Eric Mcshane, University of California, Berkeley Industrial Electrochemistry and Electrochemical Engineering Division Student Achievement Award

www.electrochem.org/239

Akshay Subramaniam, University of Washington Industrial Electrochemistry and Electrochemical Engineering Division H. H. Dow Memorial Student Achievement Award

The 17th International Symposium on Solid Oxide Fuel Cells (SOFC-XVII) Sponsored by

High-Temperature Energy, Materials, & Processes Division of The Electrochemical Society, Inc. and The SOFC Society of Japan

DIGITAL MEETING July 18-23, 2021

Registration is open!

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Symposium Topics and Organizers A0A—Batteries and Energy Storage

C— Corrosion Science and Technology

239TH ECS MEETING WITH IMCS 18 • May 30-June 3, 2021

A01—A01 - New Approaches and Advances in Electrochemical Energy Systems Sri Narayan, Mani Manivannan, Hui Xu, Wu Xu Energy Technology, Battery

C01—Corrosion General Session James Noel, Dev Chidambaram Corrosion

A02—Lithium Ion Batteries Chunmei Ban, Jun Lu, Gary Koenig, Ruhul Amin Battery

D01—Chemical Mechanical Polishing 16 Robert Rhoades, Gul Basim, Yaw Obeng, Vimal Chaitanya, Gautam Banerjee Dielectric Science and Technology

A03—Large Scale Energy Storage 12 Trung Nguyen, Daniel Steingart, Bin Li, Wei Wang, Walter van Schalkwijk Energy Technology, Battery, Industrial Electrochemistry and Electrochemical Engineering A04—Battery Student Slam 5 Jie Xiao, Minghao Zhang, Zachary Hood Battery A05—Battery Safety and Failure Modes 3 Boryann (Bor Yann) Liaw, Taylor Garrick, Walter van Schalkwijk Battery, Energy Technology, Industrial Electrochemistry and Electrochemical Engineering A06—Next Generation Batteries John Vaughey, Nian Liu, Joshua Gallaway Battery A07—Ion Coordination and Dynamics in Battery Electrolytes, Interfaces and Interphases Jordi Cabana, Joaquín Rodríguez-López, George Crabtree, Kristin Persson, Kang Xu, Nitash Balsara, Vito Di Noto Battery B—Carbon Nanostructures and Devices B01—Carbon Nanostructures for Energy Conversion and Storage Jeff Blackburn, Vito Di Noto, Plamen Atanassov, Min-Kyu Song, Michael Arnold, David Cliffel, Christina Bock, Xiulei (David) Ji Nanocarbons, Battery, Energy Technology B02—Carbon Nanostructures in Medicine and Biology Daniel Heller, Hiroshi Imahori, Tatiana Da Ros, Fotios Papadimitrakopoulos, Ardemis Boghossian, Mekki Bayachou, James Burgess, Larry Nagahara Nanocarbons, Organic and Biological Electrochemistry, Sensor B03—Carbon Nanotubes - From Fundamentals to Devices Ming Zheng, Pawel Kulesza, Slava Rotkin, R. Bruce Weisman, Shigeo Maruyama, Benjamin Flavel, Yan Li Nanocarbons B04—NANO in La Francophonie Richard Martel, Christophe Voisin, M.J. Nierengarten, Annick Loiseau, Jean-Christophe Charlier, Jeff Blackburn, Hiroshi Imahori, Slava Rotkin, Delphine Bouilly, Thomas Szkopek, Laurent Cognet, Ardemis Boghossian Nanocarbons, Sensor B05—Fullerenes - Endohedral Fullerenes and Molecular Carbon Shangfeng Yang, Alan Balch, Francis D’Souza, Luis Echegoyen, Dirk Guldi, Nazario Martin, Steven Stevenson Nanocarbons B06—2D Layered Materials from Fundamental Science to Applications Michael Arnold, Yaw Obeng, Stefan De Gendt, Z. Karim, Colm O’Dwyer, Slava Rotkin, Vito Di Noto Nanocarbons, Dielectric Science and Technology, Energy Technology, Interdisciplinary Science and Technology Subcommittee B07—Light Energy Conversion with Metal Halide Perovskites, Semiconductor Nanostructures, and Inorganic/Organic Hiroshi Imahori, Prashant Kamat, Kei Murakoshi, Vito Di Noto, Tsukasa Torimoto, Masako Kato Nanocarbons B08—Porphyrins, Phthalocyanines, and Supramolecular Assemblies Karl Kadish, Roberto Paolesse, Tomas Torres, Nathalie Solladie, Diane Smith, Norbert Jux Nanocarbons

D—Dielectric Science and Materials

D02—Plasma and Thermal Processes for Materials Modification, Synthesis, and Processing 3 Thorsten Lill, Mahendra Sunkara, Peter Mascher, Uros Cvelbar, Dennis Hess, Oana Leonte, Sreeram Vaddiraju Dielectric Science and Technology, High-Temperature Energy, Materials, & Processes, Sensor D03—Plasma Electrochemistry and Catalysis Mohan Sankaran, Mahendra Sunkara, Richard Van De Sanden, Uros Cvelbar, Davide Mariotti Dielectric Science and Technology D04—Quantum Dot Science and Technology Dong-Kyun Ko, Davide Mariotti, Vladimir Svrcek, Soong Ju Oh Dielectric Science and Technology E—Electrochemical/Electroless Deposition E02

Electrodeposition as Enabler of (other) Electrochemical Processes and Devices Giovanni Zangari, Yasuhiro Fukunaka, Thomas Moffat, Elizabeth Podlaha, Natasa Vasiljevic, Daniel Schwartz Electrodeposition, Battery

F—Electrochemical Engineering F01—Advances in Industrial Electrochemistry and Electrochemical Engineering Douglas Riemer, John Staser, Hui Xu Industrial Electrochemistry and Electrochemical Engineering F03—Characterization of Porous Materials 9 John Staser, Iryna Zenyuk, Sri Narayan, Vito Di Noto Industrial Electrochemistry and Electrochemical Engineering, Energy Technology F04—Multiscale Modeling, Simulation, and Design 4: Enhancing Understanding and Extracting Knowledge from Data Venkat Subramanian, John Harb, Shawn Litster, Scott Calabrese Barton Industrial Electrochemistry and Electrochemical Engineering, Energy Technology G—Electronic Materials and Processing G01—Silicon Compatible Emerging Materials, Processes, and Technologies for Advanced CMOS and Post-CMOS Applications 11 Hemanth Jagannathan, Kuniyuki Kakushima, Paul Timans, Zia Karim, Evgeni Gousev, Stefan De Gendt, Durga Misra, Yaw Obeng, Fred Roozeboom Electronics and Photonics, Dielectric Science and Technology G02—Processes at the Semiconductor Solution Interface 9 Colm O’Dwyer, D. Noel Buckley, Arnaud Etcheberry, Andrew Hillier, Robert Lynch, Philippe Vereecken, Vidhya Chakrapani, Heli Wang Electronics and Photonics, Dielectric Science and Technology, Electrodeposition, Physical and Analytical Electrochemistry G03—Organic Semiconductor Materials, Devices, and Processing 8 Benjamin Iniguez, M. Jamal Deen, Hagen Klauk, David Gundlach, Sunghwan Lee, Zhi Chen Electronics and Photonics, Dielectric Science and Technology H—Electronic and Photonic Devices and Systems H01—Wide Bandgap Semiconductor Materials and Devices 22 Vidhya Chakrapani, Jennifer Hite, John Zavada, Travis Anderson, Marko Tadjer, Steve Kilgore Electronics and Photonics H02—High Purity and High Mobility Semiconductors 16 Eddy Simoen, Oleg Kononchuk, Osamu Nakatsuka, Cor Claeys Electronics and Photonics

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

I—Fuel Cells, Electrolyzers, and Energy Conversion I01—Ionic and Mixed Conducting Ceramics 13: Symposium in Honor of Anil Virkar Xiao-Dong Zhou, Turgut Gur, Tatsuya Kawada, Dong Ding, Venkataraman Thangadurai, Karen Swider-Lyons, Mani Manivannan High-Temperature Energy, Materials, & Processes, Battery, Energy Technology I02—Hydrogen or Oxygen Evolution Catalysis for Water Electrolysis 7 Hui Xu, Joshua Spurgeon, Elizabeth Podlaha, Santosh Vijapur, Andrew Herring, Peter Pintauro, Plamen Atanassov, Lauren Greenlee, Jingyi Chen Energy Technology, Electrodeposition, Industrial Electrochemistry and Electrochemical Engineering I03—Renewable Fuels via Artificial Photosynthesis or Heterocatalysis 6 Nianqiang Nick Wu, Bunsho Ohtani, Pawel Kulesza, Eric Miller, Vaidyanathan Subramanian, Mani Manivannan, Dongling Ma, Gary Wiederrecht, Tianquan Lian, Scott Cushing, Heli Wang, Jae-Joon Lee, Frank Osterloh Energy Technology I04—Energy Conversion Systems Based on Nitrogen 4 Gang Wu, Hui Xu, Shelley Minteer, Katherine Ayers, Julie Renner, Lauren Greenlee, Cortney Kreller Energy Technology, High-Temperature Energy, Materials, & Processes, Industrial Electrochemistry and Electrochemical Engineering, Physical and Analytical Electrochemistry K—Organic and Bioelectrochemistry K01—Advances in Organic and Biological Electrochemistry 2: In Memory of Dennis Peters Diane Smith, Flavio Maran, Scott Calabrese Barton, Mekki Bayachou, Alice Suroviec, Song Lin Organic and Biological Electrochemistry, Energy Technology K02—Pharmaceutical Organic and Biological Electrochemistry Sadagopan Krishnan, Shelley Minteer, John Staser, Matthew Graaf, Mekki Bayachou Organic and Biological Electrochemistry, Industrial Electrochemistry and Electrochemical Engineering L—Physical and Analytical Electrochemistry, Electrocatalysis, and Photoelectrochemistry L01—Physical and Analytical Electrochemistry, Electrocatalysis, and Photoelectrochemistry General Session and Grahame Award Symposium Andrew Hillier, Petr Vanysek, Katie Li-Oakey, Justin Sambur, Stephen Paddison Physical and Analytical Electrochemistry L02—Electrocatalysis 11 Gessie Brisard, Plamen Atanassov, Minhua Shao, Gang Wu, Anne Co, Svitlana Pylypenko, Sanjeev Mukerjee Physical and Analytical Electrochemistry, Energy Technology L06—Nanostructured Functional Materials for Electrochemistry Pawel Kulesza, Hiroki Habazaki, Plamen Atanassov, Vito Di Noto, Iwona Rutkowska, Brian Skinn, Andrew Herring Physical and Analytical Electrochemistry, Energy Technology

Z—General Z01—General Student Poster Session Alice Suroviec, Vimal Chaitanya, Andrew Herring, Kalpathy Sundaram All Divisions Z02—COVID-19 and Pathogen Related Research, Development, and Engineering in Sensors and Systems - A Joint Symposium of ECS and IMCS Peter Hesketh, Uros Cvelbar, Plamen Atanassov, Sadagopan Krishnan, Durga Misra, Xiangqun Zeng, Gary Hunter, Angela Ervin, Daniel Heller, Joseph Stetter Sensor, Dielectric Science and Technology, Energy Technology, Nanocarbons, Organic and Biological Electrochemistry

18th International Meeting on Chemical Sensors (IMCS) IMCS 01—Artificial Intelligence, Machine Learning, Chemometrics, and Sensor Arrays Kevin Johnson, Lok-kun Tsui, Jian-Hui Jiang Sensor IMCS 02—Chemical and Biosensors, Medical/Health, and Wearables Nianqiang Nick Wu, Larry Nagahara, Chenzhong Li, Hong Zhou, Leyla Soleymani, Joseph Wang, Wei-Hua Huang, Sadagopan Krishnan, Ajit Khosla Sensor IMCS 03—Electrochemical and Metal Oxide Sensors Sheikh Akbar, Joseph Stetter, Nosang Myung, Lili Deligianni, Jong-Heun Lee, Geyu Lu Sensor IMCS 04—Sensors for Agricultural and Environmental Applications Ramaraja Ramasamy, Bryan Chin, Aicheng Chen, Xing-Jiu Huang, Pengyu Chen, Wenzhuo Wu Sensor IMCS 05—Recent Advances and Future Directions in Chemical and Bio Sensor Technology and Networked Systems Gary Hunter, Guobao Xu, Joseph Stetter, Wenzhuo Wu, Jin-Woo Choi, Praveen Kumar Sekhar, Ajit Khosla, Vimal Chaitanya Sensor, Dielectric Science and Technology IMCS 06—MEMS/NEMS, FET Sensors, and Resonators Peter Hesketh, Petr Vanysek, Thomas Thundat, Farrokh Ayazi, Eric Vogel, Ajit Khosla Sensor Division; Physical and Analytical Electrochemistry Division IMCS 07—Microfluidic Devices and Sensors Jessica Koehne, Sushanta Mitra, Ingrid Fritsch, Marc Madou, Ajit Khosla Sensor; Physical and Analytical Electrochemistry IMCS 08—Optical Sensors, Plasmonics, Chemiluminescent, and Electrochemiluminescent Sensors Guoobao Xu, Jing Zhao, Muthukumaran Packirisamy, Uros Cvelbar, Huan-Tsung Chang, Ming Li, Zhifeng Ding, Giovanni Valenti Sensor, Dielectric Science and Technology IMCS 09—Sensors for Breath Analysis, Biomimetic Taste, and Olfaction Sensing Peter Hesketh, Dong-Joo Kim, Perena Gouma Sensor IMCS 10—Chemical and Biosensing Materials and Sensing Interface Design Xiangqun Zeng, Xi Chen, Osamu Niwa Sensor

L07—Complex and Dynamic Electrochemical Systems Raphael Nagao, Istvan Kiss Physical and Analytical Electrochemistry, Energy Technology L08—Electrochemical Studies by Synchrotron Techniques Anne Co, Svitlana Pylypenko, Iryna Zenyuk, Ahmet Kusoglu, Johanna Weker, Deborah Myers Physical and Analytical Electrochemistry, Energy Technology

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

239TH ECS MEETING WITH IMCS 18 • May 30-June 3, 2021

H04—Wearable and Flexible Electronic and Photonic Technologies 3 Luyao Lu, Yu-Lun Chueh, Jong Hyun Ahn, Sang-Woo Kim, Jessica Koehne, Ajit Khosla, Wei Gao, Durga Misra, Shelley Minteer, Scott Calabrese Barton, Lain-Jong Li, Colm O’Dwyer Electronics and Photonics, Dielectric Science and Technology, Energy Technology, Physical and Analytical Electrochemistry, Sensor, Interdisciplinary Science and Technology Subcommittee

18th International Meeting on Chemical Sensors (IMCS) 239TH ECS MEETING WITH IMCS 18 • May 30-June 3, 2021

DIGITAL MEETING May 30-June 3, 2021

18th

he North America, Asia, and Europe Committees for the International Meeting on Chemical Sensors invite you to IMCS, being held digitally in May 2021. This is the 18th in a series of successful meetings for researchers, professionals, and business leaders to view the state of the art in sensors for gases, liquids, biologicals, for applications in health and environment, wearables and fixed infrastructure, as well as wired and wireless. Chemical and biosensors for gases, vapors, and liquids are becoming more critical due to recent developments in changing weather patterns and the impact of greenhouse gases and their adverse effects on the environment. We anticipate sweeping changes to the application of sensors to air quality monitoring, food safety, and water quality in the near future. Sensor technology is also widely applied to human medical diagnostics and health and fitness monitoring. The demand for environment sensing and development of sensor technology to determine the effects on human and animal health are critically important. This is an opportunity to participate in the revolution that is taking place in sensor technology leading to new monitoring and sensing systems connected to the Internet of Things.

Symposium Topics • Artificial Intelligence, Machine Learning, Chemometrics, and Sensor Arrays • Chemical and Biosensors, Medical/Health, and Wearables • Electrochemical and Metal Oxide Sensors • Sensors for Agricultural and Environmental Applications • Recent Advances and Future Directions in Chemical and Bio Sensor Technology and Networked Systems • MEMS/NEMS, FET Sensors, and Resonators

• Microfluidic Devices and Sensors • Optical Sensors, Plasmonics, Chemiluminescent, and Electrochemiluminescent Sensors • Sensors for Breath Analysis, Biomimetic Taste, and Olfaction Sensing • Chemical and Biosensing Materials and Sensing Interface Design • COVID-19 and Pathogen Related Research, Development, and Engineering in Sensors and Systems

Plenary Speakers

(Check the online program for further information.)

“Rational Design of Oxide Chemiresistors for Next-Generation Gas Sensors and Artificial Olfaction” Jong-Heun Lee, Korea University

Jong-Heun Lee has been Professor in the Department of Materials Science and Engineering, Korea University, since 2003. His research interests include semiconductor gas sensors and functional oxide nanostructures. He received his BS, MS, and PhD from the Department of Inorganic Materials and Engineering, Seoul National University, Seoul, South Korea, in 1987, 1989, and 1993, respectively. As Senior Researcher at the Samsung Advanced Institute of Technology from 1993 and 1999, he developed automotive airfuel-ratio sensors. He was a Society of Technical Analysts Fellow at the National Institute for Research in Inorganic Materials (currently NIMS, Tsukuba, Japan) from 1999 to 2000, and a research professor at Seoul National University from 2000 to 2003. He is an editor of Sensors and Actuators B: Chemical, Fellow member of the Korean Academy of Science and Technology, and general member of the National Academy of Engineering of Korea. In 2014, he was honored as a Highly Cited Researcher by Thomson Reuters for ranking in the top 1 percent most cited papers. He has won numerous awards including the POSCO TJ Award (2017), Knowledge Creation Award (2014), 100 Future-Leading Technologies and Their Developers (2013), Korean Sensor Society Academic Award (2016), Korea University Special Award for Distinguished Research (2014), and Patent of the Year (2001). He was co-chairman of the International Meeting on Chemical Sensors 2016, Jeju, Korea. He has published 305 peer-reviewed papers and holds 40 domestic and international patents. 30

“Wearable Sensors for Monitoring Chemical Markers: Beyond Steps and Vitals” Joseph Wang, University of California, San Diego

Joseph Wang is SAIC Endowed Chair and Distinguished Professor in the Department of Nanoengineering at the University of California, San Diego (UCSD), U.S. He is also Director of the UCSD Center of Wearable Sensors and Founding Editor of Electroanalysis. He served as Chair of the Department of Nanoengineering (20142019) and Director of the Center for Bioelectronics at Arizona State University, U.S. (ASU, 2004-2008). Prof. Wang has made pioneering contributions to wearable biosensors, electrochemical devices, nanomachines, and nanobioelectronics. He has published more than 1,060 papers, 11 books, and holds 30 patents. His publications have been cited over 107,000 times; his h-index is 160. He was an ISI Thomson Reuters Highly Cited Researcher in Chemistry and Engineering from 2014-2019. Prof. Wang received numerous national ECS, American Chemical Society, and Society for Electroanalytical Chemistry awards in instrumentation and electrochemistry, 10 honorary professorships around the globe, and Medals of Honor from the United Kingdom, Australia, and Czech Republic. He is a Fellow of The Electrochemical Society, Royal Society of Chemistry, and of the American Institute of Medical and Biological Engineering. Prof. Wang has guided over 300 PhD students and postdoc fellows.

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Special Events

(Check the online program for further information.)

These sessions showcase live technical talks by invited and contributing speakers across all IMCS symposia, and offer opportunities for speaker and topical Q&A.

Sponsors Forum Invited presenters from funding organizations and government agencies provide their perspective on current programs and strategies for securing funding and sustaining research activities on chemical and biosensors at universities and other institutions.

“Electrochemical/Optical Sensors in Medicine: Meeting Needs for the 21st Century” Mark E. Meyerhoff, University of Michigan

Mark E. Meyerhoff is currently Philip J. Elving Professor of Chemistry in the Department of Chemistry at the University of Michigan (U of M). He received his PhD from the State University of New York at Buffalo, U.S., in 1979, working with Prof. Garry A. Rechnitz. Following a short postdoctoral at the University of Delaware, U.S., he joined U of M as Assistant Professor in the fall of 1979. Prof. Meyerhoff’s primary research interests are in the field of analytical chemistry, particularly the development of new ion-, polyion-, gas-, and bio-selective electrochemical/optical sensors suitable for direct measurements of clinically important analytes in physiological samples. He also has a very active research program in the area of biomaterials, especially the development and characterization of novel nitric oxide (NO) releasing/generating polymeric materials. Since beginning his independent academic career at U of M, he and his collaborators have authored more than 380 original research papers on these and other topics. Meyerhoff received the Ralph Adams Award in Bioanalytical Chemistry from the Pittsburgh Conference on Analytical Chemistry (2014), U of M Distinguished Faculty Achievement Award (2011), Society for Electroanalytical Chemistry Reilley Award (2006), U of M Outstanding Graduate Mentoring Award (2006), and American Chemical Society Division of Analytical Chemistry Award in Electrochemistry (2003).

Industry Roundtable Features a range of sensor companies participating in a roundtable discussion regarding key steps and barriers for commercializing chemical and biosensors.

Networking Session for Young Professionals Offers young professionals a chance to meet session chairs, conference organizers, invited speakers, and industry leaders in an informal setting to help build a network, establish collaborations, brainstorm new ideas, or find a mentor.

“From Gene to Device: The Route to Diagnostics in Low Resource Countries” Elizabeth “Lisa” A. H. Hall, University of Cambridge

Lisa Hall is Professor of Analytical Biotechnology and Head of Department in the Department of Chemical Engineering and Biotechnology, University of Cambridge, UK. She is an internationally recognized authority in the field of biosensors. Her research is focused on understanding how biology can be interfaced with electronic, mechanical, and optical systems, and new ways to answer fundamental and applied questions concerning new measurement regimes to achieve diagnostic systems. She received the Analytical Division of the Royal Society of Chemistry Gold Medal in 2005, and Alec Hough-Grassby Memorial Award from the Institute of Measurement & Control in 2009. Prof. Hall was appointed a CBE (Commander of the Order of the British Empire) for services to higher education and sport for the disabled in the Queen’s Birthday 2015 honors list. The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

239TH ECS MEETING WITH IMCS 18 • May 30-June 3, 2021

Live Symposia Sessions

‘‘

inning isn’t everything; it is the only thing...” is the quote often attributed to the famous American football coach, by Krishnan Vince Lombardi. This column examines the near misses in public acclamation (e.g., Nobel Prize) of some otherwise famous scientists and engineers in solid state and allied pursuits. If (and that’s a big if) we accept the Lombardi dictum, then the people identified below came out a distant second. The analysis of “who won and who didn’t” is commonly done in the sporting world where candidates to a particular Hall of Fame or aspirants to the Greatest of All Time (GOAT) accolade are discussed. Let us establish at the outset that this is at best an imperfect exercise given that: (a) performance conditions or even norms can often vary across generations, and (b) the judgment as to the awardworthiness of a given candidate is done by a committee of peers who are human and is, therefore, inevitably subjective. Incidentally, the process of how committees work (or don’t work) to reach a consensus is in itself a fascinating sociological topic that we will not have space to delve into in this present column. We begin with surface and interface science; surfaces are ubiquitous and dictate the performance of many materials in servicing our everyday living. They also represent an important technical content for our Society. Irving Langmuir, perhaps, was the first scientist from industry (General Electric or GE, Schenectady, NY) to be awarded the Nobel Prize in Chemistry in 1932 for his work on surfaces. Almost every scientist is familiar with Langmuir-Blodgett films, singlemolecule surface layers that have transformed the development of membranes and sensors. Yet, how many know that Katharine Burr Blodgett worked closely with Langmuir at GE? Didn’t she, therefore, deserve to share the award with Langmuir? Much more recently, Gerhard Ertl won the Nobel Prize in Chemistry in 2007 “for his studies of chemical processes on solid surfaces.” Interestingly, the person with whom he shared the Wolf Prize (considered by many to be a forerunner to the Nobel Prize),

Gabor Somorjai, missed out on sharing the award recognition with Ertl. Ertl was a graduate student of Heinz Gerischer, arguably the father of semiconductor electrochemistry and photoRajeshwar electrochemistry. This field happens to be one of my research specialties; it plays a key role in renewable energy technologies, as discussed elsewhere in this issue of the magazine. Yet Gerischer missed out on the Nobel Prize, and there is general belief that he should have shared the award with Rudy Marcus, who won it in 1992. That brings us to a rather remarkable story related to the Marcus Nobel Prize in Chemistry. Marcus happened to be attending the ECS biannual meeting in Toronto when the call came from Stockholm, and he had to be ushered out of a symposium to take the call. The Society celebrated this award recognition in a fitting fashion, and I, among many others, was fortunate to be there to share the excitement. Prof. Marcus won the award for his “contributions to the theory of electron transfer processes in chemical systems.” Electron transfer underpins many phenomena and devices that we encounter in everyday life, including photosynthesis, solar cells, batteries, transistors, etc. It is worth noting that Marcus won the award nine years after Henry Taube got the 1983 Nobel Prize in Chemistry “for his work on the mechanisms of electron transfer reactions, especially in metal complexes.” Marcus could well have shared the award with Taube, but his turn had to await experimental verification of his theoretical predictions, for example, the inversion regime. In retrospect, it turned out well for both of them, not having to share the prize! Nobel recognitions have been bestowed in at least four other instances where the awardees have been active ECS members. In three of these, one can talk about near misses. Jack S. Kilby won the Nobel Prize in Physics in 2000 for “basic work on information and communication technology.” However, the late Robert Noyce should also have been recognized for his role in developing the microchip. In fact, he may have missed out on at least one other occasion when Leo Esaki was awarded the 1973 Nobel Prize in

Winner Takes All “Winning isn’t everything; it is the only thing...”

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Physics for his “pathbreaking work on the tunnel diode…” This was a device on which Noyce had written a complete description nearly a year and a half before Esaki published his work in 1958. The fascinating behind-the-scenes story has been documented.1 The discovery of Buckyballs, a new form of carbon, ushered in the era of nanotechnology. Three scientists, Smalley, Curl, and Kroto, shared the Nobel Prize in Chemistry in 1996 for this discovery, which incidentally also helped to spawn one of the more active and vibrant divisions in our beloved Society, namely, Nanocarbons. However, the graduate students (Heath, O’Brien, and Liu) who performed many of the key experiments that led to this discovery had to be left out. The Nobel Prize rules stipulate that: (a) only three scientists may be recognized, and (b) awards may The first Nobel Prize Ceremony in 1901. not be given posthumously. The latter criterion most certainly impeded Robert Noyce from collecting the award. Light-emitting diodes (LEDs) have transformed the lighting industry, and the development of blue LEDS was significant for generating white light. Akasaki, Amano, and Nakamura shared the Nobel Prize in Physics in 2014, and these inventors have close ties with the ECS. However, there are many who vouch that other pioneers in LEDs, such as Losev, Holonyak, Neumark, and Maruska, should also have been recognized. There is the Nobel Rule of Three rearing its head again. The metal-oxide-silicon field-effect transistor (MOSFET), invented by Mohamed M. Atalla and Dawon Kahng in Bell Labs in 1959, arguably has been a dominant semiconductor technology in the microelectronics industry. MOS technology has paved the way for Nobel Prize-winning breakthroughs, such as the quantum Hall effect and the charge-coupled device (CCD), yet the MOSFET discovery itself has not garnered the Big Prize, an omission apparently acknowledged by the Royal Swedish Academy of Sciences itself. We remember the winners but not the runners-up. This is equally true for sporting events as it is for other peer awards and recognitions. For example, I may well remember an Oscar winner in a given category, but certainly not the others who may have been nominated. Let me close by looking beyond the boundaries of the solid state Daniel B. Wood, “Why Robert Noyce should have won two Nobel Prizes, but didn’t,” The Christian Science Monitor, Dec. 12, 2011.

About the Author Krishnan Rajeshwar specialized in solid state chemistry for his doctoral degree at the Indian Institute of Science in Bangalore, India. After a postdoctoral stint at Colorado State University, Fort Collins, CO, he joined the faculty of the Department of Chemistry and Biochemistry at The University of Texas at Arlington. He is now a Distinguished University Professor at UTA. He is a past

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

sciences and note that perhaps the above omissions pale before the Group of Six who must rank among the biggest Nobel Prize snubs: Mahatma Gandhi, Stephen Hawking, Eleanor Roosevelt, Jonas Salk, Leo Tolstoy, and Rosalind Franklin. Science can claim three of these candidates and 50 percent is not a bad statistic when it comes to underscoring the importance of science to society. I would challenge anyone who would not love to be included in the group of “also-rans” identified here. In that light, is Alfred Nobel, 1885. He founded the Nobel Prizes. winning everything? My sincere thanks to Jennifer Bardwell, Paul Cooper, Dennis Hess, Vistasp Karbhari, Rohini Krishnan, Paul Maggard, and Bob Savinell for their comments on initial drafts. © The Electrochemical Society. DOI: 10.1149.2/2.F04211IF.

president of The Electrochemical Society, and past editor of The Electrochemical Society Interface. His research interests span a broad spectrum in solid state chemistry, materials chemistry, and energy R&D. He has published some 400 papers in peer-reviewed journals, two monographs, and many chapters in these areas. This body of work has been cited ~ 22,000 times, and his h-index is 70. Rajeshwar has won many awards and recognitions (e.g., ECS Fellow, ETD Research Award, Electrodeposition Division Award). Very recently, he appeared in Stanford University’s World’s Top 2% Scientists list, ranked #95 in the energy category (https://data. mendeley.com/datasets/btchxktzyw/2). He may be reached at rajeshwar@uta.edu. https://orcid.org/0000-0003-4917-7790 33

Discoveries need discoverability.

Find out more about how ECS Author Choice Open Access can accelerate the impact of your research. The Electrochemical Society Interface • Spring 2021 • www.electrochem.org www.electrochem.org/oa

SOCIE PEOPLE T Y NE WS Aurbach Named Top Scientist

oron Aurbach has made Stanford University’s World’s Top 2% Scientists list, which represents the world’s top two percent of the most-cited scientists in a variety of fields. An ECS Fellow and technical editor for the Journal of The Electrochemical Society, Doron ranked 474th on the prestigious list of the top 100,000 scientists. Doron is a professor in the Department of Chemistry at BarIlan University in Israel, where he founded and currently leads the Electrochemistry Group. In addition, he is the head of the Israel National Research Center for Electrochemical Propulsion. Doron has published more than 540 peer-reviewed papers, which have received more than 37,000 citations. Doron Aurbach

SEARCHING FOR PEOPLE NEWS Interface is searching for People News for our upcoming summer issue. If you have news you would like to share with the ECS Society about a promotion, award, retirement, or other event, please email it to

MaryBeth.Schwartz@electrochem.org.

Participate in our next meeting! Build your community with ECS! • EXHIBIT • SPONSOR • ADVERTISE Contact sponsorship@electrochem.org The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

A Centennial Celebration:

100 Volumes of ECS Transactions

It all began in 2005.

ECS Transactions first publishes with Volume 1, Issue 1: “Physics and Chemistry of SiO2 and the Si-Si02 Interface – 5.” ECS Transactions was launched to replace the hardcover books that were published in The Electrochemical Society Proceedings Volumes.

Fast forward to 2021.

ECS Transactions publishes Volume 100: “IV Congreso Colombiano de Electroquímica (IVCCEQ2020).” Today, ECS Transactions is the official conference proceedings publication of The Electrochemical Society. This publication features full-text content of proceedings from ECS meetings and ECS-sponsored meetings. ECST is a high-quality venue for authors and an excellent resource for researchers. The papers appearing in ECST are reviewed to ensure that submissions meet generally accepted scientific standards.

Be a part of ECS history.

Get published in an upcoming volume of ECS Transactions. For more information, visit www.electrochem.org/publications/ecst.

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Looking at Patent Law:

Patenting a Solid State Lithium-Metal Battery – A Case Study by E. Jennings Taylor and Maria Inman

n this installment of the ‟Looking at Patent Lawˮ articles, we present a case study of a rechargeable solid state/lithium-metal battery. We have chosen this invention to align with the focus of this issue of Interface on solid state energy conversion. Recall from our previous article,1 the prosecution history (examination record) of a patent application is publicly available in the file wrapper on the U.S. Patent & Trademark Office (USPTO) Patent Application Information Retrieval (PAIR) system.2 With the USPTO PAIR system as the primary source of information for this case study, we illustrate the prosecution events encountered during the examination of U.S. Patent No. 9,761,861, “Pulse Plating of Lithium Material in Electrochemical Devices.”3 The ‘861 patent issued on September 12, 2017, with co-inventors Timothy Holme, Marie Mayer, Ghyrn Loveness, Zhebo Chen, and Rainer Fasching. The patent is assigned to QuantumScape Corp. of San Jose, CA. A second patent related to the subject invention issued on September 22, 2020, and an additional patent application filed on August 11, 2020, is pending.4,5 The factors leading to the additional patent and application will become evident as we review the prosecution events herein. QuantumScape was co-founded in 2010 by Jagdeep Singh, Prof. Fritz Prinz, and Dr. Tim Holme. Mr. Singh serves as CEO. Prof. Prinz is a professor of materials science at Stanford University and serves as state/lithium-metal Chief Scientific battery Advisor. Dr. adapted Holmefrom received his PhD in Fig 1. Solid concept investor presentation. Charged Discharged

Anode Current Collector

(as manufactured) Anode Current Collector

Lithium-Metal Anode

Solid State Separator

Active (prelithiated) Cathode

Active (lithiated) Cathode

Cathode Current Collector

Cathode Current Collector Not to scale

Fig 1. Solid state/lithium-metal battery concept adapted from the investor presentation.

mechanical engineering from Stanford University and serves as Chief Technology Officer. Dr. Holme is also a co-inventor on the ‘861 patent. QuantumScape’s focus is directed towards the commercialization of a solid state/lithium-metal battery for electric vehicle applications. Solid state/lithium-metal batteries hold promise for achieving the U.S. Department of Energy (DOE) technical and cost goals for battery packs, specifically 235 Wh/kg, 500 Wh/L, and 125 US$/kWh.6 QuantumScape investors include Bill Gates, Stanford University, and the Volkswagen Group.7 According to QuantumScape’s investor presentation on September 3, 2020, they have developed the only solid state/lithium-metal battery that has been validated by an automotive original equipment manufacturer (OEM).8 The ‘861 patent is generally directed towards a rechargeable solid state/lithium-metal battery method and device. Specifically, a pulse current is used to plate lithium metal onto the anode current collector during the initial in-situ formation of the lithium-metal anode. The lithium ions are derived from the cathode that has been prelithiated. With this approach, the inventors disclose an ‟anodelessˮ cell design and avoid the challenges associated with producing lithium-metal anodes during manufacturing. A pulse current is also used during subsequent recharging of the battery. The general concept of the solid state/lithium-metal battery is shown in Fig. 1. It is adapted from the September 3, 2020, investor presentation. As described in the patent, the pulse current during the initial formation and subsequent recharging of the lithium-metal anode may consist of both cathodic and anodic pulses. The cathodic pulses cause lithium metal to be plated on the anode current collector. The anodic pulses cause lithium dendrites formed during the plating pulses to be removed. In this manner, the inventors address the dendrite formation challenge associated with high-rate recharging of lithium-metal anode batteries.

Patent Applications The patent applications associated with the subject invention are presented in Table 1. A U.S. provisional patent application, 61/839,339, was filed on June 25, 2013. Subsequently, a U.S. utility patent application, 14/288,406, was filed on May 28, 2014. The U.S.

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(continued on next page) 37

Taylor and Inman

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utility filing was within one year of the filing date of the provisional patent filing date and thereby maintained the priority date (June 25, 2013) of the provisional patent application.9 A provisional patent acts as a filing date placeholder for the subsequently filed utility patent application. It is not examined and does not issue as a patent.10 Fig. 2 illustrates a battery cell (100) from the ‘406 patent application. The battery cell (100) includes a cathode current collector (101), a cathode region (102), an electrolyte (103), an anode region (104), and an anode current collector (105). The cathode region (102) is lithiated and can accommodate lithium ions when the battery cell (100) is discharged. The electrolyte (103) is a solid electrolyte material with a high level of ionic conductivity. The anode region (104) is formed by applying a pulsed current across the cathode current collector (101) and anode current collector (105) of the battery cell (100). During the initial charging of the battery cell (100), lithium ions migrate from the cathode region (102) through electrolyte (103) and plate onto the anode region (104). Candidate materials for the various components of the solid state/lithium-metal battery are listed in the ‘406 patent application. In order to establish a filing date, a utility patent application must include the following. 1. Specification11 “…a written description of the invention, and the manner and process for making it…to enable any person skilled in the art…to make and use [the invention]…” 2. Minimum of one claim12 “…particularly pointing out…the subject matter… as the invention…” 3. Drawings13 “…where necessary for understanding the subject matter… to be patented…” In order to maintain the filing date, the following additional criteria are required. 1. Filing fee in accordance with the current USPTO fee schedule.14 2. Inventor oath or declaration asserting15 a. The patent application was authorized by the inventor(s), b. The inventor(s) believe he/she is the original inventor or they are the original joint inventors. The ‘406 patent application was filed on May 28, 2014. The patent application included a specification, claims, drawings, and the required filing fee. Consequently, the ‘406 patent application met the requirements to establish a filing date. The specification included a description of the prior art, problems within the prior art, a summary of the invention describing various embodiments of the invention addressing the prior art problems, and a detailed description of the invention regarding the solid state/ lithium-metal battery (100). The utility patent application contained claims directed towards two statutory patent classes, method (process) claims and device (manufacture) claims.16 On June 9, 2014, the USPTO notified the applicants that the inventor oath/declaration had not been filed and that failure to do so would result in abandonment of the patent application. On June 18, 2014, the applicants submitted the declaration. The declaration included an assertion by the inventors stating,

“I believe that I am the original inventor or an original joint inventor of a claimed invention in the application.” The declaration also acknowledged that the inventors were aware of the penalties for a false statement,17 “I hereby acknowledge that any willful false statement made in this declaration is punishable…by fine imprisonment of not more than five (5) years, or both.” Please note that the “named inventors” must be correctly represented on a U.S. patent application.18 Specifically, the inclusion of a colleague as a co-inventor who did not participate in the conception of the invention is known as a misjoinder and invalidates an otherwise valid patent. Similarly, the exclusion of a co-inventor who participated in the conception is known as a nonjoinder and invalidates an otherwise valid patent. If an inventor is erroneously included or erroneously omitted as an inventor, the misjoinder/ nonjoinder may be corrected, and the patent remains valid.19 With the submission of the inventor oath along with the filing fee provided in the original patent application, the requirements to maintain a filing date were fulfilled. On June 18, 2014, the USPTO issued a filing receipt, and the utility patent application was assigned number 14/288,406, with a filing date of May 28, 2014.

Inventor Assignment, Power of Attorney, Nonpublication Request

The assignment of the inventor’s rights to QuantumScape Corp. was recorded at the USPTO on March 20, 2015. A power of attorney appointed registered patent practitioners from the firm Squire Patton Boggs, LLP “…prosecute this application and to transact all business in the United States Patent and Trademark office connected therewith…” Along with the ‘406 patent application, the applicants submitted a nonpublication request by asserting20 “I hereby certify that the invention disclosed in the attached application has not and will not be the subject of an application filed in another country…that requires publication at eighteen months after filing.” By avoiding the 18-month publication from the patent application’s priority date (June 25, 2013), the applicants were able to avoid public disclosure while the patent was being examined. The avoidance of public disclosure was presumably balanced against: 1. the loss of the potential to receive damages from infringement of the subsequently issued patent as of the publication date of the patent application, and 2. the loss of foreign patent rights, such that the potential to receive royalties from products manufactured and sold outside of the U.S. Note, in order to receive damages as of the publication date of the patent application, 1. the infringed claim of the issued patent must be “substantially identical” to that in the patent application,21 and

Table I. Patent Applications and Patents Associated with the Solid State Lithium-Metal Invention

APPL. TYPE

APPL. NO.

PAT. No.

TITLE

FILING DATE

ISSUE DATE

U.S. Provisional

61/839,339

N/A

Pulse Plating of Lithium Material in Electrochemical Devices

June 25, 2013 (Priority Date)

N/A

U.S. Utility

14/288,406

9,761,861

Pulse Plating of Lithium Material in Electrochemical Devices

May 28, 2014

Sep. 12, 2017

U.S. Utility (Divisional)

15/671,056

10,784,497

Pulse Plating of Lithium Material in Electrochemical Devices

Aug. 7, 2017

Sep. 22, 2020

U.S. Utility (Divisional)

16/990,318

Pending

Pulse Plating of Lithium Material in Electrochemical Devices

Aug. 11, 2020

Pending

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Requirement for Restriction/Election

On October 7, 2016, the USPTO issued a restriction/election requirement for the ‘406 patent application. A restriction/election requirement states that the subject patent application contains two or more inventions, and the applicant must “elect” which invention to prosecute first28 “If two or more independent and distinct inventions are claimed in one application… [the USPTO] may require the application to be restricted to one of the inventions…” The USPTO stated that the ‘406 patent application contained three inventions: Group I Claims 1-19 and 33; drawn to a method of forming an anode. Group II Claims 20-25; drawn to a device. Group III Claims 26-32; drawn to a method of charging. Fig 2. Figure 1 from ‘861 patent illustrating a battery cell of the subject invention.

2. the infringer must have had “actual notice” of the published patent application.22

Information Disclosure Statement

On March 16, 2015, the attorneys for the applicants submitted an “Information Disclosure Statement” (IDS) in accordance with U.S. patent laws. The IDS is the submission of relevant background art or information to the USPTO by the applicant. The “Duty of Candor” requires that the inventor submit an IDS within a reasonable time of submission of the patent application disclosing23 “…to the Office [USPTO] all information known to that individual to be material to patentability…” The “Duty of Candor” is specific to any existing claim and requires that the IDS be continually updated while the claim is pending. The “Duty of Candor” ceases only when the claim is allowed and the patent issue fee is paid. The “Duty of Candor” extends to any individual associated with the filing of the patent application, including: 1. inventor(s), 2. patent counsel, or 3. persons who are substantially involved in the preparation or prosecution of the patent application. Substantial involvement in the preparation of the patent application could include technical assistants, collaborators, or colleagues. Substantial involvement would generally not extend to clerical workers. Furthermore, the inclusion of a reference in an IDS24 “…is not taken as an admission that the reference is prior art against the claims.” If a finding of a violation of the “Duty of Candor” resulting in “inequitable conduct” regarding any claim in a patent is determined, then all the claims of the subject patent are rendered invalid.25 Finally, in spite of the requirement of the “Duty of Candor”, the applicant is cautioned not to “bury” the examiner with a long list of non-material references in hopes that the examiner will not notice the relevant material references.26 The specific guidance from the USPTO is to27 “…avoid the submission of long lists of documents if it can be avoided…If a long list is submitted, highlight those documents which have been specifically brought to the applicant’s attention and/or are known to be of most significance.”

The examiner provided an analysis per the Manual of Patent Examining Procedure (MPEP) that the three inventions were each distinct from the other. In comparing the inventions with Group I Claims and Group II Claims, as well as inventions with Group II Claims and Group III Claims, the examiner noted the inventions are related as “…process of making and product made.” Per the MPEP, the examiner noted that the inventions are distinct if one or both of the following criteria are met:29 1. The process as claimed can be used to make another or materially different product, or 2. The product as claimed can be made by another and materially different process. The examiner concluded that in the case of inventions with Group I Claims and Group II Claims as well as inventions with Group II Claims and Group III Claims, “…the product as claimed can be made by another and materially different process, such as coating the anode material in liquid from and drying.” In comparing the inventions with Group I Claims and Group III Claims, the examiner noted the inventions are related as “…directed towards related processes.” Per the MPEP, the examiner noted that the inventions are distinct if:30 1. The inventions as claimed are either not capable of use together or can have materially different design, mode of operation, function, or effect; 2. The inventions do not overlap in scope, i.e., they are mutually exclusive; and 3. The inventions as claimed are not obvious variants. The examiner concluded that in the case of inventions with Group I Claims and Group III Claims, “…the inventions as claimed have a different mode of operation because Group III is based on determining electrical properties and parameters for forming a lithiated anode region while Group I is based on the steps of forming the deposited material on the anode…there is nothing of record to shown them to be obvious variants.” The applicants “elected” to prosecute the invention with Group I Claims first. Inventions with Group II Claims and Group III Claims were subsequently prosecuted as divisional patent applications. (See Table 1.) (continued on next page)

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Taylor and Inman

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Exemplary independent claims31,32 from the ‘406 patent application directed towards invention with Group I Claims are reproduced herein Claim 1. A method for forming a lithium-metal anode in an electrochemical device, the method comprising: providing a cathode, the cathode having a positive current collector; providing a lithium conducting electrolyte region having a top surface and a bottom surface; the top surface interfacing a lithiated cathode; providing a negative current collector interfacing the bottom surface of the electrolyte region; and supplying a plurality of current pulses, the plurality of current pulses comprising a first pulse and a second pulse, the first pulse causing a formation of a layer of lithium-metal anode positioned between the negative current collector and the bottom surface, the first pulse being characterized by a first amount of charge and first polarity during a first duration, the second pulse being characterized by a second amount of charge and second polarity during a second duration, the first amount of charge being greater than the second amount of charge. Claim 1 essentially disclosed a pulse reverse waveform (Fig. 3) for forming a lithium-metal anode. Claim 15. A method for operating a lithium-metal anode electrochemical device, wherein the electrochemical device comprises a cathode current collector, an anode current collector, a solid electrolyte region positioned between the cathode current collector and anode current collector, and an anode region defined between the anode current collector and the solid electrolyte region, the method comprising: applying a plurality of current pulses between the cathode current collector and the anode current collector; causing lithium material within the electrochemical device to plate onto the anode region in response to the first pulse of current. Dependent Claim 19 is presented herein. Claim 19. The method of Claim 15 further comprising removing a dendrite layer formed near the anode region. This claim was particularly directed towards avoiding the adverse effects of dendrite formation during the initial formation and subsequent charging of lithium-metal anodes (Fig. 4). As noted above, the elimination of dendrite formation is an important hurdle to Fig 3. Figure the commercialization of lithium-metal anode batteries.

Non-Final Office Action (NFOA)

• Claim 17: Mayers discusses that the current pulses are interspersed by rest periods. • Claim 18: Mayers discloses that the pulse duration is longer than the relaxation time of the layers. Since Mayers did not disclose removing dendrites using reverse (anodic) pulses, Claim 19 was not rejected but was “objected to” as being dependent on a rejected base claim. The examiner noted that Claim 19 would be allowable if rewritten in independent form including all the limitations of base Claim 15.

Examiner Interview

On March 23, 2017, the applicants (patent counsel as well as lead inventor) conducted a telephone interview with the patent examiner in order to better understand the basis for the rejections in lieu of the cited prior art. (Note, examiner interviews should be conducted by/ with patent counsel.) While telephone interviews can be helpful in clarifying the issue with the examiner, a caution regarding telephone interviews is that a verbal agreement by the examiner does not bind the examiner to the agreement.35 Furthermore, all business with the USPTO should be conducted in writing.36 “The action of the Patent and Trademark Office will be based exclusively on the written record in the Office. No attention will be paid to any alleged oral promise, stipulation, or understanding in relation to which there is disagreement or doubt.”

Consequently, subsequent to the interview on March 29, 2017, the applicants submitted a written “Applicant-Initiated Interview Summary” of the interview. The interview was summarized as follows. “Discussed the difference of a solid electrolyte of the present invention and the solid electrolyte interface formed from a liquid electrolyte of Mayers. Also discussed that the thickness of the solid electrolyte interface of Mayers is much less than the thickness of the solid electrolyte of the present invention. Examiner agreed that the rejection over Mayers has been overcome…” The applicants pointed out the Mayers prior art reference was directed towards liquid electrolyte lithium batteries and the formation of the solid electrolyte interface (SEI) during cycling. The ‘406 patent application is directed towards lithium batteries with solid electrolytes.

3A from the ‘406 patent application illustrating a pulse waveform.

On January 26, 2017, the USPTO issued a NFOA. The NFOA 1) allowed Claims 1 to 14 and Claim 33, 2) rejected Claims 15 to 18, and 3) objected to Claim 19. Note, Claims 2 to 14 depended from Claim 1 and thereby add limitations vis-à-vis Claim 1. Consequently, since independent Claim 1 was allowed, all claims which depend from Claim 1 were allowed. Claims 15 to 18 were rejected as being anticipated in view of the prior art33 based on a single prior art reference; Mayers, “Suppression of Dendrite Formation via Pulse Charging in Rechargeable LithiumMetal Batteries.”34 The examiner stated that Mayers teaches all the limitations of Claims 15 to 18. Specifically, regarding • Claim 15: Mayers discloses a process of operating a lithiummetal battery comprising a solid electrolyte by applying a plurality of current pulses to plate lithium material onto the anode. • Claim 16: Mayers teaches that the net charge of the plurality of current pulses is greater than zero (i.e., net cathodic). 40

Fig 3. Figure 3A from the ‘406 patent application illustrating a pulse reverse waveform. The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Response to NFOA Based on the examiner interview, the applicants responded by adding a minimum thickness limitation to independent Claim 15 in order to distinguish from the SEI of the prior art reference (Mayers) and solid electrolyte of the ‘406 patent application. The amended Claim 15 with inserted text and (deleted) text is presented. Claim 15 (Amended). A method for operating a lithium-metal anode electrochemical device, wherein the electrochemical device comprises a cathode current collector, an anode current collector, a solid electrolyte having a thickness of at least 400 nm [region] positioned between the cathode current collector and anode current collector, and an anode region defined between the anode current collector and the solid electrolyte having a thickness of at least 400 nm [region], the method comprising: applying a plurality of current pulses between the cathode current collector and the anode current collector; and causing lithium material within the electrochemical device to plate onto the anode region in response to the first pulse of current. Assuming the examiner would allow amended independent Claim 15 based on the interview, then dependent Claims 16 to 19 would also be allowed, and Claim 19 would not need to be rewritten in independent form as suggested in the office action.

Allowance of Patent Application Based on the amended independent Claim 15, on June 8, 2017, the USPTO issued a notice of allowance for the U.S. utility patent application with Claims 1 to 19 and 33. After payment of the issue fee on August 8, 2017, the 14/288,406 patent application issued as U.S. Patent No. 9,761,861 on September 12, 2017.

Divisional Patent Applications

After the allowance of the ‘861 patent, and prior to its issuing on September 12, 2017, the applicants filed divisional Patent Application No. 15/671,056 with the Group II Claims on August 7, 2017. U.S. Patent No. 10,784,497 based on the ‘056 patent application issued on September 22, 2020. After the allowance of the ‘497 patent, and prior to its issuing on September 22, 2020, the applicants filed divisional Patent Application No. 16/990,318 with the Group III Claims on August 11, 2020. The '318 patent application is pending at the time this article was prepared. The provisional and utility applications are summarized in Table 1.

Change in Small Entity Status

Subsequently, on May 17, 2019, the applicants notified the USPTO that they were no longer eligible for small entity status. The USPTO requires the applicant’s notification of 37 “…loss of entitlement of small entity status is required

Fig 4. Figure 4 from the issue ‘406 patent application illustrating when and maintenance fees aredendrite due…”formation on the lithium-metal anode.

Electric field concentration at the dendrite tips. “mossy” dendritic growth Evenly plated Li

While the applicants initially claimed small entity status and paid lower filing and issue fees, the applicant’s status changed, and they concluded they would no longer be able to claim small entity status when the three-and-a-half-year first maintenance fee was due.

Summary

In this installment of our “Looking at Patent Law” series, we present a case study of the prosecution of U.S. Patent No. 9,761,861, “Pulse Plating of Lithium Material in Electrochemical Devices.” We have chosen this invention to align with the focus of this issue of Interface on solid state energy conversion. The ‘861 patent was issued on September 12, 2017, with co-inventors Timothy Holme, Marie Mayer, Ghyrn Loveness, Zhebo Chen, and Rainer Fasching. The patent is assigned to QuantumScape Corp. of San Jose, CA. A second patent related to the subject invention issued on September 22, 2020, and an additional patent application filed on August 11, 2020, is pending. The case study begins with a brief synopsis of the background of the invention followed by 1) a discussion of the patent applications associated with the invention, 2) inventor assignment and power of attorney designations, 3) submission of the information disclosure statement and duty of candor, 4) restriction/ election requirement, 5) non-final office action resulting in rejection of the patent application, 6) applicant interview with the examiner, 7) applicant response to the non-final office action, 8) allowance of the patent application, 9) subsequent divisional patent applications, and 10) applicant change from small entity status. As discussed above, the applicants submitted a nonpublication request to avoid publication of the patent application 18 months after filing of the provisional patent application. By avoiding the publication of the patent application, the applicants were able to avoid public disclosure while the patent was being examined. The avoidance of public disclosure was presumably balanced against 1) the potential to receive damages from infringement of the subsequently issued patent as of its publication date, and 2) the ability to file foreign patent applications. With this case study, we hope to demystify the patent prosecution process and better prepare electrochemical and solid state scientists, engineers, and technologists to interact with their patent counsel regarding their inventions. © The Electrochemical Society. DOI: 10.1149.2/2.F05211IF.

About the Authors E. Jennings Taylor is the founder of Faraday Technology, Inc., a small business focused on developing innovative electrochemical processes and technologies based on pulse and pulse reverse electrolytic principles. Taylor leads Faraday’s patent and commercialization strategy and has negotiated numerous patents via field of use licenses as well as patent sales. In addition to technical publications and presentations, Taylor is an inventor on 40 patents. Taylor is admitted to practice before the United States Patent & Trademark Office (USPTO) in patent cases as a patent agent (Registration No. 53,676) and is a member of the American Intellectual Property Law Association (AIPLA). Taylor has been a member of ECS for 42 years and is a fellow of ECS. He may be reached at jenningstaylor@faradaytechnology.com. https://orcid.org/0000-0002-3410-0267 Maria Inman is the research director of Faraday Technology, Inc., where she serves as principal investigator on numerous project development activities, and manages the company’s pulse and pulse reverse research project portfolio. In addition to technical publications and presentations, she is competent in patent drafting and patent drawing preparation

Fig 4. Figure 4 from the ‘406 patent application illustrating dendrite formation on the lithium-metal anode. The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

(continued on next page) 41

Taylor and Inman

(continued from previous page)

and is an inventor on seven patents. Inman is a member of ASTM and has been a member of ECS for 25 years. Inman serves ECS as a member of numerous committees. She may be reached at mariainman@faradaytechnology.com. https://orcid.org/0000-0003-2560-8410

References 1. E. Jennings Taylor and Maria Inman, “Looking at Patent Law: Opportunity Prospecting by Analysis of Analogous Patent Art,” Electrochem. Soc. Interface 26(4), 57-61 (Winter 2017). 2. USPTO Patent Application Information Retrieval (PAIR) https://portal.uspto.gov/pair/PublicPair 3. T. Holme, M. Mayer, G. Loveness, Z. Chen, and R. Fasching, “Pulse Plating of Lithium Material in Electrochemical Devices,” U.S. Patent No. 9,761,861 issued September 12, 2017. 4. T. Holme, M. Mayer, G. Loveness, Z. Chen, and R. Fasching, “Pulse Plating of Lithium Material in Electrochemical Devices,” U.S. Patent No. 10,784,497 issued September 22, 2020. 5. T. Holme, M. Mayer, G. Loveness, Z. Chen, and R. Fasching, “Pulse Plating of Lithium Material in Electrochemical Devices,” U.S. Patent Appl. No. 16/990,318 filed August 11, 2020. 6. P. Albertus, S. Babinec, S. Litzelman, and A. Newman, “Status and Challenges in Enabling the Lithium Metal Electrode for High-Energy and Low-Cost Rechargeable Batteries,” Nature Energy Vol. 3, pp. 16-21, January (2018). 7. https://www.quantumscape.com/team/ (accessed November 24, 2020) 8. https://www.quantumscape.com/wp-content/uploads/2020/10/ QuantumScape-Investor-Presentation-Sept2020.pdf (accessed November 24, 2020). 9. 35 U.S.C. §111 Application. 10. 35 U.S.C. §119 Benefit of Earlier Filing Date; Right of Priority. 11. 35 U.S.C. §112(a) Specification/In General. 12. 35 U.S.C. §112(b) Specification/Conclusion. 13. 35 U.S.C. §113 Drawings. 14. https://www.uspto.gov/learning-and-resources/fees-andpayment/uspto-fee-schedule#Patent%20Fees 15. 35 U.S.C. §115(b)(1)(2) Inventor’s Oath or Declaration/ Required Statements.

16. 35 U.S.C. §101 Inventions Patentable. 17. 18 U.S.C. §1001Statements or Entries Generally. 18. E. Jennings Taylor and Maria Inman, “Looking at Patent Law: Why Is the Word ‘Right’ Mentioned Only Once in the Constitution of the United States?” Electrochem. Soc. Interface 26(2), 45-47 (Summer 2017). 19. Manual of Patent Examination Procedure (MPEP) §1481.02 Correction of Named Inventor. 20. 35 U.S.C. §122(b)(2)(B)(i) Confidential Status of Applications: Publication of Patent Applications. 21. 35 U.S.C. §154(d)(1)(B) Contents and Term of Patent; Provisional Rights. 22. 35 U.S.C. §154(d)(2) Contents and Term of Patent; Provisional Rights. 23. 37 CFR §1.56(a) Duty to Disclose Information Material to Patentability. 24. Riverwood Int’l Corp. v. R.A. Jones & Co., 324 F.3d 1346, 135455, 66 USPQ2d 1331, 1337-38 (Fed Cir. 2003). 25. Manual of Patent Examination Procedure (MPEP) §2016 Fraud, Inequitable Conduct, or Violation of Duty of Disclosure Affects All Claims. 26. R. B. Taylor, “Burying,” Mich. Telecomm. & Tech. Law Rev. 99, 19 (2012). 27. Manual of Patent Examination Procedure (MPEP) §2004.13 Aids to Comply with Duty of Disclosure. 28. 35 U.S.C. §121 Divisional Applications. 29. Manual of Patent Examination Procedure (MPEP) §806.05(f) Process of Making and Product Made. 30. Manual of Patent Examination Procedure (MPEP) §806.05(j) Related Products; related Processes. 31. E. Jennings Taylor and Maria Inman, “Looking at Patent Law: Patentable Inventions, Conditions for Receiving a Patent, and Claims,” Electrochem. Soc. Interface 26(3), 44-48 (Fall 2017). 32. 35 U.S.C. §112(c) Specification/Form. 33. 35 U.S.C. §102 Conditions for Patentability; Novelty. 34. M. Mayers, J. Phys. Chem.,Vol. 116, pp. 26214-26221 (2012). 35. In re Milton (Patent Petition 2007, Appl. No. 09/938,465). 36. 37 CFR § 1.2 Business to be Transacted in Writing. 37. CFR § 1.27(g)(2) Notification of Loss of Entitlement to Small Status.

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T ECH HIGHLIGH T S All-Dry Synthesis of Single Crystal NMC Cathode Materials for Li-Ion Batteries NMC materials with various stoichiometries continue to be some of the most heavily researched cathodes for Li-ion batteries. Numerous methods are being investigated to enhance their electrochemical performance, including increasing Ni content and the use of novel electrolyte additives. Single crystal (SC) cathode materials are also being considered as a means to boost performance. SC materials consist of particles, which are composed of one or few grains as opposed to polycrystalline (PC) materials, which are aggregates of many small crystallites. Particle cracking remains a challenge for PC materials as it leads to isolated active materials and capacity fading. Commercial SC cathode materials are prepared using a co-precipitation method, which can produce significant amounts of wastewater and is a costly process. In an attempt to address the shortcomings of the co-precipitation method, researchers from Dalhousie University and Acadia University have developed a method to prepare SC-NMC from submicron ballmilled oxide precursors. This all-dry process has many advantages over the traditional coprecipitation method including, high yield, low waste production, and lower cost. The method outlined in this report is a promising route for the scalable synthesis of SC cathode materials. From: L. Zheng, J. C. Bennett, and M. N. Obrovac, J. Electrochem. Soc., 167, 130536 (2020).

In-Situ Time-Lapse SKPFM Investigation of Sensitized AA5083 Aluminum Alloy to Understand Localized Corrosion 5xxx aluminum alloy (Al-Mg) is susceptible to intergranular corrosion in a saline environment due to the sensitization involving supersaturated Mg precipitation at the grain boundary, forming electrochemically active intermetallic phases (IMPs) such as Al3Mg2 and silicide. These IMPs in 5xxx alloys can form micro-galvanic cells between the particles and alloy matrix and thus increase susceptibility to localized corrosion, which can be intensified in a thin-film electrolyte environment. Liew et al. utilized Scanning Kelvin Probe Force Microscopy (SKPFM) to conduct in-situ Volta potential measurement on a highly sensitized AA5083 surface in a simulated chloride-bearing thin-film electrolyte condition by varying relative humidity (RH) at different time courses. They found that magnesium-silicide particles (either Mg-rich or Mg-lean) inverted from noble (positive Volta potential) to active (negative potential compared to the matrix) when at higher RH (~80%) and longer exposure time (>22hrs). This inversion is caused by preferential dissolution of Mg and the formation of porous mixed-oxide containing SiOx, MgOx, and hydroxide. In contrast, aluminide particles mainly stayed as local cathodes over the course of exposure.

This study investigated the nobility change of the IMPs with respect to alloy matrix and elucidated the underlying localized corrosion mechanism at the earliest stage.

From: YH. Liew, C. Örnek, J. Pan, et al., J. Electrochem. Soc., 167, 141502 (2020).

Imaging Cycle-Induced Damage of MnO2 Microparticles Intercalation of cations into MnO2 is often proposed as a basis for electrochemical energy storage devices. However, progressive capacity loss results in low cycle life, especially in certain electrolytes. A team at the University of Florida has devised a method to follow the progressive physical effects of cycling on monodisperse MnO2 microparticles. They accomplish this by use of a gold-microtube membrane, on which MnO2 is electrodeposited, resulting in discrete 5-μm microparticles affixed to the membrane surface, which are individually electronically wired through the gold microtubes. To demonstrate the method, they cycled the MnO2 in two electrolytes: 0.1 M LiClO4 in H2O and 1 M LiClO4 in propylene carbonate. In the non-aqueous propylene carbonate system, the particles retained their shape and size through 500 oxidation/reduction cycles. In contrast, the particles in the aqueous system became diffuse and highly dendritic, losing much of their physical integrity. Because a significant concentration of Mn was found in the aqueous electrolyte by ICPAES, the team concluded that the degradation mechanism was due to Mn(II) dissolution as a result of acid-induced disproportionation. The microtube-membrane method is a promising strategy to monitor the fate of particles, which is often challenging within composite porous electrodes. From: S. N. Bush, J. Experton, A. Teyssendier de La Serve, et al., J. Electrochem. Soc., 167, 132501 (2020).

Psychoactive Substances and How to Find Them: Electrochemiluminescence as a Strategy for Identification and Differentiation of Drug Species Many novel psychoactive substances (NPS) have imitative effects of illicit drugs but are not the targets of the historical standard presumptive tests due to their similar yet different chemical structures. Tremendous efforts are being spent to develop comprehensive screening technologies for NPS detection. In a recent report, researchers from the University of Strathclyde of UK and Deakin University of Australia conducted a proof-of-concept study of the use of electrochemiluminescence (ECL) as such a technology. ECL is a powerful yet simple analytical technique especially suitable for “in-field” and point-of-care applications. However, the lack of selectivity limits its application to differentiate structurally similar compounds. With a multiple-luminophore strategy, the authors investigated the ECL

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

behaviors of a number of structurally closely related amine-containing drug compounds on carbon paste electrode surfaces modified with Os-, Ir-, and Ru-based luminophores. It was found that while the traditional Os complex luminophore could not differentiate the drug molecules, Ir and Ru complexes offered rather different ECL selectivity. In combination with other approaches such as pH control, the authors envisioned the development of ECL sensor arrays to further improve the method’s selectivity. From: K. Brown, P. Allan, et al., J. Electrochem. Soc., 167, 166502 (2020).

A Sensitive Carbon Paste Electrode for Selective Detection of Lead Based on the Synergistic Effect of Bismuth and Chelating Agent Analytical techniques to detect lead at levels of 10 micrograms/liter, such as AAS, ICP-AES, need large-scale instruments. Electrochemical techniques like Differential Pulse Stripping Voltammetry (DPSV) offer a simple way with good sensitivity and selectivity. In DPSV, mercury is used as the working electrode. Given the toxicity of mercury, researchers from Shenzhen University, Dongguan University of Technology, and Qingdao University of Science and Technology came up with an innovative way of using bismuth and diphenyl thiocarbazone as part of the carbon paste electrode (CPE) to effectively detect lead with concentrations as low as 10 micrograms/ liter. To evaluate the role and significance of each of the components of the electrode, the team built CPE, Bi-CPE, Di-CPE, and Bi-DiCPE and characterized the electrodes using SEM. Researchers evaluated the response of the electrodes to different concentrations of lead and ascertained the strong synergistic effect of bismuth and diphenyl thiocarbazone. They also found linearity in response from 10 to 80 µg/l. The team also confirmed that interference from other metallic ions did not impact detectability. They concluded the study with the determination of lead level in real water and compared this with other established techniques. From: Q. Yang, C. Yang, J. Yi, et al., J. Solid State Sci. Technol., 9, 101012 (2020).

Tech Highlights was prepared by Joshua Gallaway of Northeastern University, David McNulty of Paul Scherrer Institute, Chao (Gilbert) Liu of Shell, Zenghe Liu of Abbott Diabetes Care, Chock Karuppaiah of Vetri Labs, and Donald Pile of EnPower, Inc. Each article highlighted here is available free online. Go to the online version of Tech Highlights in each issue of Interface, and click on the article summary to take you to the full-text version of the article. 43

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Solid State Aspects of Energy Conversion by Paul A. Maggard

fficient energy conversion forms the foundation for harnessing our widespread, renewable sources of energy (e.g., solar, geothermal, wind, etc.) to meet the rising global energy demands of society. Most often, this conversion requires that the incident radiation, excess heat, or mechanical energy be transformed into transportable fuels or electrical power. Electrochemical reactions that occur at the interfaces of solids represent a common underlying strategy to drive the formation, storage, and/or release of energy. While usually simple in conceptualization, reactions at solid state interfaces are highly dependent on a plethora of parameters, including chemical composition, crystalline structure, particle morphology and microstructure, the orientation of the exposed surface facets, and so on. This special issue focuses on the many aspects of solid state chemistry that impact the efficiency of electroactive solids in energy conversion. Described in the first article in this issue, “In Search of the “Perfect” Inorganic Semiconductor/Liquid Interface for Solar Water Splitting,” by Rajeshwar, O’Donnell, and myself, is the concept of designing the most efficient possible photoelectrode for the production of chemical fuels from sunlight. This article breaks down the key solid state semiconductor properties into those that (a) best optimize its photovoltaic function and those that (b) are required for its optimal electrochemical performance. The synergistic overlap of both sets of attributes within single or multiple n-/p-type semiconductors has been a daunting task the field has not yet solved. Effective strategies in the field have relied on the careful control of the crystalline structure and chemical composition, e.g., utilizing multiple metal cations and/ or anions, or in manipulating the extent of atomic-site disorder or crystallographic anisotropies. The second article in this issue, “Synthesis as a Design Variable for Oxide Materials,” by Vaughey, Trask, and Poeppelmeier, looks at the many synthetic parameters that can be used in preparing and tuning the properties of electroactive solids. This feature discusses how the optimization of physical properties is fostered when the key factors in solid state synthesis are more deeply understood. Described therein, current techniques extend beyond traditional solid state ceramic methods, including lower-temperature flux and synthetic hydrothermal routes wherein a molten salt or an aqueous solution serve as the reaction media, respectively. Synthetic variables such as reaction stoichiometry, heating profile, and reaction medium can play predominant roles in determining the resulting crystal polymorph or size. These characteristics translate directly to electrode fabrication, where the particle sizes and suspension rheology are critical to the creation of high quality, electroactive monoliths. The next article in this issue is “Electrodeposition as a Powerful Tool for the Fabrication and Characterization of Next-Generation Anodes for Sodium Ion Rechargeable Batteries” by Gimble, Nieto, and Prieto. This feature focuses on the advantages of electrodeposition as a powerful synthetic tool in the acceleration of solid state battery research. Specifically, electrodeposition research in the Prieto group has demonstrated this approach is ideally suited for optimizing the liquid electrolytes and additives needed to develop sodium ion rechargeable batteries. Further, it allows the three-dimensional

architecture of the electrode to be modulated concomitantly with tuning the chemical composition and crystalline structure. This is achieved without the traditional binders required in the electrode fabrication process. These features all combine within a solid film to yield electrodes targeted at higher power density and greater mechanical stability. The last article, “A Vision for Sustainable Energy: The Center for Hybrid Approaches in Solar Energy to Liquid Fuels (CHASE),” by Dempsey, Heyer, and Meyer, provides a compelling vision for the future integration of molecular catalysts and solid state semiconductors. As described therein, the goal of efficiently producing chemical fuels from sunlight will ultimately be achieved within three-dimensional photoelectrode architectures by optimal spatiotemporal control of incident photons, charge carriers, and downstream product formation. The assembled teams of CHASE investigators serve to underscore the required application of fundamental scientific principles across a wide swath of disciplines, ranging from molecules to solids. A daunting multitude of synthetic and structural parameters are described that will need to be probed and understood at the interfaces of molecular catalysts with solid state semiconductors. Approaches to efficient energy conversion in these feature articles cover only a small part of the potential applications, which also include related research into supercapacitors, fuel cells, and dielectrics, to name a few. The current technological stage of each of these fields ensures that the solid state aspects of the underlying electrochemical properties cannot be productively ignored. Clearly, research progress will be most accelerated by strategies that effectively leverage an indepth understanding of the underlying solid state characteristics, e.g., crystalline structure, particle morphology, and chemical composition. I hope that these feature articles help to illustrate many of the solid state guiding principles that are effectively driving these important technological fields. © The Electrochemical Society. DOI: 10.1149.2/2.F06211IF.

About the Author Paul A. Maggard earned his PhD in inorganic solid state chemistry at Iowa State University. Following a postdoctoral appointment at Northwestern University, he took a faculty position at North Carolina State University’s Department of Chemistry. Research efforts in his laboratory group center on the flux and hydrothermal synthesis of metal oxides and metal-oxide/organic hybrids for novel investigations into their catalytic, electronic, and photoelectrochemical properties for solar energy conversion. He currently holds the position of associate professor. Maggard has published >100 papers and book chapters and given a number of invited presentations. He has received several awards, including the NSF CAREER award, Beckman Young Investigator award, and Scialog award. Maggard may be reached at paul_maggard@ncsu.edu. https://orcid.org/0000-0002-3909-1590

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In Search of the “Perfect” Inorganic Semiconductor/Liquid Interface for Solar Water Splitting by Krishnan Rajeshwar, Paul A. Maggard, and Shaun O’Donnell

Introduction

Design Criteria

rguably, one would be hard-pressed to envision a more ideal renewable energy conversion system than the solar splitting of water. The energy-rich product, hydrogen, may be stored and used later on-demand for generating power either via combustion or in a fuel cell. In scenarios where dioxygen is needed for respiration (e.g., space travel), CO2 may be used instead of water as the reactant feed. Both these applications require a photon absorber for capturing sunlight, and an inorganic semiconductor fulfills this function. Therefore, a photoelectrochemical (PEC) system may be devised based on an nor p-type semiconductor electrode in contact with the reactant fluid. On bandgap excitation of the photoelectrode, the generated holes or electrons respectively are used to drive the oxidation or reduction of the reactant species. In the case of water splitting, these are the OH- or H3O+ ions, respectively. In a CO2 photoreduction system, the corresponding species are OH- and (dissolved) CO2. In both cases, the analogy with a plant photosynthesis system is direct. This article reviews design criteria for the choice of the semiconductor photoelectrode and the underlying challenges.1,2 The present discussion is confined to solar water splitting rather than CO2 reduction. Our focus here is on electrodes rather than the related photocatalytic strategy involving semiconductor nanoparticle suspensions. While considerable progress has been made on tandem photovoltaic-PEC cell combinations, the discussion below centers on integrated assemblies wherein the semiconductor electrode(s) fulfill(s) both the photovoltaic (PV) and electrochemical functions, shown in Fig. 1. This inevitably complicates the materials’ design, but the potential technology payoff justifies the R&D endeavor involved. Dye-sensitized PEC designs are also not considered herein; i.e., in all the cases below, the inorganic semiconductor (instead of a dye) functions as the photoabsorber. New-generation PV materials such as organic perovskites are also beyond the scope of this discussion that is focused on oxide semiconductors.

In discussing the semiconductor photoelectrode material prerequisites, it is expedient to consider the photocurrent density Jph as a figure of merit and consider its component parameters:4 (1) Here, φ is the photon flux and the and the third, fourth, and fifth ɳ terms represent the efficiency terms for light-harvesting (LH), charge (i.e., electron-hole) separation and transport to the surface (CS), and charge transfer (CT) across the interface, respectively. Of these three ɳ terms, the first two impact the photovoltaic (PV) performance of the material, while the last term encompasses its electrochemical (EC) activity. A “perfect” PEC photoelectrode is a perfect PV and EC material; herein lies the challenge. What might be considered to constitute a perfect EC material? Given that electrochemical processes are surface-confined, the material has to have excellent catalytic attributes. The kinetic constraints are even more drastic for the four-electron water oxidation process (oxygen evolution reaction or OER) relative to the two-electron hydrogen evolution reaction (HER). Unfortunately, inorganic semiconductor surfaces are typically only poorly catalytic, and as such, co-catalysts are needed to drive the multielectron water-splitting reactions. These catalysts should ideally be derived from Earth-abundant and nontoxic elements when the PEC water-splitting system is scaled up. Recall also that any solar energy conversion system requires large active areas for the photon-harvesting component, although this constraint impacts PV and PEC devices alike. As if the above criteria are not stringent enough, the need for photoelectrode stability (minimum 10-year lifetime) is an added complexity (relative to a PV device counterpart) in the PEC system. This is much less of a concern with a PV system in that the device is all solid state, i.e., containing no electrolytes with corrosive or (continued on next page)

Single or Dual Photoelectrode Designs? The PEC cell may be designed with a single n- or p-type photoelectrode and a dark counterelectrode where either the proton reduction or water oxidation respectively occurs. Alternatively, the plant photosynthesis system may be mimicked via a two-photon approach (e.g., a so-called Z-scheme) using an n- and p-type semiconductor photoelectrode in concert. The maximum theoretical efficiencies have been computed for both approaches.3 The dual-photoelectrode cell design is complicated by the need for carefully matching the photocurrents at both terminals. Fig. 1. Schematic diagrams of the functional operation of water-splitting semiconductor systems that are (a) photovoltaic driven with a coupled electrolyzer unit or (b) photoelectrochemically driven with a light absorbing photoanode and a metal cathode. The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

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complexing component species. The PEC stability includes preservation of surface chemical fidelity both in the dark and under bandgap irradiation of the photoelectrode. Note that efficiency and stability are intertwined in the sense that if the last term in Eq. 1 above is not optimal, charge carriers will accumulate at the surface and will attack the semiconductor itself. Also, note that the foregoing discussion (and Eq. 1) apply equally well to PEC interfaces derived from n- or p-type semiconductors. The distinction is that the photocurrent is anodic for n-type, e.g., Fig. 1b, and cathodic for p-type semiconductors, and the relevant minority carriers that feed into Eq. 1 are holes and electrons, respectively, for the two semiconductor types. Table 1 captures the essential combination of attributes sought for a PEC Fig. 2. Composition line diagrams (see also Ref. 1) for various stoichiometric oxides in the (a) MO-V2O5 (b) M2O-V2O5, (c) MO-WO3, and (d) M2O3-V2O5 compound families. M = Cu or Bi. semiconductor electrode. The threshold voltage for water splitting needs to be given here.1,7-9 As in the PV case, the search has progressed at 298 K is 1.23 V; to this thermodynamic value must be added kinetic beyond elemental semiconductors to binary compounds, to ternary (overpotential) and other electrical (e.g., iR drop) losses. Thus, the net compounds and beyond. For solid state PV devices (where corrosion critical voltage amounts to ~ 1.7 V. If the open circuit photovoltage is stability is not an overriding concern as in the PEC counterparts), Si, set to ~70 % of the semiconductor bandgap, it becomes immediately CdTe, and ternary (and multinary) chalcogenides (e.g., copper indium obvious that Si (with a bandgap of 1.1 eV) can be ruled out. In fact, gallium selenide or CIGS) have emerged as promising candidates.10 it is quite unlikely that a single semiconductor will fulfill the energy In the PEC case, oxide semiconductors have been intensely studied requirements for unassisted (zero bias) water splitting. A sequence since they appear to at least partly meet the stringent requirements of two semiconductors with bandgaps of ~ 1.9 eV and ~1.3 eV has discussed above. However, these materials have exhibited rather low been proposed to attain the requisite voltage to split water.5 Further, device efficiencies for water splitting relative to other candidates the semiconductor energy levels in this combination must be such such as group III-V semiconductors. Nonetheless, the community that the conduction band edge lies at a potential more negative than continues to pursue the search for an optimal oxide in the hope that the HER potential. The valence band edge must be more positive good corrosion stability can be combined with high charge transfer than the OER potential. In this manner, the photogenerated electrons efficiency. and holes will have sufficient potential to reduce protons and oxidize In this vein, the remainder of this article focuses on oxide water, respectively, without the need for an external bias potential. semiconductors. While ternary oxides (e.g., SrTiO3) featured fairly Unfortunately, the state-of-the-art synthetic routes do not yet early on in the history of PEC water splitting, the vast majority of enable one to simply dial in the attributes listed in Table 1 and secure the studies focused on binary oxides, of which TiO2, Fe2O3, WO3, the “ideal” semiconductor photoelectrode. Given this roadblock, and Cu2O are worthy of mention.11-16 Of these, both Fe2O3 and there is no alternative to the painstaking synthesis-characterizationCu2O have the optical advantage of a low bandgap. However, Cu2O optimization loop. Combinatorial approaches suggest a potential way is not stable in aqueous solutions; Fe2O3, while stable, has rather out of this impasse; note that the water-splitting community shares a poor charge transport properties. These findings have prompted similar challenge with the pharmaceutical enterprise in this regard.6 researchers (including the present authors) to pursue ternary oxides, However, at this writing, there is, unfortunately, no magic bullet such as many derived from Cu2O,17-22 in the hope that the otherwise semiconductor that fulfills all the criteria listed above. excellent PEC performance can be combined with enhanced stability via the incorporation of a second metal cation. In this regard, ternary Photoelectrode compositions based on another copper oxide, namely CuO, have also Semiconductor Candidates been considered. (See Fig. 1c.) The progress with the PEC materials genome for solar water splitting has been thoroughly reviewed such that only a snapshot Table I. Characteristics of an ideal PEC semiconductor electrode for solar water splitting.

PV Properties

Electrochemical Properties

High absorption coefficient

High catalytic activity for OER and HER

Optimal bandgap

High corrosion stability in the dark and under irradiation

Other Criteria Earth abundance and non-toxicity of component elements Ease of synthesis and scale-up

Large minority carrier diffusion length Negligible bulk recombination Negligible surface and space charge layer recombination Negligible bulk resistance 48

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Ternary and Multinary Oxides In exploring the myriad compositions to be considered in the discovery phase, ternary or higher multinary oxides may be considered as derivatives of their binary oxide components. Consider, for now, the ternary oxides that may be derived from combinations of CuxO (x = 1 or 2), WO3, and V2O5. The chemical compositions may be expressed in a line diagram bounded by the two end-members (binary oxides) and the position of the ternary compound on the line dictates its stoichiometry. This is illustrated in Fig. 2 for several examples that have been most heavily investigated for their PEC performance as photoelectrodes. The Cu-V-O system in Figs. 2a and b, for example, features a rich array of compounds with varying stoichiometry and the A cation (Cu) in two different oxidation states. This has enabled an examination of their PEC properties as a function of the Cu:V ratio in the compound.23,24 The activity toward OER has been found to improve with decreasing Cu:V ratio. In general, while the bandgaps of these compounds are in the right range (1.8-2.0 eV), their PEC properties have much room for improvement. In this vein, alloying of +2 cations (e.g., Sr) onto the Cu site has been found to enhance the PEC activity. With The Materials Project database currently listing ~30 distinct structures in this system,25 these compounds represent the tip of the iceberg in regard to possible structures and compositions. In the related Cu-W-O system, CuWO4 (Fig. 2c) repairs two handicaps associated with the use of WO3 as a photoanode for solar water splitting: (a) it harvests longer wavelengths of the solar spectrum owing to its smaller bandgap; (b) it does not degrade under long-term irradiation in electrolytes with neutral pH as long as complexing ions (e.g., phosphate) are not present. Water photooxidation, however, is hindered by a large charge transfer resistance such that Jph is limited to only fractions of an mA/cm2.26 (See Table 1.) Nonetheless, the nearly quantitative Faradaic efficiency reported for OER bodes well for further optimization, and the improvement over WO3 constitutes a step in the right direction. While only CuWO4 is listed on this diagram, and which has been the focus in recent investigations, the predicted existence of 10 or more new compositions in this system portends a promising future path to tuning the CuO and WO3 components and understanding their relative impacts on the charge transfer resistance.25,26 Of all the ternary oxide photoelectrode material candidates explored to date, BiVO4 (Fig. 2d) has garnered the most attention. Initial studies revealed its surface to have very poor hole transfer efficiency, but this handicap has been partly remediated with the use of co-catalysts such as cobalt phosphate, FeOOH, or MnOx.27

Nonetheless, surface recombination is still a problem that must be further tackled with this material. (See Table 1.) Surface modification may prove to be a way out of this difficulty; for example, Jph has been boosted to ~2.7 mA/cm2 by chloride modification.28 Photocorrosion of BiVO4 is another concern; in-operando strategies for understanding and remediating photocorrosion pathways offer hope for the future. The foregoing discussion was only meant to provide a capsule summary of the promise offered by ternary and multinary oxide semiconductors. Other than the candidates identified here, there are many other families of ternary oxides (e.g., delafossite ABO2, perovskite ABO3) that are promising.18 We next turn to more fundamental solid state aspects associated with the materials in Fig. 2. In the subsequent section, the roles of the AOx and BOx components are analyzed from a solid state perspective.

Solid State Aspects of Ternary and Multinary Oxides

The PEC properties of semiconducting oxides are fundamentally determined by their crystalline structures and chemical compositions. The crystalline structure is, in turn, dictated by local and extended bonding configurations of the constituent components, such as for the AOx and BOx within an ABO2x composition. Thus, the choice of the different metal cations, as well as their relative molar ratios, has a significant influence on their PEC properties through concomitant changes in their crystalline and electronic structures. As discussed above, the many underlying and interdependent factors (e.g., atomic orbital energies, ionic radii, oxidation states) make it virtually impossible to dial in an optimal set of semiconductor PEC properties. Yet, much progress towards a deeper understanding of the key structure-property relationships is emerging. For example, the relative stoichiometric ratios of the AOx and BOx components generally influence whether the structure forms with either isolated AOx/BOx units or extended [-A-O-A-O-]n (n = repeating unit) and [-B-O-B-O-]n bonding, shown in Fig. 3. While the former leads to localization and trapping of the charge carriers, the extended bonding in the latter can yield the desired high majority carrier diffusion lengths in more delocalized band states owing to their greater dispersion. As a test case, in the Cu-V-O chemical system, the higher molar concentration of the V2O5 component in CuV2O6 (i.e., 1:1) leads to extended two-dimensional [-V-O-V-O-]n sheets, Fig. 3 (left). By comparison in Cu5V2O10, Fig. 3 (right), the higher CuO:V2O5 molar ratio of 5:1 gives a structure with only isolated VO4 tetrahedra but extended [-Cu-O-Cu-O-]n layers. Intermediate compositions nearer to a 1:1 metal ratio are more optimal for finding structures with extended bonding for both metal cations, such as is the case for CuWO4, Fig. 3 (middle). In this example, a wide band dispersion can occur in both the valence and conduction bands owing to the extended bonding of both [-Cu-O-Cu-O-]n and [-W-O-W-O-]n components that form as chains. This is one potential key to efficient charge separation of excited electrons and holes and transport over separate structural components. Many other solid state principles have also been discovered that demonstrate how the choice of multiple different metal cations, and thus the AOx and BOx components, can yield semiconductors with smaller bandgaps, greater band dispersion and charge carrier mobility, energetic tuning of deep versus shallow trap states, as well as tuning between n-type and p-type semiconducting behavior. An archetype oxide example results from the combination of two metal cations with a sum of oxidation states of +6 and Fig. 3. Crystalline structures with varying Cu: T. M. (T. M. = transition metal) atomic ratios and metalhaving the ABO3 composition. The choice oxide connectivity, including with extended vanadate layers in CuV2O6 (1:1; left), cuprate layers in Cu5V2O10 (5:1; right), and with both tungstate and cuprate chains in CuWO4 (middle).

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of two metal cations with compatible ionic radii (i.e., satisfying the Goldschmidt tolerance factor) can result in the ubiquitous perovskite-type structure, such as in highly studied n-type SrTiO3 films. Alternately, the combination of one transition metal with a d0-electron configuration (e.g., Ti(IV), V(V)) and another with a d10/ d10s2-electron configuration (e.g., Cu(I), Pb(II)) can yield a small bandgap, as found in CuNbO3 and PbTiO3 with bandgaps of ~2.0 eV and ~2.7 eV, respectively.29,30 Multiple metal cations can thus be used advantageously to satisfy many of the desired semiconductor PEC properties listed in Table 1. The challenging side of this approach is that semiconductors containing a combination of multiple metal cations can suffer from a high degree of both crystallographic anisotropy and order/disorder issues, shown in Fig. 4. Frequently, a low degree of symmetry is enforced upon the crystalline structure because of the disparate coordination preferences and connectivity of the separate AOx and BOx components. This is the case for the connectivity of the titanate and stannate chains in Sn2TiO4, illustrated in Fig. 4, as a result of the Ti(IV) and Sn(II) cations having dissimilar ionic radii and coordination preferences. The net consequences are large differences in charge carrier mobility and absorptivity with crystal orientation, e.g., such as only down the one-dimensional chains. Thus, highly anisotropic structures necessitate a favorable alignment of the directions of high carrier mobility within the photoelectrode film so that the majority and minority carriers can efficiently transport to the back contact and outer film surfaces, respectively. At the opposite extreme, completely disordered structures also occur, e.g., as solid solutions, when the multiple metal cations are sufficiently similar in chemistry. A representative example is Sn(Zr1-xTix)O3, Fig. 4 (right), with the Zr(IV) and Ti(IV) cations completely disordered over the same crystallographic sites of the perovskite structure because of their similar ionic radii and

coordination preferences. A significant amount of trapping and scattering of charge carriers would be expected in this case with high atomic-site disorder. Surprisingly, several solid-solution semiconductors show promisingly high photocurrents and photocatalytic activity, i.e., such as for BaTa(O2N) and (Ba1-xSnx) (Zr1-xTix)O3,31,32 with mixed anion and cation sites, respectively. This counterintuitive property emerges when the percolation thresholds of their bonding networks have been exceeded. Many such fundamental relationships remain to be discovered in these more complex systems.

Outlook and Prospects

The preceding discussion ought to make it abundantly clear that fascinating solid state chemistry lurks within the search spaces encompassing the elusive “perfect” inorganic semiconductor photoelectrode. While only the future holds the answer to whether we will ultimately succeed in this search, much progress would have been made regardless in our fundamental understanding of the structure-optoelectronic property correlations in solid state inorganic frameworks. Solid state sciences undeniably contributed handily to the search for high-temperature superconductivity and energy storage devices (e.g., Li ion batteries). It will not be a stretch to imagine a similar outcome in the area of solar water splitting. The ingenuity of the human mind and the inspiration derived from the rich history of scientific and technologic advances will surely drive future progress toward the goal of efficiently and persistently splitting water using sunlight.

Acknowledgement Paul A. Maggard gratefully acknowledges the support of this work from the National Science Foundation (DMR-2004455). © The Electrochemical Society. DOI: 10.1149.2/2.F07211IF.

Fig. 4. Comparison of the ordered structure of Sn2TiO4 with significant crystallographic anisotropy (i.e., one-dimensional), left, and the disordered structure of Sn(Zr1-xTix)O3 with percolation thresholds for site-to-site charge carrier diffusion, right. 50

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

About the Authors Krishnan Rajeshwar specialized in solid state chemistry for his doctoral degree at the Indian Institute of Science in Bangalore, India. After a postdoctoral stint at Colorado State University, Fort Collins, CO, he joined the faculty of the Department of Chemistry and Biochemistry at The University of Texas at Arlington. He is now a Distinguished University Professor at UTA. He is a past president of The Electrochemical Society, and a past editor of The Electrochemical Society Interface. His research interests span a broad spectrum in solid state chemistry, materials chemistry, and energy R&D. He has published some 400 papers in peer-reviewed journals, two monographs, and many chapters in these areas. This body of work has been cited ~ 22,000 times, and his h-index is 70. Rajeshwar has won many awards and recognitions (e.g., ECS Fellow, ETD Research Award, Electrodeposition Division Award). Very recently, he appeared in Stanford University’s World’s Top 2% Scientists list, ranked #95 in the energy category (https://data.mendeley.com/ datasets/btchxktzyw/2). He may be reached at rajeshwar@uta.edu. https://orcid.org/0000-0003-4917-7790 Paul A. Maggard earned his PhD in inorganic solid state chemistry at Iowa State University. Following a postdoctoral appointment at Northwestern University, he took a faculty position at North Carolina State University’s Department of Chemistry. Research efforts in his laboratory group center on the flux and hydrothermal synthesis of metal oxides and metal-oxide/organic hybrids for novel investigations into their catalytic, electronic, and photoelectrochemical properties for solar energy conversion. He currently holds the position of associate professor. Maggard has published >100 papers and book chapters and given a number of invited presentations. He has received several awards, including the NSF CAREER award, Beckman Young Investigator award, and Scialog award. Maggard may be reached at paul_maggard@ncsu.edu. https://orcid.org/0000-0002-3909-1590 Shaun O’Donnell obtained his BS degree in chemistry from Clemson University in 2017, where he studied halogen bonding in organoiodides under the direction of Prof. William T. Pennington. He is currently a PhD candidate in the research group of Prof. Paul A. Maggard at North Carolina State University. His current research is focused on photocatalytic oxides, with an emphasis on the synthesis of metastable Sn(II)-containing oxides using flux and ion-exchange techniques. Additional research interests include the synthesis and discovery of new materials and understanding structure-property relationships in solid state materials. He may be reached at scodonne@ncsu.edu. https://orcid.org/0000-0003-1487-4836

References 1. K. Rajeshwar, J. Appl. Electrochem., 37, 765 (2007). 2. K. Sivula and R. van de Krol, Nature Rev., 1, 1 (2016). 3. E. L. Miller, A. Deangelis, and S. Mallory, in Photoelectrochemical Hydrogen Production, R. van de Krol and M. Grätzel, Editors, p. 205, Springer, New York (2012).

4. C. Zachäus, F. F. Abdi, L. M. Peter, and R. van de Krol, Chem. Sci., 8, 3712 (2017). 5. K. T. Fountaine, H. J. Lewerenz, and H. A. Atwater, Nat. Commun., 7, 13706 (2016). 6. C. Jiang, R. Wang, and B. A. Parkinson, ACS Combi. Sci., 15, 639 (2013). 7. W. Yang, R. R. Prabhakar, J. Tan, S. D. Tilley, and J. Moon, Chem. Soc. Rev., 48, 4979 (2019). 8. H. He, A. Liao, W. Guo, W. Luo, Y. Zhou, and Z. Zou, Nano Today, 28, 100763 (2019). 9. Y. He, T. Hamann, and D. Wang, Chem. Soc. Rev., 48, 2182 (2019). 10. M. Tao, H. Hamada, T. Druffel, J. -J. Lee, and K. Rajeshwar, ECS J. Solid State Sci. Techol., 9, 125010 (2020). 11. D. E. Scaife, Solar Energy, 25, 41 (1980). 12. K. Sivula, F. Le Formal, and M. Grätzel, ChemSusChem, 4, 432 (2011). 13. A. Paracchino, V. Laporte, K. Sivula, M. Grätzel, and E. Thimsen, Nature, 10, 456 (2011). 14. K. Rajeshwar, R. McConnell, S. Licht, eds., Solar Hydrogen Generation, Springer-Verlag (2008). 15. L. M. Peter, H. J. Lewerenz, eds., Photoelectrochemical Water Splitting: Materials, Processes, and Architectures, RSC Publishing (2013). 16. J. Zheng, H. Zou, Y. Zou, R. Wang, Y. Lyu, et al. Energy & Environ. Sci., 12, 2345 (2019). 17. I. Sullivan, B. Zoellner, and P. A. Maggard, Chem. Mater., 28, 5999 (2016). 18. K. Rajeshwar, M. K. Hossain, R. T. Maculuso, C. Janaky, A. Varga, and P. J. Kulesza, J. Electrochem. Soc., 165, H3192 (2018). 19. O. Palasyuk, A. Palasyuk, and P. A. Maggard, J. Solid State Chem., 183, 814 (2010). 20. I. Sullivan, P. P. Sahoo, L. Fuoco, A. S. Hewitt, S. Stuart, D. Dougherty, and P. A. Maggard, Chem. Mater., 26, 6711 (2014). 21. L. Zhou, A. Shinde, D. Guevarra, J. A. Haber, K. A. Persson, J. B. Neaton, and J. M. Gregoire, ACS Energy Lett., 5, 1413 (2020). 22. M. K. Hossain, P. Sotelo, H. P. Sarker, M. T. Galante, A. Kormanyos, C. Longo, R. T. Macaluso, M. N. Huda, C. Janaky, and K. Rajeshwar, ACS Appl. Energy Mater., 2, 2837 (2019). 23. C.-M. Jiang, G. Segev, L. H. Hess, G. Liu, G. Zaborski, F. M. Toma, J. K. Cooper, and I. D. Sharp, ACS Appl. Mater. Interfaces, 10, 10627 (2018). 24. Q. Yan, J. Yu, S. K. Suram, L. Zhou, A. Shinde, P. F. Newhouse, W. Chen, G. Li, K. A. Persson, J. M. Gregoire, and J. B. Neaton, Proc. Natl. Acad. Sci., 114, 3040 (2017). 25. A. Jain, S. P. Ong, G. Hautier, W. Chen, W. D. Richards, S. Dacek, S. Cholia, D. Gunter, D. Skinner, G. Ceder, and K. A. Persson, APL Mater., 1, 011002 (2013); Website: https:// materialsproject.org (accessed: Dec. 30, 2020). 26. K. J. Pyper, J. E. Yourey, and B. M. Bartlett, J. Phys. Chem. C., 117, 24726 (2013). 27. D. K. Zhong, S. Choi, and D. R. Gamelin, J. Am. Chem. Soc., 133, 18370 (2011). 28. Z. Li, Q. Zhang, X. Chen, F. Yang, D. Wang, et al. ChemComm., 13153 (2020) 29. U. A. Joshi, A. M. Palasyuk, and P. A. Maggard, J. Phys. Chem., 115, 13534 (2011). 30. D. Arney, T. Watkins, and P. A. Maggard, J. Am. Ceram. Soc., 94, 1483 (2011). 31. M. Higashi, K. Domen, and R. Abe, J. Am. Chem. Soc., 135, 10238 (2013). 32. S. O’Donnell, C. -C. Chung, A. Carbone, R. Broughton, J. L. Jones, and P. A. Maggard, Chem. Mater., 32, 3054 (2020).

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Synthesis as a Design Variable for Oxide Materials by Jack Vaughey, Steve Trask, and Ken Poeppelmeier

Introduction

hen studying a new electrochemical couple, numerous variables affect how it is evaluated, how successful it is judged to be, and system properties. In the energy storage field, many researchers evaluate materials using performance metrics that might include capacity, rate capability, or cell impedance values to assess various cell chemistries. Behind these numbers are underlying attributes such as particle morphology, tap density, particle size, surface functionality, and even growth facet that are influenced by the method synthesis. These characteristics can carry through to the final product as the material is transformed into an electrode, high-surfacearea catalyst support, or a stand-alone sintered ceramic. In this article, the focus will be on, at a high level, how the synthesis procedure chosen and the variables that come with that choice influence the observed properties of the final product. For instance, while creating a material with the correct stoichiometry may be the goal, if it does not have the desired cation ordering or polytype, it may not be the final step in the materials creation.1,2 An example in the area of lithium ion batteries is Li(Mn1.5Ni0.5)O4, often called “5V spinel,” where the synthesis temperature used has an observable impact on the electrochemical response.3 This material contains two active redox metals (Mn, Ni) mixed over the octahedral site of the spinel structure. Depending on its annealing history, the transition metals in this material disorder if heated to 900°C (Space Group: Fd-3m) driven by a small reduction of some of the manganese or, when annealed at 700°C, the cations order (Space Group: P4332) over two related octahedral sites yielding only subtle differences in diffraction patterns, but notable differences in electrochemical discharge curves and performance.4,5 We will, at a high level, be examining the synthetic methods employed by researchers to create bulk electroactive or related materials, the advantages and disadvantages, synthesis design issues, and conclude with an analysis from the perspective of electrode creation. More indepth reports on specific materials, methodology reviews, or analysis can be found in the references and in the relevant literature.

Traditional Solid State Synthesis For commonly studied ternary lithium oxides, i.e., LiMn2O4, LiCoO2, the earliest studies relied on samples that were made by traditional solid state methods.6,7 In a typical reaction scheme, investigations are initiated with an evaluation of possible starting materials, their decomposition temperatures, purity, availability, and

decomposition pathway. For lithium-containing oxides, the most common lithium sources are lithium hydroxide hydrate or lithium carbonate due to their stability, availability, and active temperature range. The choice often comes down to issues associated with the temperature range used and matching the stability of the transition metal source. For early-stage research reactions, lithium hydroxide monohydrate is commonly chosen, however depending on lab storage conditions, the water content may be variable, adding an extra level of uncertainty to weight for stoichiometry-defined measurements. Once an early level of success has been achieved, albeit possibly, with small amounts of impurity or inhomogeneity, extra investments in time and effort will be necessary to achieve single-phase materials as lithia evaporation, reactions with crucibles, and non-stoichiometric starting materials may need to be compensated for in the reaction scheme. Similar concerns exist for other emerging alkali metal oxide systems, i.e., Na2O, K2O, where materials loss due to evaporation might also be expected, and utilization of a closed reaction system, for instance a sealed tube, may be required to maintain stoichiometry. For the transition metal cation source, variables that need to be considered include the possibility of having the correct oxidation states, coordination preferences, or identifying a viable precursor. A common first attempt may involve simply mixing and heating the binary oxide samples with a lithium source. (See Table 1.) These types of reactions are useful as information on phases present may also be mixed with information on kinetics, intermediate phase formation, the extent of lithium oxide losses to evaporation, cation mixing, or even the role of atmosphere. For transition metal oxides, two broad classes arise—ones that contain materials that have stable oxidation states under most non-reducing synthetic conditions (i.e., Sc+3, Ti+4) and ones where multiple oxidation states are accessible (i.e., Ni+2, Mn+3).

Stable Oxidation States

The most straightforward reactions are those that use and maintain metal cations in their most stable oxidation state. Solid state synthetic techniques utilize a choice of temperature, time at temperature, and in practice, crucible materials. Technologically important materials that fall into this category include solid state electrolytes, select oxide LIB anodes, and non-stoichiometric solid oxide fuel cell materials. The atmosphere is usually less critical as long as the temperature range is controlled and the materials are stable to evaporation. A recent example of this type of chemical control is the Mg-ion cathode MgCr2O4.8 This stable spinel phase is cubic and has a normal cation distribution with Mg+2 on the tetrahedral A-site. In this case, all of the components are in their normal and most stable oxidation state, and (continued on next page)

Table I. Commonly used lithium salts for the synthesis of lithium-containing oxides.

Lithium Salt

Temperature (melting or decomposition), °C

Comments

LiNO3

255 (m.p.), 600 (decomposes)

Decomposes with release of NOx, oxidizing agent.

LiOH • H2O

462

Exists in samples with LiOH, the bulk water content may be variable.

LiI

469

Iodine vapor is byproduct.

LiBr

550

Bromine vapor is a possible byproduct.

Li2[C2O4]

560 (decomposes)

Decomposes with gas release.

Li2CO3

723

Loss of CO2.

Li2SO4

859

Loss of SOx, sulfur-based impurities.

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Multiple Oxidation States

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the reaction can be run at >1000°C in the air as reduction to divalent chromium or chromium metal is unlikely. For these high-temperature reactions, the final product often has a morphology derived from the starting materials with additional particle size growth driven by particle fusion and sintering, yielding a wide range of particle sizes with non-uniform morphology. For MgCr2O4, starting with a low surface area, Cr2O3 leads to a surface-driven reaction that can take several days at 1000°C to come to completion with intermittent grinding. The reaction time can be shortened by using a transition metal oxide precursor compound, as with lithium salts above. Using a more reactive chromia source, such as Cr(NO3)3 ▪ 9H2O, produces a nanoscale Cr2O3 on heating (loss of water, loss of NOx) that shortens diffusion distances and greatly speeds up reactions, although for safety purposes, it should be done in a hood or similar well-ventilated work area. Combining the nanoscale chromia with a magnesia precursor such as Mg(OH)2 (or Mg(NO3)2) can yield a single-phase product in hours. Alternatives can be found by going slightly off stoichiometry where the excess melts at a lower temperature providing a slightly different reaction pathway. As long as the extra material can be removed, these flux reactions can dramatically speed up the process. A recent example is the spinel sulfide, MgCr2S4.9,10 Unlike the oxide, decomposition to binaries and loss of sulfur to evaporation as the temperature rises limits the window of stability. Thus, while the oxide analog can be heated to high temperature for a short while to form single-phase materials, the sulfide was found to have a window of stability between 800-900°C against mixtures of binary phases. In this window of stability, the synthesis was found to take several months with intermittent grinding. However, the addition of a small excess of MgS over the stoichiometric amount, acting as a flux, speeds up the reaction by various mechanisms that include (1) bringing a more active species to the interface, (2) refreshing the surfaces by removing product, or (3) possibly subtly shifting the reaction pathway, i.e., favoring formation at the interface of an intermediate. Alternatively, rapid synthesis of single-phase MgCr2S4 was recently achieved using a salt metathesis method by Muira et al., when they used the reaction between MgCl2 and NaCrS2 to form the desired phase driven, in part, by the formation of the very stable salt NaCl.10 A key aspect of these methods, also commonly used for crystal growth, is that after completion, the excess solid flux can be removed. For MgS, this can be done by a sulfuric acid wash that does not affect the desired MgCr2S4 spinel. With the metathesis reaction, water can be used to remove the salt. Besides fluxes, reactive precursors, and increased temperature, other synthetic avenues exist based on their redox stability during these diffusion-driven processes. Another commonly used tool is to reduce the particle size to the small micron or nanoscale range by techniques such as high-energy ball milling (HEBM) or going to nanoscale precursor particles. All seek to increase the surface areas and decrease the diffusion distances, leading to more rapid final product isolation on annealing.11,12 The nanocrystalline (or amorphous) phases produced tend to be more reactive, and upon heating, can rapidly convert to a more thermodynamically stable state, greatly reducing reaction times. If maintained at these sizes, isolation of metastable or interfacially stabilized materials can occur as surface atoms (often under-coordinated) are a much higher percentage of the material, and the observed properties may differ from the bulk-scale materials. More specific examples will be discussed as part of the following section.

While bulk materials with relatively invariant oxidation states hopefully represent more straightforward examples of solid state oxide synthesis, many technologically relevant phases contain cations that exist in multiple oxidation states. A relevant example is the simple ternary oxide and high-voltage cathode LiNiO2. On observation, the nickel is present in the trivalent state, while most precursors available to the researcher are divalent nickel. In an effort to oxidize the nickel uniformly, several issues need to be considered. The most straightforward oxidant is oxygen gas, which has the advantage then of being incorporated into the product as a needed additional anion, nominally forming Ni2O3.13 A known phase stable to ~600°C, but is often non-stoichiometric in oxide. Due to this nonstoichiometry, the phase is rarely used as a precursor. However, nickel oxyhydroxide, NiO(OH), is stable to ~260°C and often is far closer to being stoichiometric.14 In fact, rewritten as HNiO2 yields some insights to other synthetic pathways where the temperature stability can be maintained. Specifically, Palacin et al., noted that it could be ion-exchanged with LiOH to form LiNiO2 using a hydrothermal apparatus at 160°C.15 For the formation of a Ni(III) phase, a low surface area Ni(II) precursor may limit the ability of the gaseous oxygen to reach the core of the particle to oxidize the sample. The researcher needs to consider a phase that can form a high surface area nickel (II) oxide precursor, i.e., NiNO3, Ni(OH)2, as well as an oxidizing atmosphere, i.e., O2, in the presence of a lithium source. While trivalent nickel can form under the correct conditions, extra temperature stability can be found by the addition of basic cations to the lattice, which may have the effect of pushing electron density towards the higher valent cation, limiting decomposition pathways, or adding necessary bonding. In the case of LiNiO2 (or even Li2NiO3), oxide lattice stability has been observed to increase to over 700°C.16 Conversely, using air or even a nitrogen atmosphere often results in NiO or the disordered and electrochemically inactive (Li, Ni)O rock salt phase as these represent the most stable divalent nickel phases accessible in the reaction. On overheating or due to lattice instabilities on cycling to high voltage, nickel can be reduced at the interface, and this is often observed as a surface rock salt phase.17 Alternative methods to yield high surface area oxides that are commonly used in the laboratory include using reactive precursors that form nanoscale particles stoichiometrically in the reaction vessel. Classic examples of these methods include sol-gel chemistry, Pechini, and glycine-nitrate methods.18-20 In the glycine-nitrate method, nitrate salts are dissolved in water with glycine (a fuel), and on evaporation of the liquid, the decomposition of the nitrate triggers the glycine to burn, and local temperatures can reach >1000°C for a short period of time. This method is applicable to making nanoscale materials quickly, although the product is formed in an oxidative

Fig. 1. Typical setup for a CSTR reactor system. 54

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

environment, so typical products may contain metals in their higher oxidation states. For a sol-gel synthesis, for example, yttria-stabilized zirconia (YSZ), alkoxide salts, i.e., Zr(n-C3H7O)4, in the correct ratios are dissolved in supporting alcohol.18 The alcohol evaporates to form a gel. The gel then traps the dispersed cations in a matrix that upon heating and burnoff produces nanoscale oxide particles. These nanoscale particles, as with the glycine nitrate product above, are very reactive at temperature, and rapid formation of the product can be realized. Similarly, the Pechini method uses a mixture of cations dissolved in water, then chelated with a hydroxycarboxylic acid.19 The chelates are then cross-linked together with a polyalcohol to form a gel through esterification. As before, the gel is burned off to create the desired phase. For the LiNiO2 example above, moving towards hydroxide or other complex salt precursors is a method to generate nanoscale reactive species and increase the speed of the reaction relative to micron-sized metal oxide starting materials and ball-milling methods. A scale-up modification of the hydroxide precursor method that also yields morphology control is the continuously stirred tank reactor (CSTR).21 (A setup is shown in Fig. 1.) The product of these systems is a transition metal hydroxide precursor created with spherical morphology and controlled particle size. Under conditions of constant stirring, the transition metal solution is fed into the tank of a set pH, set by the addition of a metered amount of an ammonium hydroxide solution. The stirring process nucleates a spherical transition metal hydroxide of the composition of the stock solution. As the particle grows, it gradually is moved through the system and, at a certain size, is collected through a side discharge valve to an aging tank. The final hydroxide product is then isolated by filtration and materialspecific drying. A benefit of this method is the opportunity to make homogenously mixed transition metal hydroxide precursors, i.e. (Mn0.5Ni0.5)(OH)2, or by varying the flow controllers and having multiple source tanks, a gradient cathode composition can be created where the surface of the particle has a different composition than the core. Such a strategy has been used to counter capacity fade in some NMC cathodes where the surface may be more stable to the electrolyte and be Mn-rich, and bulk may have higher capacity and be Ni-rich.21 Besides direct synthesis from the oxides, numerous alternative methods have been developed and have been reviewed in more detail over the years. Many of these methods, including singlesource precursors (i.e., Ca0.5Mn0.5(CO3) + O2 r CaMnO3+ CO2), yield high-purity materials, but may be more product-specific or require synthetic skills outside the scope of this survey, although applications to new areas, including alkaline-earth battery systems, make these methods very useful.22-24

accomplished through liquid-phase transport, it is necessary to dissolve the precursors, unlike many of the previous examples where the materials may not be solubilized at the point of reaction. In order to predict if a metal oxide or hydroxide will dissolve, it is convenient to look at its acid-base behavior; basic oxides are soluble in acidic solutions and are typical compounds with a strong ionic character, such as the lanthanide sesquioxides or group 1 and 2 metal oxides.27 Acidic oxides, on the other hand, dissolve in basic media and are often covalent in character. Amphoteric oxides dissolve in both acids and bases. Transition metals oxides have different acidbase behavior based on their oxidation state, where higher oxidation states lead to more acidic behavior; as an example, chromium (II) oxide and manganese (II) oxide are basic, chromium (III) oxide and manganese (IV) oxide are amphoteric, and chromium (VI) oxide and manganese (VII) oxide are acidic. Fig. 2 shows a method for scaling up a hydrothermal reaction. In the reaction vessel, if there is no external pressure applied, the system is said to reach an “autogenous pressure,” which in the absence of a gas-producing reaction, is a function of the temperature, the solution, and the degree of filling in the vessel. At high filling percentages, the pressure is largely due to the expansion of liquid solution, but at low filling percentages and temperatures below the critical point, the pressure is primarily determined by the vapor pressure of the solution. It is fairly typical to assume that this solution is solely water in a hydrothermal reaction. However, this assumption is certainly never the case in practice. Raoult’s law notes that the partial pressure of a component is equal to the vapor pressure of the pure compound weighted by the mole fraction. The vapor pressure of the total solution depends on the vapor pressure of each component and the molar fractions thereof. As an example, when we add NaOH as a mineralizer, the vapor pressure of the solution increases with increasing temperature and decreases with increasing NaOH concentration.25 An example of the versatility of hydrothermal synthesis is the perovskite SOFC material LnMnO3 (Ln=lanthanide).27 As with the CSTR method noted previously, a distinct advantage of hydrothermal techniques is the ability to produce crystalline particles with controlled morphology. In the case of CSTR, the method is designed to produce spheres, whereas the higher temperatures of a hydrothermal system preserve the thermodynamic Wulff shape under the mild reaction conditions used or may produce a kinetic Wulff shape varying different processing parameters (e.g., temperature, pH, different reagents or concentrations thereof) or adding surfactants. The mild conditions and possibility of forming faceted crystallites make studying this approach for producing shaped-controlled materials (continued on next page)

Hydrothermal Synthesis Solvothermal synthesis is a technique in which reactions occur in a solution (water in the case of hydrothermal synthesis) inside a sealed vessel at temperatures greater than the boiling point of the solvent and pressures greater than atmospheric pressure. At these elevated temperatures, and with the addition of mineralizers (e.g., NaOH, Na2CO3, NaCl), soluble complexes are formed. Liquidphase transport of these reactants allows for nucleation and subsequent growth of a crystalline product. This method produces crystals at lower temperatures and on shorter timescales than typical solid state reactions as its reactions occur from soluble molecular species.25,26 An advantage of this method is its ability to produce crystalline particles with consistent morphology by controlling processing parameters, including temperature, pH, reagents, reagent concentrations, and the addition of surface modifying surfactants. Since nucleation of crystallites is often Fig. 2. High-Throughput Hydrothermal Synthesis. The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Vaughey et al.

(continued from previous page)

supports worthwhile. Synthesis of LnMnO3 has been demonstrated to occur under conditions that formed both LnOOH and Mn(OH)2. The formation of the more soluble and reactive LnOOH required the dehydration of Ln(OH)3, which either required higher temperatures or lower pressures. The presence of LnOOH and [Mn(OH)4]-1 led to the crystallization of the desired phase LnMnO3, with typical conditions of a reaction temperature of 225°C in a 2.5 M NaOH solution. For these types of materials, knowledge of the solution species is critical as it dictates the reaction mechanism, for example, polymerization, condensation, and growth by loss of water. For energy storage materials, some of the more common examples accessible by hydrothermal methods are phosphatebased cathodes, i.e., LiFePO4, ɛ-VOPO4. As above, these systems involved the solubilization of transition metal salts in the presence of a phosphate salt or phosphoric acid. By controlling pH, oxidation state, and pressure, phases can be formed that reflects the protonation of the phosphate anion. The three-dimensional ɛ-VOPO4 phase is an example where while it is a vanadium (V) compound, the material is more easily accessed hydrothermally as the protonated H2[VOPO4] (or kieserite-type VPO4▪H2O) vanadium (III) material and oxidized under oxygen to form the desired 2e- cathode material (with loss of water).28,29 In the case of the olivine material LiFePO4, the low-temperature nature of hydrothermal synthesis allows for a straightforward pathway to mixed cation systems, including other transition metals on the iron site, i.e., Mn, Co, Ni, or vanadium, as the [VO4]3- anion, on the phosphate site.30 By limiting the reactions to low temperature and solubilized precursors, more kinetically stabilized products can be isolated, and alternative reaction pathways can be isolated and explored.

The Influence of Synthesis on Electrode Preparation When a product is isolated, especially in the area of energy storage materials, its required form may not be the isolated powder or a single crystal but a format that takes into account its final use as a component of a system. A SOFC material may require high-temperature sintering to form a dense ceramic. For energy storage materials, a common needed form is a complex high porosity electrode that incorporates a

Fig. 3. EM images the various morphologies created using various synthetic processes. Images (a) are MoO2.8F0.2 plates and rods isolated from a hydrothermal reaction of MoO3 in a HF solution, (b) monodispersed SrTiO3 cubes from a hydrothermal reaction; (c) LiPF6 cubes grown by evaporation, and (d) a sphere of Cu6Sn5 produced by melt processing. 56

conductive additive, binder, and a current collector, typically a metal foil. For many end uses, optimized materials are integrated into the lamination process by matching the needed stability, morphology, or water sensitivity of the process to the supplied materials. (Fig. 3 highlights the morphologies of various materials isolated by various low-temperature methods.) A recent example is for NMC cathode materials, typically made using a CSTR (or related method) derived hydroxide, followed by a lithiation step and annealing. As researchers explore these types of materials, it is imperative that the synthesis route and resulting product have favorable characteristics for many of these steps needed to take the powder to the working electrode.31 For these materials, the first steps involve the formation of a slurry, a solid-liquid mixture that contains the needed electrode components in the correct ratio, as well as precursors to the binder and other needed additives. Once formulated and processed, the subsequent mixture is used to create a wet electrode, followed by drying and further analysis. While these materials may display promising electrochemical performance at small scales, the real practical value resides in their ability to be blended into a slurry, coated on the current collector at a pilot or industrial scale, to yield high-quality electrodes.32,33 The nature of scaling up promising powders often presents processing challenges that can be traced back to the initial synthesis and may need to be overcome. The same can be true for scaling up slurry preparation and electrode-coating methods relevant to industry (i.e., slot die or reverse comma methods). The production of a new powder is only the first step in taking a new discovery to the next level. For the slurry, a (non-exhaustive) list of electrode preparation properties include optimized rheology, uniform dispersion of all components (derived from surface chemistry), ability to form a homogenous material suspension, low hazard materials, uniform or bimodal particle sizes, and no tendency to form a gel from reactions with coating solvents. After the slurry has been created, a high-quality electrode laminate should have strong binder adhesion to the foil substrate, strong cohesion between particles, no visual imperfections (including streaks, agglomerates, poor edge retention, air entrapment, or ribbing), and uniform thickness of the foil substrate.32 After these variables are worked out, the ability to create an electrode with the desired thicknesses and proper amount of active material needed for the desired application is a critical deliverable to the end-user. Achieving these high-quality slurry and electrode characteristics, especially when working with lithium oxide-based powders, is dependent on the underlying materials’ properties and their synthesis. For these processes, a few rules of thumb characteristics of the powders should be considered when determining the material synthesis route and identifying the properties needed in the final product. For instance, the lithium oxide-based cathode powder should ideally have a pH in solution less than ~12. Observationally, above this value, the slurry has a tendency to undergo gelation during preparation with common casting solvents resulting in subpar electrode quality. An oxide material with a pH >12 could be an indication of residual surface compounds from the lithiation step (i.e., LiOH, Li2CO3) of the synthesis process. This has been noted several times for the lithium ion cathode materials, notably high lithium content lithiumrich cathodes and garnet solid electrolytes based on Li7La3Zr2O12.34 Besides surface chemistry issues, morphology plays a critical role in electrode formation. Ideally, an oxide powder where the secondary particles exhibit a spherical morphology and uniform size distribution will perform more favorably in the slurry preparation. These spherical particles favor a uniform material distribution throughout the slurry yielding desirable rheological behavior and higher packing density of the electrode coating. The oxide, while in a coating, could be prone to cracking during the calendaring (roll press) process, so designing the particle to inherently have a higher density increases the likelihood of maintaining its shape in this stage of the process. Besides processing advantages, once the coating is annealed, the packed spherical particles lead to an electrode product with gaps that allow for electrolyte infiltration. This would be in contrast to platelet particles, where their natural tendency to lay flat would limit electrode porosity without additional engineering inputs. There may be exceptions to these cause and effect characteristics, however, due to the rarity of these exceptions, it is advantageous to The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

account for the undesirable characteristics within synthesis design so that the limiting factor for industrial acceptance is not due to the lack of achieving a quality electrode coating within reasonable measures. Of course, there are ways to engineer around some of the issues noted earlier during the slurry preparation and coating stages; however, the challenges may persist even after engineering R&D remedies are exhausted. The success of a promising lithium oxide-based powder is one where the material properties, electrochemical performance, and transformation into a high-quality electrode all work together in one accord.

Summary The creation of material for any number of purposes often dictates how it can be used and how it can be modified for specific end use. Synthetically, understanding its inherent properties are a first step in choosing reagents, reaction conditions, and reaction containers. Variables that include time and temperature are the first step. Understanding the role of particle size, cation distribution, and the avoidance of alternate phases often define the methods reported in the literature. Lower temperature methods often yield more control over initial morphology, while higher temperature methods yielded more crystalline samples. In this contribution, we have noted some of the important variables that come into play for the various common synthetic methods that are employed by researchers. Once a product is made for many electrochemical applications, additional processing is needed to put it in a useable form. In the case of making electrodes, issues that can be controlled, such as morphology, secondary surface phases, and particle size, become critical variables to creating a quality electrode or monolith. Combining the skills of many researchers is required to understand the materials potential and its possibilities.

Acknowledgements Ken Poeppelmeier would like to thank the MRSEC program of the National Science Foundation (DMR-1720139) at the Materials Research Center of Northwestern University and the Soft and Hybrid Nanotechnology Experimental (SHyNE) Resource (NSF ECCS1542205) for support. Jack Vaughey and Steve Trask gratefully acknowledge support from the U.S. Department of Energy (DOE), Office of Energy Efficiency and Renewable Energy, Vehicle Technologies Office. The Argonne National Laboratory is operated for DOE, Office of Science, by UChicago Argonne, LLC, under contract number DE-AC02-06CH11357. © The Electrochemical Society. DOI: 10.1149.2/2.F08211IF.

About the Authors Jack Vaughey is a senior scientist and the Interfacial Materials Group leader in the Electrochemical Energy Storage theme of the Chemical Sciences and Engineering Division at Argonne National Laboratory. He received his PhD from Northwestern University in inorganic chemistry. After postdoctoral positions with Allan Jacobson (Houston) and John D. Corbett (Ames Laboratory), he joined the Chemical Engineering Division’s Battery Materials Group at Argonne National Laboratory. His materials discovery work at Argonne has centered on the synthesis and characterization of electroactive materials, including lithium-rich NMC cathode materials, intermetallic anodes, organic flow batteries, solid electrolytes, multivalent cation-based energy storage systems, and silicon-based anode materials. He has been a longtime member of The Electrochemical Society, has organized several symposia at national ECS meetings, and presently serves as an at-large board member in the Battery Division. He has published ̴ 200 papers in peer-reviewed journals, has been cited ~ 17,500 times, and his h-index is 64. In 2008, Jack was awarded the Outstanding Mentor Award from the U.S. Department of Energy, Office of Science, and in

2018 was named an AAAS Fellow (Chemistry). At Argonne, Jack has leadership positions in ReCell (a multi-lab effort to enable battery recycling), the Silicon Consortium Program (a multi-lab effort to understand Si anode chemistry), and was the writing lead for the proposal that created the JCESR Science Program in 2011-2012. He may be reached at vaughey@anl.gov. https://orcid.org/0000-0002-2556-6129 Steve Trask has over 10 years of experience in advanced battery technology research and development activities. He has extensive expertise in making slurries and fabricating electrodes using novel advanced lithium ion battery chemistries. These electrodes are utilized across multiple DOE-VTO programs. He investigates and mitigates chemical, electrochemical, and materials problems related to slurry, electrode, and cell/battery development, as well as optimizes electrode formulations and cell fabrication techniques. Steve plans and conducts electrochemical tests and analyzes data from prototype batteries and their components using a variety of laboratory instrumentation. He has a Master of Materials Chemistry degree. Steve has been published in over 30 publications. In 2018, his team received the Physical Sciences and Engineering Excellence Award from Argonne, and in 2020, the DOE Vehicle Technologies Office recognized Steve’s capabilities by awarding him a team award as part of Argonne’s Cell Analysis, Modeling, and Prototyping (CAMP) Facility. He may be reached at trask@anl.gov. https://orcid.org/0000-0002-0879-4779 Ken Poeppelmeier is a Charles E. & Emma H. Morrison Professor of Chemistry at Northwestern University. His team's research emphasizes the connections between the synthesis and structure of new materials, the physical properties of new materials, and the technological advances that result from these discoveries. Inorganic materials that have unusual structures often exhibit interesting chemical and physical characteristics. For example, layered materials exhibit a wide variety of important technological uses because they offer a unique crystalline architecture that can be designed to achieve specific material properties. His team's research in these areas, ranging from discovering new battery materials to the growth of single crystals, is part of an interdisciplinary research program that involves the collaboration of physicists, materials scientists, and chemists. He has published ~500 papers in peer-reviewed journals, has been cited ~ 24,000 times, and his h-index is 76. He is director of Northwestern’s Center for Catalysis and Surface Science and was a longtime editor of the ACS journal Inorganic Chemistry. He may be reached at krp@ northwestern.edu. https://orcid.org/0000-0003-1655-9127

References 1. Post, J. E. “Manganese Oxide Minerals: Crystal Structures and Economic and Environmental Significance,” Proceeding of the National Academy of Sciences, 96, 3447 (1999). 2. Shen, Y. F., Zerger, R., Deguzman, R., Suib, S., McCurdy L., Potter, D. I., O’Young, C. “Manganese Oxide Molecular Sieves– Preparation, Characterization, and Applications,” Science, 260, 511 (1993). 3. Ooms, F. G. B., Kelder, E., Schoonman, J., Wagemaker, M., Mulder F. “High-Voltage LiMgxNi0.5-xMn1.5O4 Spinels for Li-Ion Batteries,” Solid State Ionics, 152-153, 143 (2002). 4. Liu, J. Huq, A., Moorhead-Rosenberg, Z., Manthiram, A., Page, K. “Nanoscale Ni/Mn Ordering in the High Voltage Spinel Cathode LiNi0.5Mn1.5O4,” Chemistry of Materials, 28, 6817 (2016).

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5. Manthiram, A., Chemelewski, K., Lee, E. S. “A Perspective on the High-Voltage LiNi0.5Mn1.5O4 Spinel Cathode for Lithium-Ion Batteries,” Energy and Environmental Science, 7, 1339 (2014). 6. Mizushima, K., Jones, P. C., Wiseman, P. J., Goodenough, J. B. “LixCoO2 (0<x<1): A New Cathode Materials for Batteries of High Energy Density,” Materials Research Bulletin, 15, 783 (1980). 7. Thackeray, M., Johnson, P. J., DePicciotto, L., Bruce, P., Goodenough, J. B. “Electrochemical Extraction of Lithium from LiMn2O4,” Materials Research Bulletin, 19, 179 (1984). 8. Kwon, B.-J., Lau, K.-C., Park, H. Wu, Y., Hawthorne, K. L., Li, H., Kim, S.-J., Bolotin, I., Fister, T. T., Zapol, P., Klie, R. F., Cabana, J., Liao, C., Lapidus, S., Key, B., Vaughey, J. T. “Probing Electrochemical Mg-Ion Activity in MgCr2-xVxO4 Spinel Oxides,” Chemistry of Materials, 32, 1162 (2020). 9. Wustrow, A., Key, B., Phillips, P. J., Sa, N., Lipton, A., Klie, R. F., Vaughey, J. T., Poeppelmeier, K. R. “Synthesis and Characterization of MgCr2S4 Thiospinel as a Potential Magnesium Cathode,” Inorganic Chemistry, 57, 8634 (2018). 10. Miura, A., Ito, H., Bartel, C., Sun, W., Rosero-Navarro, N., Tadanaga, K., Nakata, H., Maeda, K., Ceder, G. “Selective Metathesis Synthesis of MgCr2S4 by Control of Thermodynamic Driving Forces,” Materials Horizons, 7, 1310 (2020). 11. Jansen, A. N., Clevenger, J. A., Baebler, A. M., Vaughey, J. T. “Variable Temperature Performance of Intermetallic LithiumIon Battery Anode Materials,” J. Alloys and Compounds, 509, 4457 (2011). 12. Hu, L., Jokisaari, J., Kwon, B.-J., Yin, L., Kim, S.-J., Park, H., Lapidus S., Klie, R. F., Key, B., Zapol, P., Ingram, B. J., Vaughey, J. T., Cabana, J. “High Capacity for Mg2+ Deintercalation in Spinel Vanadium Oxide Nanocrystals,” ACS Energy Letters, 5, 2721 (2020). 13. Sai, B., Gopchandran, K. G., “Nanostructured Mesoporous Nickel Oxide Thin Films,” Nanotechnology, 18, 115613 (2007). 14. Barde, F., Palacin, M. R., Chabre, Y., Isnard, O., Tarascon, J.M. “In Situ Neutron Powder Diffraction of a Nickel Hydroxide Electrode,” Chemistry of Materials, 16, 3936 (2004). 15. Palacin, M. R., Larcher, D., Audemer, A., SacEpee, N., Amatucci, GG, Tarascon, J.-M. “Low-Temperature Synthesis of LiNiO2–Reaction Mechanism, Stability, and Electrochemical Properties,” J. Electrochem Soc., 144, 4226 (1997). 16. Li, W., Reimers, J., Dahn, J. “In-Situ X-Ray Diffraction and Electrochemical Studies of Li1-xNiO2,” Sol. State Ion. 67, 123 (1993). 17. Abraham, D. P., Twesten, R. D., Balasubramanian, M., Petrov, I., McBreen, J., Amine, K. “Surface Changes on LiNi0.8Co0.2O2 Particles During Testing of High-Power Lithium-Ion Cells,” Electrochemical Communications, 4, 620 (2002). 18. Hench, L., West, J. “The Sol-Gel Process,” Chem Rev., 90, 33 (1990). 19. Lin, S.P., Fung, K. Z., Hon, Y. M., Hon, M. H. “Crystallization Mechanism of LiNiO2 Synthesized by Pechini Method,” J. Crystal Growth, 226, 148 (2001).

20. Check, L., Pederson, L., Maupin, G., Bates, J., Thomas, L., Exarhos, G., “Glycine Nitrate Combustion Synthesis of Oxide Ceramic Powders,” Materials Letters, 10, 6 (1990). 21. Wang, D., Belharouak, I., Ortega, L., Zhang, X., Xu, R., Zhou, D., Zhou, G., Amine, K. “Synthesis of High Capacity Cathodes for Lithium-Ion Batteries by Morphology-Tailored Hydroxide Co-Precipitation,” J. Power Sources, 274, 451 (2015). 22. Leonowicz, M. E., Poeppelmeier, K. R., Longo, J. “Structure Determination of Ca2MnO4 and Ca2MnO3.5 by X-Ray and Neutron Studies,” J. Solid State Chem., 59, 71 (1985). 23. May, C. D., Vaughey, J. T. “New Cathode Materials for SilverBased Primary Batteries: AgCuO2 and Ag2Cu2O3,” Electrochem. Communications, 6, 1075 (2004). 24. Wang, X., Zhang, H., Sinkler, W., Poeppelmeier, K. R., Marks, L. D. “Reduction of Magnesium Orthovanadate Mg3(VO4)2,” J. Alloys and Compounds, 270, 88 (1998). 25. Sheets, W., Mugnier, E., Barnabe, A., Marks, T. J., Poeppelmeier, K. R. “Hydrothermal Synthesis of Delafossite-Type Oxides,” Chemistry of Materials, 18, 7 (2006). 26. Hu, L., Wang, C., Lee, S., Winans, R., Marks, L. D., Poeppelmeier, K. R. “SrTiO3 Nanocuboids from a Lamellar Microemulsion,” Chemistry of Materials, 25, 378 (2013). 27. Stampler, E. S., Sheets, W., Prellier, W., Marks, T. J., Poeppelmeier, K. R. “Hydrothermal Synthesis of LnMnO3 (Ln = Ho-Lu and Y): Exploiting Amphoterism in Late Rare-Earth Oxides,” J. Mat Chem., 19, 4375 (2009). 28. Vaughey, J. T., Harrison, W. T. A., Jacobson, A. J., Goshorn, D. P., Johnson, J. W. “Synthesis, Structure, and Properties of Two New Vanadium (III) Phosphates: VPO4▪H2O, and V1.23(PO4) (OH)0.69(H2O)0.31▪H2O,” Inorganic Chemistry, 33, 2481 (1994). 29. Lin, S. C., Vaughey, J. T., Harrison, W. T. A., Dussack, L., Jacobson, A. J., Johnson, Jack W. “Redox Transformations of Simple Vanadium Phosphates: The Synthesis of ϵ-VOPO4,” Solid State Ionics, 84, 219 (1996). 30. Hong, J., Wang, C. S., Chen, X., Upreti, S., Whittingham, M. S “Vanadium Modified LiFePO4 Cathode for Li-Ion Batteries,” Electrochemical and Solid State Letters, 12, A33-A38 (2009). 31. Lipson, A. L., Durham, J. L., LeResche, M., Abu-Baker, I., Murphy, M. J, Fister, T. T., Wang, L. X., Zhou, F., Liu, Lei, Kim, K., Johnson, D. “Improving the Thermal Stability of NMC622 LiIon Battery Cathodes through Doping During Coprecipitation,” ACS Appl Materials and Interfaces, 12, 18512-18518 (2020). 32. Rodrigues, M. T. F., Kalaga, K., Trask, S. E., Shkrob, I. A., Abraham, D. P. “Anode-Dependent Impedance Rise in Layered-Oxide Cathodes of Lithium-Ion Cells,” Journal of The Electrochemical Society, 165, A1697 (2018). 33. Robertson, D. C., Flores, L., Dunlop, A. R., Trask, S. E., UsseglioViretta, F. L .E. Colclasure, A. M., Yang, Z. Z., Bloom, I. “Effect of Anode Porosity and Temperature on the Performance and Lithium Plating During Fast-Charging of Lithium-Ion Cells,” Energy Technology, 202000666 (2020). 34. Johnson, C. S., Kang, S.-H., Vaughey, J. T., Pol, S. V., Balasubramanian, M., Thackeray, M. M. “Li2O Removal from Li5FeO4: A Cathode Precursor for Lithium-Ion Batteries,” Chemistry of Materials, 22, 1263 (2010).

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Electrodeposition as a Powerful Tool for the Fabrication and Characterization of Next-Generation Anodes for Sodium Ion Rechargeable Batteries by Nathan J. Gimble,* Kelly Nieto,* and Amy L. Prieto Introduction

Electrodeposition

s the number of markets, as well as the overall market size, for rechargeable batteries continues to grow, it is clear that there is no one perfect battery to suit every application. In the best case, we would have batteries that store a very large amount of energy per unit mass or volume (energy density), can charge and discharge very quickly (power density), can cycle many times with very low loss of efficiency (cycle life), and are safe. Ideally, such a battery would be made from Earth-abundant, recyclable, sustainably mined or made materials, and could be scaled using inexpensive, safe manufacturing. There is, as of now, no such battery. Because we do not have a battery that is one size fits all, the wide range of potential applications for energy storage is a significant driving force for discovering and implementing a diversity of new battery chemistries to meet a wide range of requirements. In this Interface article, we describe the use of electrodeposition as a synthesis method for battery materials to enable and accelerate the design, understanding, and optimization of electrodes for sodium ion and sodium metal rechargeable batteries for applications where cost is more important than the overall weight of the battery. Elemental sodium is an attractive alternative to lithium for battery applications because it has a significantly higher abundance relative to lithium, good global distribution, lower cost, and a standard reduction potential near that of lithium (-3.04 V for Li/Li+ and -2.71 V for Na/Na+).1 Currently, the chemistries developed for cathodes, anodes, and electrolytes for Na-ion batteries are not nearly as well developed or understood as those of Li.2–4 A common approach to Na-ion research involves screening the top candidates from Li-ion battery technologies for use in Na-ion systems. This strategy is not effective because Li and Na exhibit surprisingly different chemistries. For example, the most common anodes for Li-ion batteries, graphite, and silicon, have negligible capacities for Na.5 Although pure Na metal is amenable to electroplating and stripping (a requirement for using the pure metal as an anode), it is highly reactive and unstable in common Li-ion electrolytes. Developing guidelines to accelerate the discovery and understanding of next-generation Na-ion anode materials for sodium ion batteries is crucial for the field to progress. In order to understand each novel electrode, one must endeavor to identify the intermediate structures and their corresponding properties as the anode is cycled. Through this process, a more thorough understanding of the degradation mechanisms can be gained to optimize the anode’s performance. One challenge with Na-ion batteries is that understanding how a material reacts with sodium by itself is not sufficient; the complex interactions with all components of the battery are important. Herein, we describe how electrodeposition as a synthetic technique allows for the fundamental investigation of the intrinsic properties of anode materials that can enable precise structure-property measurements and access to energy-dense three-dimensional electrodes for the application of sodium ion batteries in energy storage systems.

The fabrication of electrodes for battery applications plays a crucial role in optimizing battery performance and, more importantly, impacts how one can study the intrinsic properties of the electrode material. Many different fabrication methods are employed to study the performance and structure-property relationships of electrode materials, such as slurry casting, sputtering, and electrodeposition.6–9 The method of making electrode materials directly affects the structure-property relationships observed while cycling as the same target electrode can be made using different additives and binders. In slurry casting, polymeric binders and amorphous carbon additives are required to cast thin-film electrodes. Although these binders and additives can enable improved cycling performance, they add inactive mass and can hinder the ability to study the intrinsic properties of the active material as they convolute the electrochemical and structural data. Sputtering can produce crystalline thin films directly, which can help remove issues related to deconvoluting observed data, but it can be expensive and slow, which is a challenge to employ at commercial levels.6,10,11 Electrodeposition is the process of depositing metal ions or complexes on the surface of a conductive substrate in solution by applying an electric current and eliminates the need for binders and additives. In Figs. 1 and 2, we describe a typical process flow in our lab for the synthesis and characterization of anode electrodes. In Fig. 1, part 1, a common setup for electrodeposition is pictured, in which the copper foil acts as the working electrode, or cathode, where the metal ions from the solution are reduced. All three electrodes are immersed in a solution containing the metal ion/complexes and/or solution additives. By connecting the electrodeposition set up to a potentiostat, chronoamperometry or chronocoulometry can be used. This means that either a potential can be applied, and the current measured, or a constant current can be applied, and the potential measured. By controlling these variables, the thickness and loading of the reduced metal can be tuned, as shown in Fig. 1, part 2a. Although additives are not required, they can still be incorporated via wellestablished co-deposition methods. Through either co-deposition or stepwise deposition, additives such as carbon nanotubes, trace amounts of other metals, or other inorganic components can be incorporated into the electrode to enhance electronic conductivity or maintain mechanical stability as the electrode is cycled.9 We hypothesize that by directly electrodepositing active electrode material, all processes, whether interactions in the bulk of the electrode structure or at the electrode/current collector or electrode/ electrolyte interface, can be correlated directly to the material in question. The samples made by direct electrodeposition onto a current collector can help probe and understand reactions previously masked by slurry cast composites. Additionally, electrodeposited thin films are amenable to being characterized by a host of methods, including structural characterization using X-ray and electron diffraction, as well as spectroscopies including IR and Raman spectroscopy, X-ray photoelectron spectroscopy, and optical imaging methods.

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Complementary characterization methods are particularly useful when the products deposited are amorphous or contain multiple phases. To study the intrinsic properties of the electrodeposited active material, the film can be cycled in different cell configurations, such as a Swagelok cell, as shown in Fig. 1, part 3. Thus, the process from electrodeposition to cycling can easily be done to not only quickly create electrodes with different parameters for testing (thickness, mass loading, morphology, etc.), but can also be scaled to make multiple electrodes with the same parameters to test other battery components such as electrolyte composition. The cell can then be tested in a battery cycler, shown in Fig. 2, part 4, where the cell can be charged and discharged either using constant current conditions, to set voltage limits, or by applying a voltage and measuring current. If the mass of the sample is known, and the number of electrons is known per process (e.g., sodiation), the specific capacity can be determined for that electrode. From these experiments, a wide range of data can be collected to inform an understanding of cycle life, rate capabilities, cell capacity, and degradation mechanisms. One of the most common forms of data analysis is to evaluate a voltage profile plot, as shown in Fig. 2, part 5. Voltage profiles allow the capacity to be measured, and a plateau on the curve signifies an electrochemical reaction is occurring, meaning specific electrochemical reactions can be directly correlated to changes in cell capacity. The capacity of the cell can then be plotted for each cycle, allowing degradation or a drop in capacity of the cell to be observed. A follow-up technique that can be used to study and understand changes in electrode materials with cycling is differential capacity analysis, seen in Fig. 2, part 6. In a differential capacity plot, more information can be obtained about the sodiation/desodiation events occurring over a potential range than in the voltage profile of the cell. The features that appear as plateaus in a voltage profile are visualized as peaks in a differential capacity plot, making subtle changes in slope (corresponding to changes in chemical processes) more easily observed. Differential capacity plots represent a fingerprint that highlights conversion reactions, cell degradation, kinetic bottlenecks, and changes in chemistry that otherwise might not be seen in a voltage profile or the cycle lifetime analysis. While electrodeposition is a useful method to fabricate electrodes, the composition of the electrode should still be carefully probed not only to understand the properties of the active material but also to

investigate the incorporation of unwanted compounds. In deposition solutions, there often are metal oxides, complexing agents, and other surfactants that may be incorporated into the film during or after electrodeposition. Typically, the inclusion of these species is minimal, but it is still important to consider whether these species are affecting the performance and electrochemical reactions seen when the electrode is cycled. Multiple studies have shown that the incorporation of metal oxides can alter the electrochemical performance of electrodes and can cause alternative degradation methods.12–14 Therefore, it is crucial to understand the solution chemistry involved in the electrodeposition of active material before claiming to study the true intrinsic properties of the target material.

3D Architectures

The synthetic technique of electrodeposition not only enables the observation of the intrinsic properties of electrode materials without binder and additives, but it also allows for the synthesis of various architectures, such as thin films, nanowire arrays, and porous three-dimensional (3D) structures, as seen in Fig. 1, part 2b. These 3D structured electrodes achieve higher rate performance, which can translate to high power density for an electrode. The use of 3D architectures can be particularly effective at helping to control mechanical stress in electrodes that change volume significantly upon sodiation and desodiation. Most studies have focused on incorporating porous carbon-based composites to access the benefits of 3D electrodes, but it has been reported that these carbon structures can have unwanted reactions with the electrolyte in the cell. Other techniques that incorporate scaffolds as the base template require intricate procedures and etching with acid to create the final electrode structure and are prohibitively complex to move to commercial scales. Electrodeposition bypasses these issues, as additives and binder are not required. Specific examples produced by various groups include the electrodeposition of antimony-based alloys on 3D copper substrates, porous nickel scaffolds, and as self-supported prisms.15–18 All of these examples use electrodeposition to grow antimony or tin antimonide onto conductive substrates with minimal workup and without binders and additives, demonstrating how electrodeposition allows for the simple fabrication of 3D electrodes with significantly improved rate, performance, and capacity. The ability to electrodeposit active material onto 3D architectures has shown significant promise in the advancement to create energy-dense electrodes, but fundamental studies on how these structures affect the electrochemical reactions of anode materials are still required. Some inherent issues present in these advanced structures are non-uniform current and voltage distribution, which can lead to uneven sodiation and desodiation reactions across the electrode.19,20 Thus, the implementation of varying 3D architectures will greatly influence which crystalline and amorphous phases are formed when cycled due to differences in mechanical integrity, diffusion pathways and lengths, and surface areas. Therefore, it is crucial to employ the step process shown in Figs. 1 and 2 to screen how different architectures impact the sodiation/desodiation reaction mechanism of anode materials. The extra surface area that comes from a 3D electrode structure leads to the significant buildup of the solid electrolyte interphase (SEI), which forms when an electrode is in contact with an electrolyte that decomposes at the voltage limits Fig. 1. Schematic of our general process flow, beginning with (1) the electrodeposition of thin films of necessary for sodiation or desodiation. materials of interest from solution, which can either be (2a) deposited with controlled thickness to control The SEI is a mixture of organic and the amount of active material on the electrode or co-deposited with materials such as carbon nanotubes, inorganic species on the surface of the or (2b) directly deposited onto or into various 3D structures and templates. Then we can (3) directly battery electrode, which can shorten battery incorporate those active electrodes into Swagelok cells to test their electrochemical performance. 60

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Fig. 2. Once a Swagelok cell is put onto the (4) cycler, experiments such as (5) applied current, measured voltage can be used to identify at what voltages particular transformations occur, and that data can be converted to (6) the differential capacity as a function of voltage in order to identify subtle changes in the phases that are formed.

lifetime through impeding ion transfer and contribute to mechanical pulverization.21,22 Furthermore, in the case of the 3D battery, over multiple cycles, the SEI can obliterate the morphology of the anode through excessive growth (Fig. 3, left).23 The electrolyte additives fluoroethylene carbonate (FEC) and particularly vinylene carbonate (VC) commonly used in Li-ion battery electrolytes can help control the SEI formation to extend the cycle life of high surface nanowire systems (Fig. 3, right), but these effects are not well understood. The uncontrolled growth of SEI must be overcome in order to successfully implement high surface area, high loading architectures. It is important to recognize that although one action can be beneficial to one area of the battery; it can have negative consequences on other components, as the whole cell is interconnected. Therefore, before advancing further to full cells, one must understand the impact 3D architectures have on the SEI formation and if there are methods to better understand electrolyte degradation on the surfaces of these advanced structures.

The Importance of Liquid Electrolytes The same electrolyte additives, FEC and VC, used in Li-ion battery systems to increase battery lifetime, are also capable of functioning in Na-ion battery systems.23,24 Similar to electrode materials, the sodium

electrolyte has been adapted from equivalent lithium systems.25,26 While the SEI has been well studied to understand the beneficial properties of electrolyte additives, there has not been a complete characterization of its composition, which limits the ability to generate design guidelines for next-generation electrolytes. The SEI is a difficult system to study as it consists of a small concentration of air-sensitive products deposited on an electrode surface.21,27 The SEI products are subject to extreme potentials and may be evolving with the charge and discharge of the battery. Furthermore, techniques to study the SEI are ex-situ and, in taking apart a battery to characterize the anode’s surface, the SEI may be changed, and soluble species may wash away. X-ray photoelectron spectroscopy (XPS) is the most accessible surface-sensitive technique to study SEI species, but airfree infrared spectroscopy and solid state nuclear magnetic resonance are used as well. Altogether, direct characterization of SEI species is limited by the few comprehensive in-situ techniques. The results of these different characterization tools can be more clearly understood with electrodeposited electrodes as the data would be the result of the interaction of the electrolyte with a pure, additive-free active surface. Due to its simplicity, a half-cell design with a sodium metal pseudo-reference counter electrode is typically used to evaluate the anode performance of new sodium electrodes and 3D architectures. (continued on next page)

Fig. 3. Adapted with permission from Jackson et al. 2016. Depicted on the left are SEM images of Cu2Sb nanowire arrays after 100 cycles with (a) 5% FEC, (b) 5% VC and 250 cycles with (c) 5% FEC, and (d) 5% VC. On the right, a graph of capacity vs. cycle number for Cu2Sb nanowire array anodes cycled in half cells between 0.10 and 1.60 V vs. Li/Li+ either with no additive (red), 5% FEC (blue), or 5% VC (green). The square symbols are lithiation capacity and circles are delithiation capacity. The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Gimble et al.

(continued from previous page)

Fig. 4. Adapted from Pfiefer et al. 2019 with permission. These are four images of sodium metal placed in battery electrolyte (a) immediately after addition in ECDMC with NaClO4 that is representative of the other electrolytes tested and (b) in EC-DMC NaClO4, (c) in PC NaClO4, and (d) in EC-DMC NaPF6 after three days.

Alkali metals form a passivation layer upon immersion in the electrolyte; sodium is more reactive than lithium, which means that a thicker passivation layer forms on sodium.2 The passivation layer, which does not have the same impact in lithium, affects the quality of sodium metal as a reference electrode in a half-cell. Specifically, electrochemically active decomposition products can cause erroneous signals in sodium ion cells.28 The passivation of sodium metal further complicates understanding the performance of electrode materials cycled in a half-cell configuration. Sodium metal soaked in battery electrolyte has been shown to cause a color change in common liquid electrolytes, implying a change in the bulk electrolyte, not just passivation of the metal surface (Fig. 4).4 A color change in the electrolyte implies that the starting material for SEI formation includes unknown decomposition products. A significant area of research for sodium-based batteries is focused on understanding the role of the additive FEC in the passivation of sodium metal and how that impacts battery lifetime. To our knowledge, no complete characterization of electrolyte decomposition products has been performed. Again, this is due to a lack of specialized techniques for examining a difficult multiphase dynamic system. Nevertheless, there is a need for carefully controlled experiments to understand the identity of the spontaneous reaction products and the properties they have when dissolved in the electrolyte and deposited on the surface of an electrode. The study of new electrodes may also implement alternatives to the use of sodium metal in half-cells. Full cells are a logical choice; however, good sodium cathode materials are limited. Symmetric cells, which involve using a pre-sodiated anode material cycled against an unsodiated electrode, may be another alternative. Finally, a recent article by Lee et al. proposes the use of a silver ion reference electrode to help alleviate the problems the sodium counter electrode has as a pseudo reference.29

Conclusion As the understanding of the reactivity of liquid electrolytes used for sodium ion batteries is in its infancy, the use of directly electrodeposited materials for active electrodes is an ideal platform for probing, characterizing, and then understanding libraries of liquid electrolytes and additives that could be used to significantly improve the overall performance of new materials for sodium-based batteries. What we have highlighted in this article is that while electrodeposition of electrode materials for batteries can be a useful synthetic method, it is also an enabling technology for studying the fundamental structure and properties of these materials in the absence of complications with binders, and can be used to generate higherorder architectures for batteries.

Acknowledgements This work was funded by NSF SSMC-1710672. We thank Jeffrey Ma for helpful discussions about sodium battery chemistry. © The Electrochemical Society. DOI: 10.1149.2/2.F09211IF. 62

About the Authors Nathan J. Gimble is a PhD candidate at Colorado State University, where he does analytical and electrochemical research under Dr. Amy L. Prieto. His work is focused on developing a fundamental understanding of the formation of the solid electrolyte interface (SEI) in sodium ion batteries. Specifically, he is measuring electrochemical events in sodium ion batteries and correlating them to the formation of SEI species detected on the surface of pure phase electrodeposited anode surfaces using X-ray photoelectron spectroscopy. He works on other projects with collaborators related to battery electrolyte decomposition. He received a BA in chemistry from The College of Wooster, working closely with Dr. Karl Feierabend. He may be reached at nathan.gimble@colostate.edu. https://orcid.org/0000-0003-0816-5291 Kelly Nieto is a PhD candidate in materials chemistry at Colorado State University under the mentorship of Dr. Amy L. Prieto. She received her BS in chemistry from Texas A&M University in 2018, where she studied materials for the application of building energy efficiency and photocatalysis under the guidance of Dr. Sarbajit Banerjee. Nieto’s graduate research focuses on understanding structure-property relationships of antimony-based anode materials for Na-ion batteries. Her work also focuses on understanding the impact electrode fabrication methods and 3D architectures have on the electrochemical properties and structural changes of alloy-based battery materials. She can be reached at k.nieto@colostate.edu. https://orcid.org/0000-0002-8833-0113 Amy L. Prieto is a professor in the Department of Chemistry at Colorado State University, FRSC, and the founder and CTO of Prieto Battery, Inc. Dr. Prieto earned her BA in chemistry and philosophy at Williams College. She then earned a PhD in inorganic chemistry from the University of California, Berkeley, where she was a cooperative research fellow supported by Bell Labs, Lucent Technologies. Her postdoctoral work was performed at Harvard University, where she was named one of the first L’Oréal USA For Women in Science Fellows. In 2011, she was named an ExxonMobil Faculty Fellow in Solid State Chemistry (ACS). That same year, she received the Presidential Early Career Award for Scientists and Engineers from President Barack Obama. Prieto also won the Excellence in Storage Technology Commercialization Award from the Colorado Cleantech Industries Association. She is an associate editor for Chemical Communications, and is a Royal Society of The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Chemistry Fellow. Her batteries are currently on display at the Smithsonian Institute, Lemelson Center, in the “Places of Invention” exhibit. She can be reached at alprieto@colostate.edu. https://orcid.org/0000-0001-9235-185X

References 1. Larcher D., Tarascon J. M. Towards Greener and More Sustainable Batteries for Electrical Energy Storage. Nature Chemistry 2015, 7(1):19–29. https://doi.org/10.1038/nchem.2085. 2. Lermakova D. I., Dugas R., Palacín M. R., Ponrouch A. On the Comparative Stability of Li and Na Metal Anode Interfaces in Conventional Alkyl Carbonate Electrolytes. Journal of The Electrochemical Society 2015, 162(13):A7060–A7066. https://doi.org/10.1149/2.0091513jes. 3. Dugas R., Ponrouch A., Gachot G., David R., Palacin M. R., Tarascon J. M. Na Reactivity toward Carbonate-Based Electrolytes: The Effect of FEC as Additive. Journal of The Electrochemical Society 2016, 163(10):A2333–A2339. https://doi.org/10.1149/2.0981610jes. 4. Pfeifer K., Arnold S., Becherer J., Das C., Maibach J., Ehrenberg H., Dsoke S. Can Metallic Sodium Electrodes Affect the Electrochemistry of Sodium‐Ion Batteries? Reactivity Issues and Perspectives. ChemSusChem 2019, 12(14):cssc.201901056. https://doi.org/10.1002/cssc.201901056. 5. Kubota K., Komaba S. Review–Practical Issues and Future Perspective for Na-Ion Batteries. Journal of The Electrochemical Society 2015, 162(14):A2538–A2550. https://doi.org/10.1149/2.0151514jes. 6. Liang S., Cheng Y. J., Zhu J., Xia Y., Müller-Buschbaum P. A Chronicle Review of Nonsilicon (Sn, Sb, Ge)-Based Lithium/ Sodium-Ion Battery Alloying Anodes. Small Methods 2020, 4(8) https://doi.org/10.1002/smtd.202000218. 7. Li Z., Tan X., Li P., Kalisvaart P., Janish M. T., Mook W. M., Luber E. J., Jungjohann K. L., Carter C. B., Mitlin D. Coupling In Situ TEM and Ex Situ Analysis to Understand Heterogeneous Sodiation of Antimony. Nano Letters 2015, 15(10):6339–6348. https://doi.org/10.1021/acs.nanolett.5b03373. 8. Jackson E. D., Mosby J. M., Prieto A. L. Evaluation of the Electrochemical Properties of Crystalline Copper Antimonide Thin Film Anodes for Lithium Ion Batteries Produced by Single Step Electrodeposition. Electrochimica Acta 2016, 214:253– 264. https://doi.org/10.1016/j.electacta.2016.07.126. 9. Schulze M. C., Belson R. M., Kraynak L. A., Prieto A. L. Electrodeposition of Sb/CNT Composite Films as Anodes for Li- and Na-ion Batteries. Energy Storage Materials 2019, In Press. https://doi.org/10.1016/j.ensm.2019.09.025. 10. Gutiérrez-Kolar J. S., Baggetto L., Sang X., Shin D., Yurkiv V., Mashayek F., Veith G. M., Shahbazian-Yassar R., Unocic R. R. Interpreting Electrochemical and Chemical Sodiation Mechanisms and Kinetics in Tin Antimony Battery Anodes Using in Situ Transmission Electron Microscopy and Computational Methods. ACS Applied Energy Materials 2019, 2(5):3578–3586. https://doi.org/10.1021/acsaem.9b00310. 11. Zhang Y., Marschilok A. C., Takeuchi K. J., Kercher A. K., Takeuchi E. S., Dudney N. J. Understanding How Structure and Crystallinity Affect Performance in Solid-State Batteries Using a Glass Ceramic LiV3O8 Cathode. Chemistry of Materials 2019, 31(16):6135–6144. https://doi.org/10.1021/acs. chemmater.9b01571. 12. Hong K. S., Nam D. H., Lim S. J., Sohn D., Kim T. H., Kwon H. Electrochemically Synthesized Sb/Sb2O3 Composites as HighCapacity Anode Materials Utilizing a Reversible Conversion Reaction for Na-Ion Batteries. ACS Applied Materials and Interfaces 2015, 7(31):17264–17271. https://doi.org/10.1021/ acsami.5b04225. 13. Li D., Yan D., Ma J., Qin W., Zhang X., Lu T., Pan L. One-Step Microwave-Assisted Synthesis of Sb2O3/Reduced Graphene Oxide Composites as Advanced Anode Materials for SodiumIon Batteries. Ceramics International 2016, 42(14):15634– 15642. https://doi.org/10.1016/j.ceramint.2016.07.017.

14. Bryngelsson H., Eskhult J., Nyholm L., Herranen M., Alm O., Edström K. Electrodeposited Sb and Sb/Sb2O3 Nanoparticle Coatings as Anode Materials for Li-ion Batteries. Chemistry of Materials 2007, 19(5):1170–1180. https://doi.org/10.1021/ cm0624769. 15. Fan X. Y., Jiang Z., Huang L., Wang X., Han J., Sun R., Gou L., Li D. L., Ding Y. L. 3D Porous Self-Standing Sb Foam Anode with a Conformal Indium Layer for Enhanced Sodium Storage. ACS Applied Materials and Interfaces 2020, 12(18):20344– 20353. https://doi.org/10.1021/acsami.9b23501. 16. Li X., Sun M., Ni J., Li L. Template‐Free Construction of Self‐ Supported Sb Prisms with Stable Sodium Storage. Advanced Energy Materials 2019, 9(24):1901096. https://doi.org/10.1002/ aenm.201901096. 17. Li J., Pu J., Liu Z., Wang J., Wu W., Zhang H., Ma H. PorousNickel-Scaffolded Tin-Antimony Anodes with Enhanced Electrochemical Properties for Li/Na-Ion Batteries. ACS Applied Materials and Interfaces 2017, 9(30):25250–25256. https://doi. org/10.1021/acsami.7b04635. 18. Fan X. Y., Han J., Jiang Y., Ni J., Gou L., Li D. L., Li L. Hierarchical Porous Sb Films on 3D Cu Substrate Have Promise for Stable Sodium Storage. ACS Applied Energy Materials 2018, 1(8):3598–3602. https://doi.org/10.1021/acsaem.8b00872. 19. Long J. W., Dunn B., Rolison D. R., White H. S. 3D Architectures for Batteries and Electrodes. Advanced Energy Materials 2020, 10(46):2002457. https://doi.org/10.1002/aenm.202002457. 20. Arthur T. S., Bates D. J., Cirigliano N., Johnson D. C., Malati P., Mosby J. M., Perre E., Rawls M. T., Prieto A. L., Dunn B. Three-Dimensional Electrodes and Battery Architectures. MRS Bulletin 2011, 36(7):523–531. https://doi.org/10.1557/ mrs.2011.156. 21. An S. J., Li J., Daniel C., Mohanty D., Nagpure S., Wood D. L. The State of Understanding of the Lithium-Ion-Battery Graphite Solid Electrolyte Interphase (SEI) and its Relationship to Formation Cycling. Carbon 2016, 105:52–76. https://doi. org/10.1016/j.carbon.2016.04.008. 22. Peled E., Menkin S. Review—SEI: Past, Present and Future. Journal of The Electrochemical Society 2017, 164(7):A1703– A1719. https://doi.org/10.1149/2.1441707jes. 23. Jackson E. D., Prieto A. L. Copper Antimonide Nanowire Array Lithium Ion Anodes Stabilized by Electrolyte Additives. ACS Applied Materials & Interfaces 2016, 8(44):30379–30386. https://doi.org/10.1021/acsami.6b08033. 24. Schroder K., Alvarado J., Yersak T. A., Li J., Dudney N., Webb L. J., Meng Y. S., Stevenson K. J. The Effect of Fluoroethylene Carbonate as an Additive on the Solid Electrolyte Interphase on Silicon Lithium-Ion Electrodes. Chemistry of Materials 2015, 27(16):5531–5542. https://doi.org/10.1021/acs. chemmater.5b01627. 25. Bommier C., Ji X. Electrolytes, SEI Formation, and Binders: A Review of Nonelectrode Factors for Sodium-Ion Battery Anodes. Small 2018, 14(16) https://doi.org/10.1002/smll.201703576. 26. Eshetu G. G., Diemant T., Hekmatfar M., Grugeon S., Behm R. J., Laruelle S., Armand M., Passerini S. Impact of the Electrolyte Salt anion on the Solid Electrolyte Interphase Formation in Sodium Ion Batteries. Nano Energy 2019, 55:327–340. https:// doi.org/10.1016/j.nanoen.2018.10.040. 27. Verma P., Maire P., Novák P. A Review of the Features and Analyses of the Solid Electrolyte Interphase in Li-ion Batteries. Electrochimica Acta 2010, 55(22):6332–6341. https://doi. org/10.1016/J.ELECTACTA.2010.05.072. 28. Lee S. E., Tang M. H. Electroactive Decomposition Products Cause Erroneous Intercalation Signals in Sodium-Ion Batteries. Electrochemistry Communications 2019, 100:70–73. https://doi. org/10.1016/j.elecom.2019.01.024. 29. Lee S. E., Tang M. H. Reliable Reference Electrodes for Nonaqueous Sodium-Ion Batteries. Journal of The Electrochemical Society 2019, 166(14):A3260–A3264. https://doi.org/10.1149/2.0401914jes.

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A Vision for Sustainable Energy: The Center for Hybrid Approaches in Solar Energy to Liquid Fuels (CHASE) by Jillian L. Dempsey, Catherine M. Heyer, and Gerald J. Meyer

Introduction

he U. S. Department of Energy (DOE) recently granted $40 million to the Center for Hybrid Approaches in Solar Energy to Liquid Fuels (CHASE)1,2 to accelerate fundamental research on the production of liquid fuels from sunlight, water, nitrogen, and/or carbon dioxide. The overarching five-year goal of CHASE is to develop a fundamental molecular-level understanding of how hybrid photoelectrodes couple single photon absorptions to the multi-electron/multi-proton chemical transformations necessary to generate liquid solar fuels. (See Fig. 1.) The mission is to develop molecule/material hybrid photoelectrodes for the cooperative sunlight-driven generation of O2 and liquid fuels from CO2, H2O, and N2. Emphasis is placed on molecular catalysts integrated with semiconducting materials with precisely controlled microenvironments created around the catalysts. There is a vast, mostly unexplored research space at the intersection between molecular catalysts and heterogeneous materials, presenting unique opportunities for advances in photocatalytic durability and product selectivity. CHASE is guided by the overarching hypothesis that the challenge of liquid solar fuel production can only be met through the cooperative interactions of molecules and materials. This hypothesis derives from observations suggesting that neither heterogeneous materials alone nor homogeneous molecular catalysts alone have proven to be sufficient and that untapped opportunities for cooperativity exist at this interface.

Fig. 1. CHASE will develop hybrid photoelectrodes where molecular catalyst cascades are integrated with semiconductors.

Major breakthroughs in liquid solar fuels will be realized with an integrated multi-disciplinary collaborative team approach. CHASE is headquartered at the University of North Carolina at Chapel Hill (UNC), with partner institutions at Brookhaven National Laboratory, Emory University, North Carolina State University, the University of Pennsylvania, and Yale University. Across these six U.S. East Coast institutions, 31 principal investigators with complementary expertise in synthesis, characterization, catalysis, photoelectrochemistry, and theory contribute to CHASE research.

Department of Energy Roundtable on Liquid Solar Fuels CHASE research benefited from a comprehensive 2019 DOE Office of Basic Energy Sciences (BES) roundtable that was cochaired by one of the authors and the accompanying 2020 report.3 This “Roundtable on Liquid Solar Fuels” sought to assess gaps in knowledge, fundamental challenges, and research opportunities (continued on next page)

Four Priority Research Opportunities (PROs) • PRO-1. Understand the mechanisms that underpin constituent durability and performance. CHASE will prioritize a fundamental mechanistic understanding of both operation and degradation in hybrid photoelectrodes through molecular-level characterization of light-driven catalysis, state-of-the-art theory, and multi-scale simulations. The tunability of molecular catalysts, along with precise materials synthesis methods, will be utilized to optimize the durability and performance of hybrid photoelectrodes once points of weakness are identified. • PRO-2. Control the catalyst microenvironment to promote selective and efficient fuel production. CHASE will tailor the catalyst microenvironment on a molecular scale to control local proton activity, electric field, dipole, and lipophilicity to direct reactivity along desired pathways for the reduction of CO2 and N2 to liquid fuels and for the oxidation of water to O2. Comprehensive characterization through microscopy and spectroscopy will provide insight into the mechanisms by which microenvironments optimize catalyst activity, selectivity, and durability. • PRO-3. Bridge the time and length scales of light excitation and chemical transformations. CHASE will examine strategies to control the temporal coupling of multi-proton/multi-electron chemical transformations with light absorption and charge separation processes under solar flux. Decoupling light absorption from catalysis will enable the buildup of many charges before rapid multiproton/multi-electron reactions. • PRO-4. Tailor interactions of complex phenomena to achieve integrated multicomponent systems. CHASE will prepare atomically precise hybrid molecule/material photoelectrodes comprised of lightabsorbing semiconductor materials with multiple molecular catalysts for liquid solar fuel generation. Comprehensive studies employing spectroscopy, microscopy, and electrochemistry (including ex situ, in situ, and operando methods), complemented by theory and multiscale modeling, will provide mechanistic insight into the factors that control efficiency, selectivity, and durability in hybrid approaches to liquid solar fuel synthesis.

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

Dempsey et al.

(continued from previous page)

for the realization of energy-rich liquids from abundant feedstocks using sunlight as the only energy source. Four Priority Research Opportunities (PROs) were identified to address the critical requirements necessary for the realization of efficient, selective, and stable production of liquid fuels directly from sunlight. Challenges and opportunities central to an artificial photosynthetic approach– where catalysis is intimately integrated with light absorption–were considered; an approach that stands in contrast to non-integrated approaches, such as the photovoltaic generation of electricity that drives catalysis at dark electrodes (PV-Electrolysis). As described on page 65, CHASE research seeks to address the PROs through critical molecular-level knowledge of the design principles necessary to access next-generation catalysts integrated into hybrid photoelectrodes with high selectivity for liquid fuels and turnover frequencies commensurate with the terrestrial solar flux.

Scientific and Technical Background Through the realization of a comprehensive mechanistic picture of the elementary steps that comprise the entire hybrid photoelectrode system, CHASE plans to move the quest for liquid solar fuels forward. Guided by theory, photoelectrode architectures that pair light-absorbing materials with molecular fuel-producing catalysts will be constructed. Mechanistic investigations will provide unparalleled depth in the understanding of the light-driven chemistry at material-molecule-solution interfaces. This approach targets design principles and foundational insights, rather than a specific solar fuels device design, with the expectation that CHASE findings will be broadly applicable in the development of many different solar fuels technologies. Progress in the field of solar fuels over the last decade has matured to the point where a large research hub striving towards liquid solar fuel production is possible. For instance, research has demonstrated the high selectivity for a single reaction product that can be achieved with molecular catalysts. Moreover, the deep knowledge base of structure-property relationships will provide the critical molecularlevel design principles necessary to enable high turnover frequencies (TOFs) commensurate with the terrestrial solar flux.4-9 Such structureproperty relationships are exceedingly difficult to realize with heterogeneous catalysts, where a distribution of reaction products is typically produced, and reaction mechanisms are challenging to probe experimentally.10

Fig. 2. The six partner institutions that comprise CHASE. 66

The remarkable scientific advances in molecular catalysis performance enabled by structure-property relationships and mechanistic studies position molecular catalysts on the trajectory needed to address liquid solar fuel challenges. In CO2 reduction, molecular catalysts are marked by their ability to achieve high activity and exquisite selectivity to specific carbon-based products.5,7,9 In N2 reduction, highly tunable molecular catalysts mediate N2 fixation to NH3 by well-defined mechanisms,11,12 and in H2O oxidation, molecular catalysts can now generate O2 at rates faster than Nature’s oxygenevolving complex.8,13 Yet despite advances over the last decade, a single molecular catalyst is not yet sufficient to drive some of the most demanding multi-electron/proton transformations necessary to selectively form a liquid fuel with the needed activity and durability for integration into a hybrid photoelectrode. A key limitation of molecular CO2 reduction catalysis, for example, is that few catalysts are capable of producing valuable liquid fuels such as MeOH, and no catalysts have been discovered that can catalytically generate multicarbon products. Effective integration of light absorbers with catalyst cascades to create hybrid photoelectrodes capable of driving efficient and selective fuel formation will require strategies that consider and control the local region surrounding active catalytic sites–defined as the catalyst microenvironment–that provide conduits for reactants, products, electron, and proton flow. Semiconductors are ideal light harvesters for solar capture applications, as is evident in the marked growth of silicon photovoltaics. Photovoltaics based on group II-VI and group III-V materials are also finding niche applications in the market. In many instances, these commercial solar cells come with 10-year warranties and efficiencies greater than 10%. At the same time, there is a need for alternative semiconductor materials with improved light-harvesting and energy levels better aligned for catalytic reactions such as water oxidation.14,15 Nanostructured materials with precisely controlled surface stabilization are also necessary for some multi-electron/ proton catalytic reactions whose turnover frequencies are small relative to the solar flux. The integration of molecular catalysts with semiconductor materials that provide controlled surface structures and stabilization layers will be a focus of CHASE research. Despite the collective recognition that neither heterogeneous materials alone nor homogeneous molecular catalysts alone can address the scientific and technical challenges impeding liquid solar fuel technologies, the integration of remarkable molecular catalysts with visible light-absorbing semiconductors to create hybrid photoelectrodes is largely unexplored.16,17 The small number of reports detailing attempts to integrate CO2 reduction or water oxidation catalysts with visible light-absorbing semiconductors have largely focused on photocurrent measurements.18-22 Comprehensive characterization of the hybrid photoelectrodes and attempts to understand reaction mechanisms of light-driven fuel production are generally missing. CHASE brings together the necessary expertise to carry out detailed characterization of interfaces and conduct in-depth mechanistic studies, recognizing that this fundamental research will be critical to realizing hybrid photoelectrodes for liquid solar fuel production. Issues of durability19,23-40 are commonplace in reports describing the integration of molecular catalysts with wide band gap semiconductors, underscoring that a key challenge in utilizing molecular catalyst-based hybrid photoelectrodes for the generation of liquid fuels is long-term durability under solar irradiance.41,42 CHASE research will identify the origins of degradation processes that impinge on durability and use the insights garnered to tune the molecular-materials interface and realize hybrid photoelectrodes with unprecedented durability. The study of surface stabilization strategies that provide molecular control of the catalyst microenvironment will identify the factors that enhance and threaten durability. CHASE research is expected to impact energy science across the U.S. and the world. All research aligns with the overarching goal of discovering, understanding, and evaluating sunlight-driven chemistry for the sustainable synthesis of liquid fuels. The mechanistic understanding and design principles that emerge from CHASE research are expected to enable efficient solar water oxidation and selective generation of organic and nitrogen-based fuels. Such major The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

breakthroughs in liquid solar fuels synthesis will spark technology development efforts that promise sustainable energy resources for future generations.

Acknowledgements This material is based upon work solely supported as part of the Center for Hybrid Approaches in Solar Energy to Liquid Fuels (CHASE), an Energy Innovation Hub funded by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences under Award Number DE-SC0021173. We acknowledge James F. Cahoon and Alexander J. M. Miller for Fig. 1 and for a careful reading of this paper. © The Electrochemical Society. DOI: 10.1149.2/2.F10211IF.

About the Authors Jillian L. Dempsey received her SB from the Massachusetts Institute of Technology in 2005. In 2011, Dempsey received her PhD from the California Institute of Technology, where she conducted research with Harry Gray and Jay Winkler. After postdoctoral research at the University of Washington with Daniel Gamelin, she started her independent career at the University of North Carolina in 2012, where she is now an associate professor, the Bowman and Gordon Gray Distinguished Term Professor, and CHASE Deputy Director. Her research program applies electrochemistry and timeresolved spectroscopy to interrogate the electron and proton-coupled electron transfer processes that underpin solar fuel production. She may be reached at dempseyj@email.unc.edu. https://orcid.org/0000-0002-9459-4166 Catherine M. Heyer received her BS (1980) and PhD (1984) from Trinity College Dublin, the University of Dublin, Ireland, where she worked with John M. Kelly on photocatalytic solar energy conversion. She performed postdoctoral research with Jean-Marie Lehn (Université de Strasbourg) and Richard S. Eisenberg (University of Rochester), and subsequently worked in industry as a research scientist, and at Duke University. Formerly the assistant director of the UNC Energy Frontier Research Center (2009-2020), she is now CHASE Managing Director. Heyer may be reached at cmheyer@unc.edu. https://orcid.org/0000-0001-7619-9106 Gerald J. Meyer received his BS from the University of New York at Albany-State (1985), and a PhD at the University of WisconsinMadison (1989), working with Arthur B. Ellis. After completing postdoctoral research at the University of North Carolina at Chapel Hill (UNC) with Thomas J. Meyer, he joined the faculty at Johns Hopkins University in 1991. He returned to UNC-Chapel Hill in 2014. His research program has focused on fundamental mechanistic investigations of molecular-semiconductor interfaces of relevance to solar energy conversion. Meyer is currently a professor of chemistry, Vice-Chair for Diversity, and CHASE Director. He may be reached at gjmeyer@email.unc.edu. https://orcid.org/0000-0002-4227-6393

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SEC TION NE WS

New ECS Section Pacific Northwest Section The ECS Board of Directors chartered the new ECS Pacific Northwest Section on October 16, 2020, providing area scientists and engineers with opportunities to network with researchers and participate in various events. Jie Xiao, ECS Fellow and Battery Division Secretary, took the lead in chartering the section and now serves as its chair. The ECS Pacific Northwest Section seeks to connect interested parties from academia, industry, and government, bridge a scientific gap, provide networking opportunities that could lead to new developments, and help members advance their careers. The section serves the universities and national labs in Washington State, Idaho, and Oregon. Xiao believes the section will bolster the growth of the electrochemistry and solid state science fields in the Pacific Northwest. Membership in the Pacific Northwest section is free for ECS members in good standing. The ECS Pacific Northwest Section has 24 members. The officers are Chair Jie Xiao (Pacific Northwest National Labs), Vice-Chair Corie Cobb (University of Washington [UW]), Secretary Yun Li (Microsoft Corporation), and Treasurer Shannon Boettcher (University of Oregon [UO]). The section has ambitious plans. Xiao proposes two events per year, quarterly seminars, and an industry day where attendees can look for electrochemistry jobs. The section executive committee hopes to promote extensive interaction and collaboration between researchers, and increase student and researcher interest in, and involvement with, the electrochemical community.

The committee launched a series of virtual events to share research progress, exchange information, and, more importantly, enhance collaborations among industry, universities, and national labs in the three states. In January, David Reed and Wei Wang (Pacific Northwest National Laboratory) presented “Energy Storage for Grid Applications,” followed in February by Kelsey Stoerzinger and David Ji (Oregon State University) on “Operando Surface Science in Electrochemical Systems/Materials for Aqueous Rechargeable Batteries.” “Physics-based electroanalytical approaches for understanding whole battery cells” is the topic of April’s speaker, Daniel T. Schwartz (UW). Industrial Day takes place in early May with representatives from Microsoft, Gamry, Boeing, IBM, Thermo Fisher Scientific, and others. Corie Cobb (UW) and Shannon Boettcher (UO) are the organizers. Dong Ding (Idaho National Laboratory) presents “Electrochemistry at Intermediate Temperatures: A Playground for Electrochemical Processing Using Solid Oxide Electrochemical Cells” at 1000h PST on June 10. July’s speaker is Shannon Boettcher (UO), presenting “Accelerating Water Dissociation in Bipolar Membranes and Electrocatalysts.” UW’s Bo Zhang presents “Single-Molecule Imaging of the Electrochemical Interface” in September. Michael Ware from Boeing will discuss aerospace batteries in October. Detailed information will be provided closer to the upcoming events. We greatly appreciate those who volunteer to support and contribute to the Pacific Northwest section. If you are interested in becoming a member, please contact the ECS Community Engagement Department at customerservice@electrochem.org.

The ECS Pacific Northwest Section committee members are (from left to right): Chair Jie Xiao, Pacific Northwest National Laboratory; Vice-Chair Corie Cobb, University of Washington; Secretary April Li, Microsoft; Treasurer Shannon Boettcher, University of Oregon; Member at Large Jerome Babauta, Gamry Instruments; Section Representative Yuyan Shao, Pacific Northwest National Laboratory.

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Global reach, access to innovative research, networking, and recognition For more information, contact customerservice@electrochem.org. The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

SEC TION NE WS Europe Section The ECS Europe Section announces that in January 2021, a new slate of officers was elected to serve on the Executive Committee for two years (2021-2022). The Executive Committee meets twice a year, during the spring and fall ECS meetings. Due to the COVID-19 pandemic and unprecedented situation, only online meetings took place in 2020. The section supports student travel grants, as well as the Europe Section Alessandro Volta Medal and Europe Section Heinz Gerischer Award. The deadline to submit nominations is February 15 in odd years for the Volta Medal, and September 30 in even years for the Gerischer Award. Information on Europe section awards is available at www.electrochem.org/awards. Please reach out to the Europe Section executive committee members at customerservice@electrochem.org. We welcome ideas and suggestions on growing the section.

ECS Europe Section New Officers CHAIR Philippe Marcus is Director of Research at the Centre National de la Recherche Scientifique (CNRS) and Head of the Physical Chemistry of Surfaces Research Group at the Institut de Recherche de Chimie Paris (Chimie ParisTechPSL), France. Dr. Marcus received his PhD in Physical Sciences from the Université Pierreet-Marie-Curie, France, in 1979. His research focuses on surface electrochemistry and corrosion science, with emphasis on understanding the relationship between the structure and properties of metal surfaces and oxide films at the atomic or nanometric scale. He is a Fellow of the Electrochemical Society (2005) and the International Society of Electrochemistry (2009). His numerous accolades include the ECS Olin Palladium Award (2017); EFC European Corrosion Medal (2015); Lee Hsun Award, Institute of Metals Research of the Chinese Academy of Sciences (2012); U.R. Evans Award, UK Institute of Corrosion (2010); NACE International Whitney Award (2008); and the ECS Corrosion Division H. H. Uhlig Award (2005). Marcus is Chairman of the EFC Working Party on Surface Science and Mechanisms of Corrosion and Protection, Chairman of the International Steering Committee for the European Conferences on Applications of Surface and Interface Analysis, and President of the French Corrosion Society. He has published over 500 papers in scientific journals, books, and conference proceedings, and presented more than 130 invited lectures at international conferences. Marcus has 19,670 citations with an h-index of 76 as of January 2021. VICE-CHAIR Roberto Paolesse is Full Professor of Chemistry in the Department of Chemical Science and Technologies at the Università degli Studi di Roma “Tor Vergata,” Italy. He started his career there in 1986 as an assistant professor. Paolesse graduated cum laude in Chemistry from the Sapienza Università di Roma, Italy, in 1983. His research interests include the applications of porphyrins and related macrocycles to develop chemical sensors and artificial sensor systems, and the development of supramolecular assemblies and their exploitation in electrochemical devices. Responsible for several national and European research projects, he is now coordinator of the FET-OPEN project INITIO in the European Union’s Horizon 2020 program. Paolesse has authored more than 400 articles in international journals, holds six patents, and edited two books. 70

SECRETARY Robert Lynch is a Senior Lecturer in Energy and Course Director of the BSc in Applied Physics at the Department of Physics, University of Limerick, Ireland. He teaches undergraduate courses and supervises PhD and Master’s students in physics and electrochemistry. Lynch is Principal Investigator of the Energy Storage and Semiconductor Technology Group at the Bernal Institute and Department of Physics at the University of Limerick. His group investigates the measurement and monitoring of flow battery systems, stabilization of electricity grids, and semiconductor nanostructure formation. He is the project manager of fundamental and industrial research projects and the scientific advisor to Lumcloon Energy, which is currently completing construction of the largest grid stabilization project using electrochemical energy storage in Europe. TREASURER Jan Macák has been a senior researcher and group leader at the Center of Materials and Nanotechnologies of the University of Pardubice, Czech Republic, since 2015. The group leader at the Central European Institute of Technology of the Brno University of Technology, Czech Republic, he has served as Treasurer of the ECS Europe Section since 2018. Macák completed his PhD in 2008 at the Friedrich-AlexanderUniversität Erlangen-Nürnberg, Germany. His research focuses on the synthesis of 1D nanotubular and nanoporous materials by anodization of valve metals and the subsequent modification of these materials by various means. In particular, his group has tailored the atomic layer deposition technique for the deposition of oxide- and chalcogenide-based materials within high-aspect-ratio nanotubular structures towards various applications. Macák is the author of 184 publications with 15,051 citations. MEMBERS AT LARGE • Krzysztof Bienkowski, University of Warsaw, Poland • D. Noel Buckley, University of Limerick, Ireland • Stefan De Gendt, Katholieke Universiteit Leuven, Belgium • Geir Haarberg, Norwegian University of Science and Technology, Norway • Adriana Ispas, Technische Universität Ilmenau, Germany • Deborah Jones, Centre National de la Recherche Scientifique, France • Pawel Kulesza, University of Warsaw, Poland • Krzysztof Miecznikowski, University of Warsaw, Poland • Iwona Agnieszka Rutkowska, University of Warsaw, Poland • Zbigniew J. Stojek, University of Warsaw, Poland • Petr Vanýsek, Brno University of Technology, Czech Republic • Benjamin Wilson, Aalto University, Finland

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SEC TION NE WS Japan Section The ECS Japan Section sponsored the 33rd ECSJ Tohoku Branch Young Scientists Meeting on December 5, 2020, via Zoom. Akichika Kumatani (Tohoku University, Japan) was the event’s chief organizer with Hitoshi Shiku (Tohoku University, Japan), Chair of the section’s Tohoku Branch, serving as meeting supervisor. The meeting consisted of five oral and 24 poster presentations, with 76 participants. A new tool developed by Hiroyuki Kai

(Tohoku University) was used in the poster session. Participants visited a virtual poster discussion board using an avatar of their choice (similar to those used in Japanese computer games). Five authors received best poster prizes. Participants discussed topics such as bioelectrochemistry, batteries, and organic electrochemistry. At the same time, members of the Japan Section’s Tohoku Branch, including senior researchers, provided inspiration and guidance to young researchers in the SEMI Conference.

Virtual poster board used as a new poster discussion tool at the 33rd ECS Japan Section Tohoku Branch Young Scientists Meeting. Photo: The image is reproduced with permission from the web (www.virtual-poster.net). Copyright: Hiroyuki Kai.

33rd ECS Japan Section Tohoku Branch Young Scientists Meeting poster prize winners are: Taisei Amanokura (top right photo, on the left), Tohoku University; (bottom photos, from left to right): Yuya Maekawa, Hirosaki University; Takuya Furuhashi, Tohoku University; Toshinari Kamimura, Iwate University; and Satoshi Chubachi, Yamagata University.

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SEC TION NE WS San Francisco Section The ECS San Francisco Section conducted its year-end business meeting and the ECS San Francisco Section Daniel Cubicciotti Student Award ceremony online on December 22, 2020. Members reviewed the section’s 2020 activities and finances, and paid tribute to departing officers Recording Secretary Xin He and Secretary Aleksandr Kiessling. The newly elected Recording Secretary, Rohit Satish (Lawrence Berkeley National Laboratory), who replaces Xin He, laid out a brief plan for 2021. The officers met in early 2021 to hammer out detailed activities for the year. Oana Leonte presented the draft plan for the next ECS San Francisco

Award, which calls for a nomination deadline of March 15 in odd years, with the award to be presented at the ECS spring meeting in even years. David G. Mackanic (Stanford University, U.S.) received the 2020 ECS San Francisco Section Daniel Cubicciotti Student Award. Bin Yao (University of California, Santa Cruz, U.S.) received the 2020 Honorable Mention. The section recognized them both at the award ceremony, where Mackanic described his award-winning activities to members. His academic advisor, Zhenan Bao, participated in the ceremony, as did Yao’s advisor, Yat Li.

Present at the ECS San Francisco Section online presentation of the Daniel Cubbiciotti Student Award are (from top, left to right): Treasurer Oana Leonte; Chair Gao Liu; Recording Secretary Rohit Satish; 1st Vice Chair Bryan McCloskey; Zhenan Bao, Stanford University; Yat Li, University of California, Santa Cruz; 2nd Vice Chair Xiaoyan Luo; Honorable Mention awardee Bin Hu; and award winner David G. Mackanic.

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SEC TION NE WS Singapore Section The ECS Singapore Section successfully launched the Electrochemistry and Materials Webinar Series on December 11, 2020. The webinars are delivered via videoconferencing with the goal of facilitating discussions on integrating materials into promising electrochemical technologies. Each webinar begins with a presentation by an internationally renowned electrochemist followed by a real-time Q&A session. Four webinars took place in January 2021, with more scheduled for later in the year. Peter Strasser (Technische Universität Berlin, Germany) delivered the first talk, “Electrolytic Hydrogen Production from Purified and Saline Water: From Electrocatalytic Fundamentals to Electrolyzer Cell Designs.” He highlighted the importance of the generation of green hydrogen, the scarcity of purified freshwater, and the various advances that could enable the electrolysis of saline water. In particular, he shared his work on various asymmetric electrolyzer cell designs that could enable effective seawater electrolysis. On December 15, 2020, Shannon Boettcher (University of Oregon, U.S.) presented “Towards a Molecular Understanding of Dynamic Fe-based Oxygen Evolution Catalysts.” The lecture highlighted the synergy between iron (Fe) and other transition metal sites such as cobalt (Co) and nickel (Ni) on mixed-metal oxyhydroxide catalysts in oxygen evolution reaction under alkaline conditions. Boettcher also described the evolution of these catalysts under active catalytic conditions. Y. Shirley Meng (University of California, San Diego, U.S.) delivered “From Atom to System–How to Enable the Tera-scale Energy Transition” on January 7, 2021. She discussed recent advances in characterization techniques and computational methods to study

intercalation compounds and their related phenomena, such as phase changes, electronic structure changes, and defect generation. She also shared her work to improve the performance of lithium-ion batteries and solid state batteries and discussed the possibility of developing a recyclable battery. The webinar series is ongoing. With more than 80 participants in each webinar thus far, the series is expected to significantly impact intellectual exchange among electrochemistry enthusiasts. “The School of Materials Science and Engineering, Nanyang Technological University, Singapore, has provided great support to make this webinar series happen,” said Zhichuan J. Xu, Chair of the ECS Singapore Section. “This is in line with Singapore’s effort in the R&D of carbon reduction techniques. The section will elaborate on advancing the intellectual exchange and connecting the local research community with those outside the island.”

Speakers at the Electrochemistry and Materials Webinar Series, organized by the ECS Singapore Section and the School of Materials Science and Engineering, Nanyang Technological University, Singapore, included (from left to right): Peter Strasser, Shannon Boettcher, and Y. Shirley Meng.

Section Leadership Section Name

Arizona Section Brazil Section Canada Section Chicago Section Chile Section China Section Cleveland Section Detroit Section Europe Section Georgia Section India Section Israel Section Japan Section Korea Section Mexico Section National Capital Section New England Section Pacific Northwest Section Pittsburg Section San Francisco Section Singapore Section Taiwan Section Texas Section Twin Cities Section

Section Chair

Candace Kay Chan Luis F. P. Dick E. Bradley Easton Open Jose H. Zagal Yongyao Xia Heidi B. Martin Kristopher Inman Philippe Marcus Seung Woo Lee Sinthai A Ilangovan Daniel Mandler Masayoshi Watanabe Won-Sub Yoon Carlos E. Frontana-Vazquez Eric D. Wachsman Sanjeev Mukerjee Jie Xiao Open Gao Liu Zhichuan J Xu Hsisheng Teng Jeremy P. Meyers Victoria Johnston Gelling

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AWARDS PROGRAM

Awards, Fellowships, Grants ECS distinguishes outstanding technical achievements in electrochemistry, and solid state science and technology, and recognizes exceptional service to the Society through the Honors & Awards Program. Recognition opportunities exist in the following categories: Society Awards, Division Awards, Student Awards, and Section Awards. ECS recognizes that today’s emerging scientists are the next generation of leaders in our field, and offers competitive Fellowships and Grants to allow students and young professionals to make discoveries and shape our science long into the future.

See highlights below and visit www.electrochem.org/awards for more information.

Society Awards The ECS Charles W. Tobias Young Investigator Award was established in 2003 to recognize outstanding scientific and/or engineering work in fundamental or applied electrochemistry or solid state science and technology by a young scientist or engineer. The award consists of a scroll, a $5,000 prize (USD), Society life membership, complimentary meeting registration, and travel assistance to the designated meeting. Materials due by October 1, 2021. The ECS Edward Goodrich Acheson Award was established in 1928 for distinguished contributions to the advancement of any of the objects, purposes, or activities of The Electrochemical Society. The award consists of a gold medal and a plaque that contains a bronze replica thereof, a $10,000 prize (USD), Society life membership, and complimentary meeting registration. Materials due by October 1, 2021.

Division Awards The ECS Electronics and Photonics Division Award was established in 1969 to encourage excellence in electronics research and outstanding technical contribution to the field of electronics science. The award consists of a scroll, a $1,500 prize (USD), and the option of up to $1,000 (USD) to facilitate travel to the designated meeting for recognition, or ECS life membership. Materials due by August 1, 2021. The ECS Energy Technology Division Research Award was established in 1992 to encourage excellence in energy-related research. The award consists of a scroll, a $2,000 prize (USD), and membership in the Energy Technology Division for as long as the recipient is an ECS member. Materials due by September 1, 2021.

The ECS Energy Technology Division Supramaniam Srinivasan Young Investigator Award was established in 2011 to recognize and reward an outstanding young researcher in the energy technology field. The award consists of a scroll, a $1,000 prize (USD), and complimentary meeting registration. Materials due by September 1, 2021. The ECS Nanocarbons Division Richard E. Smalley Research Award was established in 2006 to encourage excellence in fullerenes, nanotubes, and carbon nanostructures research. The award is intended to recognize, in a broad sense, those persons who have made outstanding contributions to the understanding and applications of fullerenes. The award consists of a scroll, $1,000 prize (USD), and up to $1,500 (USD) in travel assistance. Materials due by September 1, 2021. The ECS Nanocarbons SES Research Young Investigator Award was established in 2007 to recognize and reward one outstanding young researcher in the field of fullerenes, carbon nanotubes, and carbon nanostructures. The award consists of a scroll, a $500 prize (USD), and complimentary meeting registration. Materials due by September 1, 2021. The ECS Physical and Analytical Electrochemistry Division David C. Grahame Award was created in 1981 to encourage excellence in physical electrochemistry research and to stimulate publication of high-quality research papers in the Journal of The Electrochemical Society. The award consists of a scroll and a $1,500 (USD) prize. Materials due by October 1, 2021. The ECS Corrosion Division H. H. Uhlig Award was established in 1972 to recognize excellence in corrosion research and outstanding technical contributions to the field of corrosion science and technology. The award consists of a scroll, a $1,500 prize (USD), and possible travel assistance. Materials due by December 15, 2021.

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AWARDS AWAPROGRAM RDS The ECS High-Temperature Energy, Materials, & Processes Division Outstanding Achievement Award was established in 1984 to recognize excellence in research and outstanding technical contributions to the high-temperature energy, materials, and processes field. The award consists of a $1,000 prize (USD), complimentary registration, and up to $1,000 (USD) in travel expenses. Materials due by January 1, 2022. The ECS Luminescence and Display Materials Division Outstanding Achievement Award was established in 2002 to encourage excellence in luminescence and display materials research and outstanding technical contributions to the field. For the purposes of this award, luminescence and display materials science is defined as that area of knowledge that encompasses the physics, chemistry, and materials technology of luminescence and display materials and devices. The award consists of a scroll, a $1,000 prize (USD), and up to $1,000 (USD) in travel expenses to facilitate meeting attendance. Materials due by January 1, 2022. The ECS Sensor Division Outstanding Achievement Award was created in 1989 to recognize outstanding achievement in research and/or technical contributions to the field of sensors and to encourage work excellence in the field. The award consists of a scroll and a $1,000 (USD) prize. Materials due by March 1, 2022.

Student Awards The ECS Georgia Section Outstanding Student Achievement Award was established in 2011 to recognize academic accomplishments in any area of science or engineering in which electrochemical and/or solid state science and technology is the central consideration. The award consists of a $500 (USD) prize. Materials due by August 15, 2021. The ECS Energy Technology Division Graduate Student Award Sponsored by BioLogic was established in 2012 to recognize promising young engineers and scientists in fields pertaining to this division. The award consists of a scroll, a $1,000 (USD) prize, complimentary student meeting registration, and complimentary admission to the division business meeting. Materials due by September 1, 2021. The ECS Industrial Electrochemistry and Electrochemical Engineering Division H. H. Dow Memorial Student Achievement Award was established in 1990 to recognize promising young engineers and scientists in the field of electrochemical engineering and applied electrochemistry. The award consists of a scroll and a $1,000 (USD) prize to be used for expenses associated with the recipient’s education or research project. Materials due by September 1, 2021. The ECS Industrial Electrochemistry and Electrochemical Engineering Division Student Achievement Award was established in 1989 to recognize promising young engineers and scientists in the field of electrochemical engineering. The award consists of a scroll and a $1,000 (USD) prize. Materials due by September 1, 2021.

Edward Goodrich Acheson Award Deadline: October 1, 2021

www.electrochem.org/acheson-award The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

AWARDS PROGRAM

Award Winners Join us in celebrating your peers as we extend congratulations to all! The following awards are part of the ECS Honors & Awards Program which has recognized professional and volunteer achievement within our multidisciplinary sciences for decades.

Society Awards Allen J. Bard Award in Electrochemical Science Marc Koper is a professor of surface chemistry and catalysis at Leiden University, The Netherlands. He received his PhD degree (1994) from Utrecht University (The Netherlands) with a thesis on nonlinear dynamics and oscillations in electrochemistry. He was an EU Marie Curie postdoctoral fellow at the University of Ulm (Germany) and a fellow of Royal Netherlands Academy of Arts and Sciences (KNAW) at Eindhoven University of Technology, before moving to Leiden University in 2005. His research in Leiden focuses on fundamental aspects of electrocatalysis, theoretical and computational electrochemistry, and electrochemical surface science, in relation to renewable energy and chemistry. He has received various national and international awards, among which the Netherlands Catalysis and Chemistry Award (2019) and the Faraday Medal (2017).

Gordon E. Moore Medal for Outstanding Achievement in Solid State Science & Technology Hiroshi Iwai received BE and PhD degrees in electrical engineering from the University of Tokyo, Japan. He joined Toshiba in 1973, and contributed to the development of integrated circuit devices for 26 years. He joined Tokyo Institute of Technology in 1999, and engaged in the research of semiconductor device technologies for 21 years. He is now Professor Emeritus, Tokyo Institute of Technology, and Vice Dean and Distinguished Chair Professor, National Chiao Tung University, Taiwan. He has authored/co-authored more than 1,000 international journal and conference papers, and 500 Japanese ones. He is an inventor of 80 U.S. and 65 Japanese patents. His most famous accomplishment is the continuation of miniaturization of MOSFETs from 8 μm to recent sub-50 nm generations, contributing to the continuation of Moore’s law for 50 years. He has engaged in the development of product technologies from the early period of large scale integrated circuits; the first NMOS LSI technology at Toshiba in 1975, several generations of memories—1k SRAM, 64 k DRAM, and 1M SRAM—bipolar and BiCMOS technologies for analog and RF. He initiated an RF CMOS project in 1995, resulting in the success of Bluetooth. He has also introduced many new process technologies, which were the first or one of the first attempts in the world; BPSG planarization, source/drain ion-implantation, reactive ion etching for poly Si gate, rapid thermal annealing for shallow doping, rapid thermal oxidation for ultra-thin gate oxides, rapid thermal nitridation for oxynitride gate oxides, and NiSi silicide.

Dr. Iwai is currently Vice Dean and Distinguished Chair Professor of the ICST at the International College of Semiconductor Technology, NCTU, in Taiwan. He also holds the title of Professor Emeritus of the Tokyo Institute of Technology. Dr. Iwai is an awarded life member and a fellow of The Electrochemical Society.

Division Awards Energy Technology Division Research Award Bryan Pivovar is a senior research fellow and Electrochemical Engineering and Materials Chemistry Group Manager in the Chemistry and Nanosciences Center at the National Renewable Energy Laboratory in Golden, CO, where he oversees NREL’s electrolysis and fuel cell and materials R&D. He has been a pioneer in several areas of fuel cell development, taking on leadership roles and organizing workshops in the areas of subfreezing effects, alkaline membrane fuel cells (2006, 2011, 2016, and 2019), and renewable hydrogen at the gigaton scale (2019). He co-chaired the Gordon Research Conference-Fuel Cells (2007), and will serve as the chair for The 3rd International Conference on Electrolysis in 2022. He was responsible for leading a multinational laboratory team pursuing “Hydrogen at Scale,” investigating the energy system-wide benefits of increased hydrogen utilization. He has recently been named director for a major U.S. Department of Energy Consortium (minimum of $50M over five years), H2NEW (Hydrogen (H2) from Next-Generation Electrolyzers of Water), focused on addressing components, materials integration, and manufacturing R&D to enable manufacturable electrolyzers that meet required cost, durability, and performance targets, simultaneously, in order to enable $2/kg hydrogen. Pivovar received his PhD in chemical engineering from the University of Minnesota and led fuel cell R&D at Los Alamos National Laboratory prior to joining NREL. He was the 2012 winner of the Charles W. Tobias Young Investigator Award from The Electrochemical Society. He has co-authored over 150 papers, with over 10,000 citations in the general area of fuel cells and electrolysis.

Energy Technology Division Supramaniam Srinivasan Young Investigator Award Iryna Zenyuk is an associate professor, Department of Chemical and Biomolecular Engineering, at the University of California, Irvine. Prof. Zenyuk holds a BS (2008) in mechanical engineering from the New York University Tandon School of Engineering. She continued her studies at Carnegie Mellon University, where she earned an MS (2011) and PhD (2013) in mechanical engineering. Her graduate work focused on the fundamental understanding of electric double layers in electrochemical energy-conversion systems. The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

AWARDS AWAPROGRAM RDS After a postdoctoral fellowship at the Lawrence Berkeley National Laboratory in the Electrochemical Technologies Group, Zenyuk joined the faculty of the Department of Mechanical Engineering at Tufts University in 2015. In July 2018, she joined the Department of Chemical and Biomolecular Engineering at the University of California, Irvine, where she is also an associate director of the National Fuel Cell Research Center. At UC Irvine, Zenyuk’s group works on enabling energy solutions by researching low-temperature hydrogen fuel cells, Li-metal batteries, and electrolyzers. Zenyuk works on design strategy encompassing novel materials, diagnostic tools, and device-level testing. She is the recipient of various awards, including the NSF CAREER award (2017); Interpore Society Fraunhofer Award for Young Researchers (2017); Research Corporation for Science Advancement, Scialog Fellow in Advanced Energy Storage (20172019); ECS Toyota Young Investigator Award (2018); UCI Samueli School of Engineering Early Career Faculty Excellence in Research Award (2019); and ECS Energy Technology Division Srinivasan Young Investigator Award (2021). Prof. Zenyuk has published over 60 journal publications and delivered more than 60 invited presentations on topics related to energy conversion and storage.

Industrial Electrochemistry and Electrochemical Engineering Division New Electrochemical Technology (NET) Award Company: Faraday Technology, Inc. E. Jennings (E.J.) Taylor is the founder and CTO of Faraday Technology, Inc., a small business focused on developing innovative electrochemical processes and technologies based on pulse and pulse reverse electrolytic principles. E.J. leads Faraday’s business, technology, and commercialization strategy. In addition to 200+ technical publications and presentations, E.J. is an inventor on over 50 patents. He was part of the team that won a 2013 Presidential Green Chemistry Challenge Award for trivalent chromium plating, and was a finalist for the 2016 R&D 100 award for niobium electropolishing. E.J. has been a member of The Electrochemical Society for 42 years. He is an ECS Fellow, past treasurer, and currently serves as Chair, Interdisciplinary Science and Technology Subcommittee. Maria Inman is the research director of Faraday Technology, Inc., where she manages the company’s pulse and pulse reverse research project portfolio. In addition to numerous technical publications and presentations, Maria is an inventor of many patents. Maria was part of the team that won a 2013 Presidential Green Chemistry Challenge Award for trivalent chromium plating, and was a finalist for the 2016 R&D 100 award for niobium electropolishing. She is a member of ASTM and has been a member of ECS for over 25 years. In addition to organizing symposia at ECS meetings, Maria currently serves as Vice-Chair, Industrial Electrochemistry and Electrochemical Engineering Division.

Tim Hall is the laboratory manager at Faraday Technology, Inc., where he oversees the company’s experimental activities directed towards developing innovative pulse and pulse reverse electrolytic processes. In addition to numerous presentations and publications, Tim is an inventor on many patents. Tim is part of a team that received a 2011 R&D 100 award for developing a novel pulse reverse deposition process for an alloy coating, won a 2013 Presidential Green Chemistry Challenge Award for trivalent chromium plating, and was a finalist for the 2016 R&D 100 award for niobium electropolishing. Tim has been an ECS member for over 15 years, and is active in the Electrodeposition Division. Stephen T. Snyder is the lead design engineer at Faraday Technology, Inc. He received his BCE in chemical engineering from the University of Dayton in 2001. In 2005, he received his MS in materials engineering from Purdue University. In 2012, he obtained his drafting and design certification from Sinclair Community College. Stephen leads the design function and manages the engineering and fabrication of prototype apparatuses for Faraday. He was part of a Faraday team selected for a 2013 Presidential Green Chemistry Challenge Award for trivalent chromium plating, and was a finalist for a 2016 R&D 100 award for niobium surface finishing. Stephen has been a co-inventor to two patents and has contributed to work for numerous pending patent applications. He has been an ECS member since 2007.

Industrial Electrochemistry and Electrochemical Engineering Division New Electrochemical Technology (NET) Award Company: Urban Electric Power Inc. Urban Electric Power Inc. (UEP) develops, manufactures, and markets zinc-manganese (ZnMnO2) batteries for grid-related energy storage applications. These batteries utilize safe, inexpensive, earth-abundant raw materials that have a significantly lower carbon footprint than commercially available energy storage batteries. UEP’s patented ZnMnO2 battery revolutionizes the chemistry used in alkaline primary (single-discharge) batteries (e.g., C, D, AA, and AAA) by making it rechargeable over thousands of charge-discharge cycles. The core innovation stems from research performed at The CUNY Energy Institute that demonstrated the rechargeability of manganese dioxide in an alkaline cell without significant reduction in potential energy. Subsequent breakthroughs made by the UEP team have demonstrated high-voltage characteristics in dual electrolyte cells, which can bring manufactured cell costs down to $22/kWh and increase the energy density to be comparable with lithium-ion cells, while maintaining key safety attributes. UEP is headquartered in Pearl River, NY, where it operates a pilot manufacturing line and performs battery R&D and testing.

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AWARDS PROGRAM (continued from previous page)

Sanjoy Banerjee is CEO and Executive Chairman of Urban Electric Power Inc. (UEP) and the Director of The CUNY Energy Institute, where he also serves as Distinguished Professor of Chemical Engineering. Banerjee founded the Energy Institute on coming to CUNY in 2008, to develop sustainable energy technologies with low carbon footprints. Research in these areas, specifically modular and passively safe nuclear reactors, grid-scale electrochemical energy storage, and enhanced efficiency flow assurance for the oilgas industry, has developed at the Energy Institute under his leadership to become internationally recognized. Prior to UEP and CUNY, Banerjee had been Chair of the Chemical Engineering Department, University of California (UC), Santa Barbara, had taught at UC Berkeley and McMaster University in Canada, and worked at Atomic Energy of Canada, ultimately as Acting Director of the Applied Science Division. For periods during his tenure at UC Santa Barbara, he was Mitsubishi Professor at the University of Tokyo, Japan, the Burgers Professor at TU Delft, The Netherlands, and at ETH Zurich, Switzerland, where he continues to lecture every year. He has served on several high-level advisory boards: notably, NASA Fluid Physics, the oil industry Flow Assurance Consortium, and the Advisory Committee on Reactor Safeguards (ACRS), congressionally mandated to advise on nuclear facility licenses, where his last assignment was in the ACRS sign off for the nuclear engines in the Ford-class aircraft carrier. Prof. Banerjee’s work was most recently recognized by the 2019 ACS/EPA Green Chemistry Challenge Award (academic) for the development of rechargeable zinc-manganese dioxide batteries for grid applications, in collaboration with Urban Electric Power Inc., D.O.E. Office of Electricity, and Sandia National Laboratories. Jinchao Huang is the director of development at Urban Electric Power Inc. (UEP). She is responsible for research and development of high capacity, rechargeable, and inexpensive zinc manganese dioxide batteries for home and commercial use. Prior to joining UEP, she completed her doctoral research in chemical engineering at The City College of New York with Prof. Sanjoy Banerjee, where she focused on the immobilization of zincate ions in secondary alkaline zinc batteries, and developed several innovative ionic selective separators for long-cycle high-energy-density zinc manganese dioxide batteries. She has co-authored 12 peer reviewed papers and more than 10 patents. Gautam G. Yadav is a world-leading materials scientist and electrochemist, working as Director of Advanced Battery Development at Urban Electric Power Inc. (UEP). He earned his doctoral degree in chemical engineering from Purdue University, where he specialized in synthesizing 1D complex metal oxide nanowires for thermoelectric applications and lithium-ion batteries. Prior to joining UEP, Dr. Yadav worked as a senior scientist at the CUNY Energy Institute, where he led the advancement of highly energy dense aqueous-based batteries based on manganese dioxide (MnO2) and zinc (Zn) as a replacement for the expensive and dangerous lithium-ion batteries for grid-storage applications. He is the primary lead inventor of the reversible second-electron MnO2 78

technology and the breakthrough high voltage (2.45-2.8V) ZnMnO2 battery. He has authored 19 publications and filed over 26 patents on ZnMnO2 technology, licensed by UEP. At UEP, Dr. Yadav is leading a team of engineers and scientists to bring the second-electron MnO2 and high voltage (2.45-2.8V) ZnMnO2 battery to commercialization.

Physical and Analytical Electrochemistry Division David C. Grahame Award Bruce Parkinson went to Iowa State University and received his BS in chemistry in 1972, doing undergraduate research with Prof. Dennis Johnson on rotating electrodes. He then went on to Caltech, where under the guidance of Prof. Fred Anson, he earned his PhD in 1977, working on double-layer effects on electrode kinetics and surface phase formation on mercury electrodes. After his postdoctoral studies at Bell Laboratories, he worked on semiconductor photoelectrochemistry with Adam Heller and Barry Miller. He became a staff scientist at the Ames Laboratory from 1979-1981, and then moved on to the Solar Energy Research Institute (now known as the National Renewable Energy Laboratory) in Golden, CO, where he was a senior scientist working on solar energy conversion. He then joined the Central Research and Development Department of the DuPont Company in 1985. In 1991, he became a professor of chemistry at Colorado State University until his departure to join the Department of Chemistry and the School of Energy Resources at the University of Wyoming in 2008, where he is now J. E. Warren Professor of Energy and Environment. His current research covers a wide range of areas, including electrochemistry, materials chemistry, nanomaterials, photoelectrochemistry on the surface of Mars, and recently, on membrane applications of new two-dimensional organic framework materials. He has more than 260 publications in peer-reviewed journals and holds five U.S. patents.

Section Awards Canada Section R. C. Jacobsen Award Aicheng Chen is a professor of chemistry, and Director of the Electrochemical Technology Centre (ETC) at the University of Guelph, Canada, and Tier 1 Canada Research Chair in Electrochemistry and Nanoscience. He received his MSc from Xiamen University, China, under the supervision of Prof. S.-G. Sun and his PhD from the University of Guelph in 1998 under the direction of Prof. J. Lipkowski. Subsequent to working in the chemical industry as a research scientist and electrochemical specialist for four years, Chen joined Lakehead University, Canada, in 2002 as an assistant professor, where he was promoted to associate professor in 2005, Tier 2 Canada Research Chair in 2006, and full professor in 2010. He received a senior Japan Society for the Promotion of Science (JSPS) Fellowship in 2006, and worked with Prof. B. Ohtani at Hokkaido University, Japan. During his sabbatical in 2008, he worked with Prof. R. Compton as a visiting scholar at Oxford University, U.K. Chen relocated from Lakehead University to the University of Guelph in 2017. Dr. Chen received the Student Award of The Electrochemical Society (ECS) Canada Section in 1997, and has been an active ECS member since then. He has served many roles with the ECS The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

AWARDS AWAPROGRAM RDS Canada Section: Executive Committee Member-At-Large (20022006), Secretary (2006-2007), Vice-Chair – Programs (2007-2008), Vice-Chair – Members (2008-2009), Chair (2009-2010), Past Chair (2010-2011), and Councillor (2011-present). As a faculty advisor and ETC Director, he facilitated the establishment of the ECS Guelph Student Chapter in 2018. He also served the International Society of Electrochemistry (ISE) as a local organizing committee member of the 58th ISE Annual Meeting held in Banff in 2007, the Canada Regional Representative (2010-2012), and the Chair of the 15th ISE Topic Meeting held in Niagara Falls in 2014. Prof. Chen has been a guest editor of the Journal of The Electrochemical Society, an associate editor of the Canadian Journal of Chemistry, and an editor of Electrochimica Acta. For his accomplishments, Prof. Chen has been awarded a number of awards, including the Lash Miller Award of the ECS Canada Section. He has also been named as fellow of the Chemical Institute of Canada, fellow of the Royal Society of Chemistry (UK), and fellow of the International Society of Electrochemistry.

Student Awards Energy Technology Division Graduate Student Award Sponsored by BioLogic Charles Tai-Chieh Wan is a PhD candidate in the Department of Chemical Engineering at the Massachusetts Institute of Technology, under the co-supervision of Prof. Fikile R. Brushett and Prof. Yet-Ming Chiang. In 2017, he received his BS in chemical and biomolecular engineering at Cornell University, where he graduated summa cum laude. Wan’s graduate thesis work focuses on developing designer electrode microstructures and surfaces for redox flow batteries by advancing unconventional yet potentially beneficial paradigms. His research efforts include leveraging principles of phase separation to synthesize and probe new electrode microstructures, investigating thin-film organic coatings to mediate the electrodeelectrolyte interface, and examining biomass-derived materials for use in redox flow batteries.

Industrial Electrochemistry and Electrochemical Engineering Division H. H. Dow Memorial Student Achievement Award Akshay Subramaniam studied chemical engineering at the Institute of Chemical Technology in India, receiving a bachelor’s degree in 2013, followed by a master’s degree from the Indian Institute of Technology (IIT) Bombay, India, in 2016. He is currently a doctoral student in chemical engineering at the University of Washington (UW), co-advised by Profs. Venkat Subramanian and Dan Schwartz. Akshay’s research focuses on the development and application of electrochemical modeling and simulation tools, with an emphasis on next-generation lithiummetal batteries. He is engaged in developing multiscale continuum simulation frameworks to advance understanding of the effect of external pressure and deformation effects on the overall performance and lifetime of lithium-metal cells. In doing so, he intends to leverage detailed electrochemical models and robust simulation approaches to correlate practically relevant cell-level variables with internal

electrochemistry. A secondary goal is the development of accessible design and validation tools to better inform experimental studies. Akshay is also engaged in more applied research on the development of reduced-order modeling techniques that can convert detailed models into computationally efficient forms that greatly increase their utility in real-time prediction, control, and optimization applications. Over the course of his doctorate, Akshay has been part of multiple academic and industrial collaborations, including the Battery500 consortium. He has co-authored seven peer-reviewed publications, with more manuscripts under preparation. He received departmental fellowships at UW in 2017, and the graduate fellowship from the UW Clean Energy Institute in 2018.

Industrial Electrochemistry and Electrochemical Engineering Division Student Achievement Award Eric McShane received his BS in chemical and biomolecular engineering from Cornell University in 2016, where he worked as an undergraduate researcher studying scalable synthesis methods for Si and Ge nanowires in the lab of Tobias Hanrath as part of the Rawlings Cornell Presidential Research Scholars Program. He then earned the NSF Graduate Research Fellowship before beginning his graduate studies at the University of California, Berkeley, in the fall of 2016, joining Bryan McCloskey’s lab to study the kinetic, transport, and degradation phenomena underpinning lithium-ion battery operation during a fast charge. McShane was recognized for his passion for teaching with the Outstanding Graduate Student Instructor Award.

San Francisco Section Daniel Cubicciotti Student Award

(Winner)

David Mackanic is founder and CEO of Anthro Energy, a company inventing nextgeneration polymer materials to create batteries that are flexible, safe, and high performance. He earned his PhD in chemical engineering from Stanford University, with a focus on polymer science and electrochemistry. David was supported by graduate research fellowships from Stanford University and the National Science Foundation. He was listed on Forbes 30 Under 30 in Energy for 2021, and was awarded the MRS Gold Award and the ACS Bright Science Award. Additionally, David previously worked in venture capital as an investment partner with the Dorm Room Fund.

(Honorable Mention)

Bin Yao received his PhD degree in chemistry and materials science at the University of California, Santa Cruz, in 2020, under the supervision of Prof. Yat Li. His research focuses on the rational design and additive manufacturing (3D printing) of electrodes for energy storage and conversion, including supercapacitors, batteries, and photoelectrochemical water splitting. He serves as a reviewer for more than 25 peerreviewed journals. He has received a number of awards, including the MRS Graduate Student Gold Award.

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

NE W MEMBERS

Member Spotlight I was inspired to join ECS at the recommendation of my former boss, Dr. Neal Golovin (consultant to ARPA-E at Booz Allen Hamilton). He suggested being involved with ECS would help me grow as an John Mitchell electrochemist and allow me access Daramic, LLC to research that I could use to further my knowledge.The benefit most valuable to me is the access to articles. I work as an R&D tech, so having access to articles has been one of the easiest ways for me to see what new information is out there.”

Venkat Viswanathan Carnegie Mellon University

Mami Nonoguchi Fujii

Some of the committee members recommended that I join.The most valuable benefit to me is the discount of the meeting registration fees.”

Nara Institute of Science and Technology

Would you like to be featured in our new Member Spotlight, and be entered for a chance to win a

ECS is my home community in terms of my research; ECS has been very generous to me over the years. I received the ECS San Francisco Section Daniel Cubicciotti Award in 2010 and was an ECS Herbert H. Uhlig Summer Fellow in 2009.”

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ECS is proud to announce the following new members for October, November, and December 2020. (Members are listed alphabetically by family/last name.) Members

Luiz Jacobsohn, Clemson, SC, USA

Asim Biswas, Guelph, ON, Canada

Joanna Burdynska, Bloomington, IN, USA

Pieremanuele Canepa, Singapore, Singapore, Singapore

Shima Dalirirad, Cherry Hill, NJ, USA

Emory De Castro, Cambridge, MA, USA

Mami Fujii, Ikoma, Nara, Japan

Mahesh Hariharan, Trivandrum, Kerala, India

Sridhar Kanuri, South Glastonbury, CT, USA Kanarindhana Kathirvel, Bangalore, KA, India Atsushi Kobayashi, Sapporo, Hokkaido, Japan

Anil Mane, Lemont, IL, U John Mitchell, Owensboro, KY, USA Bhuvaneswari Modachur Sivakumar, Richland, WA, USA Malachi Noked, Ramat Gan, Tel Aviv, Israel

Anant Patel, Lewis Center, OH, USA

Hanida Sary, Jakarta, Aceh, Indonesia Samaneh Shahgaldi, Milton, ON, Canada

Toshiyuki Tabata, Gennevilliers, Hauts-deSeine, France Yusuke Tsutsumi, Tsukuba, Ibaraki, Japan

Zhao Liu, Portland, OR, USA

Jozef Ociepa, London, ON, Canada

Carlos Villa, Lake Jackson, TX, USA

Wagon Wills, Farmington, MI, USA Terence Wong, Singapore, Singapore, Singapore

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

NE W MEMBERS Y

Litao Yan, Richland, WA, USA Michael Yandrasits, Hastings, MN, USA

Joseph Ziegelbauer, Sterling Heights, MI, USA

Student Members

Zahra Abooalizadeh, Calgary, AB, Canada Moin Ahmed, Waterloo, ON, Canada Elena Alfonso-Gonzalez, Mostoles, MAD, Spain Emilee Armstrong, Seattle, WA, USA Jaschar Atik, Münster, NRW, Germany

Behrouz Bahadormanesh, London, ON, Canada Srikanth Balijapelly, Rolla, MO, USA Tharanga Batugedara, Detroit, MI, USA Marlena Bela, Münster, NRW, Germany Debora Belami, Liverpool, Merseyside, UK Yasmine Benabed, Montreal, QC, Canada Joshua Botham, Swansea, Wales, UK Valerie Brunskill, Calgary, AB, Canada

Stephanie Castro Baldivieso, State College, PA, USA Murat Ceylan, Kocaeli, Izmit, Turkey Bowen Chen, Philadelphia, PA, USA Xin Chen, St. Andrews, Scotland, UK Victor Coca Ruiz, Cadiz, Andalucia, Spain Nicholas Cross, State College, PA, USA

Chathuri De Alwis, Raleigh, NC, USA Carlos Del Burgo Olivares, Arganda del Rey, MAD, Spain Pachari Detpunyawat, Calgary, AB, Canada Venkata Swaroopa Datta Devulapalli, Philadelphia, PA, USA

Rajkeerthi E., Chennai, TN, India Michael Eck, Medford, MA, USA Elnaz Erfanian, Calgary, AB, Canada

Carlos Fernandez, Atlanta, GA, USA Jayson Foster, Lakewood, CO, USA

Ozhan Gecgel, Lubbock, TX, USA Yang Goh, Los Angeles, CA, USA Manisha De Goonatilleke, Oak Ridge, TN, USA

Rebecca Griffin, Hereford, West Midlands, UK Alexandra Guboova, Kosice, Kosice Region, Slovakia Joseph Gurrentz, Austin, TX, USA

Aylin Habibiyan, Calgary, AB, Canada Jonathan Hammond, Vancouver, WA, USA Evan Hansen, Kelowna, BC, Canada Samuel Hardisty, Ramat Gan, Tel Aviv, Israel Matthias Hartmann, Steinfurt, NRW, Germany Mohamed Hassan, Potsdam, NY, USA Collan Henderson, Lexington, KY, USA Gabriel Hiestand, York, PA, USA Pia Hoenicke, Ulm, BW, Germany Tom Hsaio, Taipei, Tainan City, Taiwan

Tjark Ingber, Münster, NRW, Germany

Imen Karmous, Gennevilliers, Île-de-France, France Gayan Karunasinghe, Lexington, KY, USA Michelle Katz, Bellevue, WA, USA Kerstin Koeble, Ulm, BW, Germany

Robert Lavelle, State College, PA, USA Guesang Lee, Seattle, WA, USA Benjamin Lincoln, Calgary, AB, Canada Yan Luo, Chongqing, Chongqing, China

Edris Madadian, Scarborough, ON, Canada Negar Manafi Rasi, Calgary, AB, Canada Greg McArthur, Stourbridge, West Midlands, UK Chirag Mevada, Ahmedabad, GJ, India Julia Meyer, West Lafayette, IN, USA Anindya Mitra, Calgary, AB, Canada Shahab Mollah, Columbia, SC, USA

Arash Namaeighasemi, Athens, OH, USA Jonas Neumann, Münster, NRW, Germany Alexander Ng, Philadelphia, PA, USA Veronika Niscakova, Kosice, Kosice Region, Slovakia Viswanath Nukala, Stillwater, OK, USA Cassandra Nunez, University Park, PA, USA

Bebi Patil, Chelsea, MA, USA Yu Pei, Vancouver, BC, Canada Christoph Peschel, Münster, NRW, Germany Martina Petrakova, Kosice, Kosice Region, Slovakia Emily Pirtz, State College, PA, USA Susana Portela Garcia de Blas, Madrid, MAD, Spain

Ihsan Rachman, Saitama City, Saitama, Japan Rasoul Rahimzadeh Bafti, Lubbock, TX, USA Vaithilingam Rajendiran, Stillwater, OK, USA Milad Rasouli, Tehran, Tehran, Iran Friederike Reissig, Münster, NRW, Germany Renato Rogosic, Maastricht, Limburg, Netherlands Jimmy Rojas, Stanford, CA, USA Leah Rynearson, North Kingstown, RI, USA

Rebecca Schmitt, Albuquerque, NM, USA Emily Searles, Houston, TX, USA Akansha Sharma, Stillwater, OK, USA Prakhar Sharma, Chennai, TN, India Keita Shichijo, Fukuoka, Fukuoka, Japan Sharma Shrishti, Pilani Town, RJ, India Thomas Stracensky, Boston, MA, USA Björn Stuhmeier, Garching, Bavaria, Germany Helen Stute, Munich, Bavaria, Germany Qiang Sun, Malden, MA, USA

Ponsuge Thisera, Lexington, KY, USA

Pratik Walimbe, Pune, MH, India Nathan Wilson, Lubbock, TX, USA

Rui Yin, Philadelphia, PA, USA

Ehsan Zamani, Lincoln, NE, USA Jiaxun Zhang, College Park, MD, USA Tianyu Zhang, Cincinnati, OH, USA Yihui Zhang, Philadelphia, PA, USA Haoran Zhong, Stillwater, OK, USA Hanwei Zhou, West Lafayette, IN, USA

Tiwalola Ogunleye, Stillwater, OK, USA Kaitlynn Olczak, Gainesville, FL, USA Harmen Oterdoom, Düsseldorf, NRW, Germany

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

NE W MEMBERS New Members by Country

Look who joined ECS in the Fourth Quarter of 2020.

Canada

Japan

China

Netherlands

France

Singapore

Germany

Slovakia

India

Spain

Indonesia

Taiwan

Iran

Turkey

Israel

Canada................. 17 China..................... 1 France.................... 2 Germany.............. 12 India....................... 7 Indonesia............... 1 Iran........................ 1 Israel...................... 2 Japan..................... 5 Netherlands............ 1 Singapore.............. 2 Slovakia................. 3 Spain..................... 4 Taiwan.................... 1 Turkey.................... 1 UK.......................... 5 USA..................... 65

USA

240th ECS Meeting ORLANDO, FL October 10-14, 2021

Orange County Convention Center

SUBMIT NOW

Abstract deadline: April 9, 2021

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

ST UDENT NE WS Calgary Student Chapter The ECS Calgary Student Chapter has been active through the fall, passing the baton to new committee members for the 2020-2021 academic year, and pivoting from in-person events to socially distanced online workshops. The new executive committee was officially announced in September 2020: President Maedeh Pahlevaninezhad, Vice President Oliver Calderon, Secretary Jialang Li, Treasurer Samantha Luong, and Members at Large Annie Hoang, Hamideh Eskandari, Amir Alihosseinzadeh, and Irfan Aydogdu. From September to December, the chapter used two-hour online Zoom workshop formats to focus on professional skills development. A virtual “Industrial Roundtable on Careers in Science and Engineering” was held on November 12, 2020, with Holly Bri Sebastian (Director of Laboratory Operations, Psygen Labs Inc.), Derek Wasylenko (Research Scientist, NOVA Chemicals Corporation), and Tianpei Shu (Account Manager, Shennan Circuits Co., Ltd). The industry panelists invited people in the fields of pharmaceutical research, plastics development, and electronic component sales. The panelists gave attendees insights into their respective fields, commented on working life outside of academics, and advised members on job searches. The extended Q&A with panelists was especially popular and appreciated by students evaluating job prospects after graduation. On December 3, 2020, the chapter reached out to Syed Atif Pervez, Postdoctoral Fellow in the Department of Chemical and Petroleum Engineering at the University of Calgary, Canada, for a workshop

on “Interfaces in Solid State Li-Metal Batteries: Fundamentals & Applications.” He presented the fundamentals of Li-metal batteries and shared his research and associated goals, benefits, and challenges relating to Li-metal batteries.

Calgary area student chapter members elect a new slate of officers: (from top, left to right): Maedeh Pahlevaninezhad, President; Members at Large Behzad Fuladpanjeh-Hojaghan, Annie Hoang, Hamideh Eskandari, Marwa Atwa, and Zohreh Fallah; Jialang Li, Secretary; Samantha Luong, Treasurer; and Oliver Calderon, Vice President. Photo: Maedeh Pahlevaninezhad

Colorado School of Mines Student Chapter The ECS Colorado School of Mines Student Chapter held virtual elections for their executive committee on September 2, 2020. The new slate of officers is President Samantha Medina, Vice President Ivy Wu, Secretary Saeed Ahmadi Vaselabadi, and Treasurer William Smith. The student chapter met online several times in September for members to practice and receive feedback on their ECS talks. Students were encouraged to attend the online PRiME 2020 meeting

in October. The chapter held a digital electrochemistry trivia meeting with gift card prizes on January 28, 2021. Local industry professional Dean Frankel from Solid Power presented “Development of Solid State Lithium Batteries” online in February. Elections for the 20212022 academic year will be held on April 16, followed by a socially distanced outdoor pizza party.

Ilmenau Student Chapter Members of the recently founded ECS Ilmenau Student Chapter January 2020, described his experience as a doctoral student in an gathered for an initial chapter meeting on October 30, 2020. The electroplating company where he developed a predictive model for chapter developed from a PhD student meeting, formerly held the time dependence of concentrations in plating baths. René Böttcher biannually since 2017. This earlier meeting format combined with the presented a short hands-on seminar on the use of CAD programming current ECS group meeting provides opportunities for professional to design experimental setups like electrochemical cells. The meeting exchange and personal networking between internal and external concluded with Martin Leimbach’s presentation on scientific graduates. While the chapter is now centered in the Electrochemistry publishing in the field of electrochemistry and electroplating. and Electroplating Group at Technische Universität Ilmenau, Germany, where some PhD student members work in the labs, most members are employed in companies and research institutes throughout Germany and neighboring countries. Research interests range from lithium and post-lithium based battery systems to photoelectrochemical water splitting and deposition of metals from aqueous and non-aqueous electrolytes. Due to the pandemic, the October 30 meeting was a combination of virtual and in-person sessions at Ilmenau. It opened with the introduction of two new members who briefly described their research topics. Nurul Amanina Binti Omar discussed the electroless deposition of Ni-P-B coatings for wear protection applications. Lukas Grohmann reviewed the interdiffusion of gold and nickel, which occurs Participants of the ECS Ilmenau Student Chapter hybrid meeting on October 30, 2020. during the fabrication of glass feedthroughs for The meeting was held with the biannual PhD student meeting of the Electrochemistry and wire contacts in electronic devices and batteries. Electroplating Group at Technische Universität Ilmenau. Next, Christoph Baumer, who completed his PhD in Photo: René Böttcher The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

ST UDENT NE WS Munich Student Chapter More than 20 participants attended the December 16, 2020, ECS Munich Student Chapter Material & Methods Club series online webinar, “A three-dimensional, electro-chemo-mechanically coupled model for fully resolved finite element simulations of all-solid-state lithium-ion cells (ASSB).” The speaker, Stephan Sinzig, from the Institute for Computational Mechanics at Technische Universität München, Germany, focused on the geometric and mathematical setup of the ASSB model. Such an ASSB simulation can result in predicting the change in thickness of the cell components during cycling, the spatially resolved lithium concentration, or potential at any time during the applied charge protocol. Elaborating on the comparison of experimental and numerical results showed the model’s current limitations and capabilities. The conclusion: experiments and simulations have strengths and weaknesses; combining both can lead to new insights. The chapter’s annual meeting was digital. Members summarized 2020 activities, which unfortunately were vastly influenced by COVID-19. Annual elections were held, and planning for 2021 events began, including a Material & Methods Club webinar on the XPS analysis of energy materials.

The chapter plans to organize a large event on relevant aspects of climate change, which will be open to a broader public, including scientists and students. Excursions to industry partners are planned, including visits to the BMW battery pilot production plant and Freudenberg fuel cell research department. A goal is to promote further exchange with the ECS Ulm Student Chapter.

A screenshot from the ECS Munich Student Chapter’s ASSB modeling webinar featuring speaker Stephan Sinzig. Photo: Christoph Schmidt

National Chiao Tung University Student Chapter The first activity of the ECS National Chiao Tung University accomplished and enthusiastic speakers. We eagerly look forward to (NCTU) Student Chapter was a professionally guided tour of the planning future activities. National Synchrotron Radiation Research Center (NSRRC), Taiwan, on October 8, 2020. More than 14 student members actively participated in the event, where they learned about the scientific and engineering facilities of synchrotron radiation. During the visit of the experimental field, members engaged in talks, small discussions, and connected with other students and researchers. The guide presented a video of the working of two beamlines, described the background of NSRRC, and then demonstrated two representative beamlines, Taiwan Photon Sources (TPS) and Taiwan Light Source (TLS). An expert in highenergy powder diffraction, Yu-Chun Chuang, provided insights into the High-Resolution Powder X-Ray Diffraction beamline in 19A beamline source. Along with getting solutions to research problems, the tour provided members with opportunities for professional development and engaging with NSRRC scientists. On August 15, 2020, the student chapter’s annual election brought new members and Attendees and members of the ECS NCTU Student Chapter with Prof. Fang-Chung Chen at the officers to the group. The chapter is grateful for National Synchrotron Radiation Research Center. the opportunities ECS provides to meet with Photo: Gajendra Suthar

Advertisers Index BioLogic............................................................................ 4 El-Cell............................................................................. 19 ECS Transactions 239th ECS Meeting with IMCS 18.................................................................. 46

Gamry............................................................................... 6 Park Systems....................................................................17 Pine Research Instrumentation....................................... 2 Scribner Associates.......................................................... 1 Wiley............................................................................... 44 The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

ST UDENT NE WS National Tsing Hua University Student Chapter The ECS National Tsing Hua University (NTHU) Student Chapter was founded in 2020. The chapter members thank the Society for providing NTHU students with the opportunity to connect internationally and grow academically. The chapter is based in the Department of Materials Science and Engineering building. It is deeply engaged in the Industry Mentor Program, where alumni who are senior supervisors in industry serve as mentors. The program enables chapter members to gain insight into industry trends and research opportunities. Students visited several prominent industrial companies in Taiwan over the last six months. The chapter is collaborating with Epistar Corp., the largest manufacturer of light-emitting diodes in Taiwan and a leading company in solid state lighting, new generation quantum dot lighting, and displays. Industry Mentor Program workshops are taking place in the spring semester. The chapter is hosting a workshop at Touch Taiwan–Display International 2021, held from April 21-23, 2021. The chapter is proud to participate in this renowned international exhibition, which is now the most influential display industry supply chain exhibition in the world.

The ECS National Tsing Hua University (NTHU) Student Chapter hosts one of its workshops. Photo: Department of Materials Science and Engineering

Norwegian University of Science and Technology Student Chapter The highlight of 2020 for the ECS Norwegian University of Science and Technology (NTNU) Student Chapter was the election on September 8 of new board members: President Faranak Foroughi, Vice President Simon Birger Byremo Solberg, Secretary Henrik Erring Hansen, and Treasurer Harald Norrud Pollen. A kickoff meeting planned for November 2020 to introduce the ECS student chapter and its incredible benefits to undergraduate and graduate students was canceled, unfortunately, due to COVID-19. We are looking forward to some fun events for this upcoming year.

New ECS Norwegian University of Science and Technology Student Chapter board members are (from left to right): Treasurer Harald Norrud Pollen, Secretary Henrik Erring Hansen, President Faranak Foroughi, and Vice President Simon Birger Byremo Solberg. Photo: Faranak Foroughi

Pennsylvania State University Student Chapter The ECS Board of Directors officially approved the ECS Pennsylvania State University Student Chapter on October 16, 2020. The chapter is off to a great start with more than 25 undergraduate and graduate student members on the roster. The goal is simple—to unite students and researchers from across the university campus who share a common interest in electrochemistry. The chapter hosted five virtual seminars during the fall 2020 semester featuring talks by university postdoctoral researchers and faculty from departments including Chemical Engineering, and Materials Science and Engineering. The seminars covered a broad range of experimental and computational research topics and shed light on exciting electrochemical research. Despite being virtual, the seminars

were widely attended by students, staff, and faculty. Seminar speakers included Nathan Smith, Ismaila Dabo, Michael Janik, Susan Sinnott, and Michael Hickner. The chapter is hosting additional virtual seminars to promote electrochemical research. Despite the challenges of the COVID-19 pandemic, the chapter is working actively to uphold The Electrochemical Society’s mission and engage with potential new members. While unable to meet in person this spring, the chapter’s virtual social events are helping to build community among student members. The chapter is very excited to be part of the ECS community and looks forward to establishing connections and collaborating with fellow student chapters.

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

ST UDENT NE WS Purdue University Student Chapter The ECS Purdue University Student Chapter was founded to promote networking, collaboration, engagement, and exchange of scientific inquiries and perspectives related to electrochemistry among undergraduate and graduate students, faculty members, and others in the scientific community. The chapter organizes regular talks, meetings, coffee hours, and lab tours. However, the COVID-19 pandemic, which is undoubtedly more than just a health crisis, hindered planned in-person activities (such as high school outreach, a poster competition, and setting up a booth at on-campus cultural/scientific events). In the hope of creating a new normal amid unprecedented challenges, the chapter launched a weekly webinar series during the 2020 fall semester. • Siddhartha Das from the Screenshots from lectures in the ECS Purdue University Student Chapter Fall Webinar Series. University of Maryland, Photo: Susmita Sarkar and Navneet Goswami Department of Mechanical • In his lecture on “Inactive and Active Safety of Lithium-ion Engineering, was the inaugural Batteries,” Kyle Crompton (Naval Surface Warfare Center, speaker. In “Ionics and Liquid Transport at PolyelectrolyteCrane Division) highlighted thermal runaway events of battery Brush-Functionalized Interfaces,” he elaborated on the systems and relevant destructive testing methods. combined interactions of the structure, ionics, and liquid transport at the polyelectrolyte-brush-grafted interface that was • Hongyi Xu (University of Connecticut) in his talk, investigated through all-atom molecular dynamics simulations. “Computational Modeling of Battery Separator Microstructure by Statistical Characterization and Stochastic Reconstruction,” • Rebecca Ciez (Purdue University, Department of Mechanical explained innovative virtual reconstruction techniques Engineering) highlighted the thermo-economic analysis applicable to different material systems and how those can be associated with the use of energy storage systems for leveraged to compute microstructural properties of interest. carbon footprint reduction in her talk, “Energy storage for decarbonization goals.” • Ryan Kohlmeyer (Xerion Advanced Battery Corp/Air Force Research Laboratory), in “Exploring Routes to Enable Next • Judy Jeevarajan (Underwriters Laboratories) presented Generation, Safer & High-Temperature Li-Ion Batteries,” “Application-oriented Research and its Relevance to Standards described a novel thermally stable separator that can be in Batteries.” She demonstrated the myriad safety hazards employed to extend the operational temperature window of stemming from battery applications and provided critical lithium-ion battery systems. insights about adopting suitable safety standards. • Chien-Fan Chen (Enphase Energy) discussed design principles related to battery modeling from the cell/module level to the system level in “ESS Lithium-ion Battery Modeling and Applications.” • Corey T. Love (U.S. Naval Research Laboratory) delivered “Small Thermal Gradients Can Lead to Big Changes in Electrochemical Performance & Safety of Li-ion Batteries,” speaking at length on how the electrochemical response of battery systems changes when a thermal gradient is subjected across the electrodes. • In “Understanding Lithium Deposition and Dendrite Growth in LLZO Solid Electrolytes,” Pallab Barai (Argonne National Laboratory) elucidated the dendrite growth mechanism in LLZO electrolytes through a mesoscale modeling perspective and shed light on possible strategies to suppress the same.

The webinar series was well received, led to great research discussions, and was a great morale booster for students from various science and engineering disciplines. The series helped attendees conceptualize aspects of electrochemistry in industry and national labs that they may not experience in academic settings. Because we experienced these benefits firsthand during the pandemic, virtual learning and webinars will be a part of our regular events. Follow the ECS Purdue Student Chapter on Twitter (@EcsPurdue). We are keen to collaborate with ECS student chapters around the world and organize virtual events. For more information, contact purdueecschapter@gmail.com.

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

ST UDENT NE WS University of Cambridge Student Chapter The ECS University of Cambridge Student Chapter kicked off its inaugural year in February 2020, with “Challenges for Electrochemistry in the 21st Century.” Jeremy Baumberg, Erwin Reisner, Siân Dutton, and Alex Forse, academics working across a range of electrochemical topics, presented 15-minute talks introducing and explaining the trials and tribulations their groups overcome to tackle electrochemical challenges facing society. Topics ranged from the development of powerful optical characterization techniques to novel biocatalyst electrode architectures, from using magnetic measurements to identify the state of charge of lithium batteries through methods of achieving net-zero energy storage. The chapter’s social networking channels raised a great deal of interest for the evening event. Over 60 attendees reveled in the intellectual discussion and the brief networking and soft drinks reception that followed. Several individuals expressed interest in attending other similar events and joining our mailing list. Due to the pandemic, the chapter’s second event was digital. Students delivered brief three-minute one-slide presentations on their research. The event provided a platform to introduce students’ research, receive valuable talk practice, and facilitate interstudent communication on a variety of topics related to the use of electrochemistry and electrochemical methods. Six MS to third-year

PhD students presented a variety of topics. A brief Q&A session followed with a prize awarded to the best speaker. The event was well received by speakers and attendees. The ECS University of Cambridge Student Chapter hopes to facilitate similar events in the future.

One of the speaker events hosted by the ECS University of Cambridge Student Chapter. Photo: Rajesh Jethwa

University of Kentucky Student Chapter The ECS University of Kentucky (UK) Student Chapter hosted three virtual seminars during the fall semester. Time was allotted at the end of each seminar for speaker-attendee interaction. Early in the semester, ECS members discussed ways to recruit graduate and undergraduate students from various UK departments. This year, the chapter attracted 17 members from departments including Chemistry, Materials Engineering, Chemical Engineering, Electrical Engineering, Mechanical Engineering, and Physics. In the first seminar, “Structure, Surface, and Interfacial Modifications of Carbon and Supported-Metal Electrodes for Electrochemical Carbon Dioxide Conversion,” Namal Wanninayake (UK Department of Chemistry) addressed the need to close the carbon cycle to mitigate the effects of greenhouse CO2 on climate change. He focused on how structural, interfacial, and surface modification of nanostructures can lead to an effective catalyst for the electroreduction of CO2. The next seminar, “Polymer Electrolytes for Advanced Electrochemical Devices,” presented by Yu Seung Kim (Los Alamos National Laboratory), concentrated on the importance of designing effective polymer electrolytes for various electorchemical applications. He presented how these thoughtfully designed electrolytes can improve performance in alkaline anion-exchange membrane fuel cells, low-temperature fuel cells, high-temperature fuel cells, and alkaline water electrolyzers. Xin Gao (Research Engineer, University of Kentucky Center for Applied Energy Research) showed that capacitive deionization could

be more cost effective than reverse osmosis for water purification in “Surface charge effect on salt removal in a capacitive deionization cell.” He also discussed how the surface charge and porosity of the carbon electrodes could play a key role in CDI cell performance. Faculty and students from the UK College of Engineering and the College of Arts & Sciences attended these online events. We printed T-shirts with the ECS logo to distribute to current and new members.

“Polymer Electrolytes for Advanced Electrochemical Devices” presented by Yu Seung Kim at the ECS UK Student Chapter seminar.

University of Washington Student Chapter The ECS University of Washington (UW) Student Chapter stayed connected through the beginning of the academic year. Several UW chapter members attended and presented at the PRiME 2020 meeting, where they engaged in conversations about their research and learned about advances in the field.

At a chapter kickoff meeting in the fall, students met with others who are passionate about electrochemical and solid state sciences. Conversations continued through the winter months. The chapter’s upcoming meetings involve journal club discussions and presentations from members about their research. These dialogs are essential for engaging students in electrochemistry and staying informed about current research.

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

ST UDENT NE WS University of Waterloo Student Chapter The ECS University of Waterloo Student Chapter hosted three events for the community’s benefit. As the COVID-19 pandemic triggered a crisis in the job market, we stepped up to support job search efforts for recent graduates and graduate students nearing the end of their degrees. At the virtual Mini Career Fair 2021 on January 28, students networked virtually with four Canadian-based electrochemistryrelated companies. Felice Frankel, a professional science photographer and research scientist at the Massachusetts Institute of Technology

(MIT), presented a virtual workshop titled “Designing Scientific Figures” on February 25. She shared tips and processes for creating compelling scientific figures and photographs for professional scientific publications. On March 25, students learned to effectively present ideas and scientific findings to their target audience in a virtual workshop, “Scientific Presentation Skills.” Presenter Michael Alley, Associate Professor of Engineering Communication at Pennsylvania State University, is the author of several popular books on scientific communication.

Western University Student Chapter The ECS Western University Student Chapter hosted the fourth Western University ECS Student Symposium virtually on December 9-10, 2020. Lectures by 10 chapter graduate students and postdocs were enjoyed by 65 unique attendees from Western’s Physics, Engineering, Chemistry, and Biology Departments in a laid-back, discussion-oriented symposium. The objective was to foster scientific relationships between different disciplines, promote research, and provide a safe place to ask simple questions stimulating scientific growth. Guest speakers included Yolanda Hedberg (Western University, Canada) on “A Discussion on Different Paradigms of Corrosion Mechanism in the Human Body,” and Jeff Dahn (Dalhousie University, Canada), “How Long Can Li-Ion Cells Last in Electric Vehicle and Grid Energy Applications?” These talks provided remarkable insights into world-class research covering a range of interesting topics. Our data analysis workshop series continued on November 6 with a virtual workshop on X-ray photoelectron spectroscopy (XPS) by Mark Biesinger. As Director of Surface Science at Western University, Biesinger applies his research skills in the analysis of metallic XPS spectroscopy on samples from many industrial and academic sectors, including energy and nuclear, mineralogy, health services, automotive, aerospace, environmental, and electronics. He lectured on the fundamentals of XPS analysis and detailed studies of real datasets submitted by members. Biesinger provided insight into the analysis of different elements and common challenges and errors that occur in XPS fitting. The event was a resounding success, with

over 35 members attending, including international attendees from two universities. Our chapter hopes to continue our electrochemical/surface analysis workshop series in order to educate members, promote members’ research, and develop meaningful connections. We look forward to our fifth annual research symposium this year! These events provide an excellent opportunity for members to connect with each other—a difficult task during pandemic lockdowns.

A virtual group picture of attendees at the fourth annual Western University ECS Student Symposium. Photo: Jonathan R. Adsetts

Xi’an Jiaotong University Student Chapter The first seminar of the ECS Xi’an Jiaotong University Student Chapter was held in the university’s Physics Electronic Department on November 19, 2020. Researchers from different fields, including thin-film transistors (TFTs), diamond and graphene materials, and plasma, attended the seminar. Reports by Zhu Yifei and Wang Ruozhen were discussed. Chairman Wang Yaogong introduced chapter members to the history of ECS. Liu Weihua shared research on hysteresis behavior of graphene field-effect transistors due to hydrogen-complexed defects in silicon dioxide. The direction of all-inorganic hybrid halogen perovskite solar cells was the topic of Yin Xingtian’s presentation. Li Gaoming described research on ultraviolet detectors’ field and analyzed the influence of surface plasma on the performance of semiconductor ultraviolet photodetectors. Li Jie shared the characteristics of secondary electron emission. Participants gather for the ECS Xi’an Jiaotong University Student Chapter’s first seminar. We plan to hold seminars regularly. The hope Photo: Linggung Liu is that with the ECS Xi’an Jiaotong University Student Chapter’s help, cooperation between disciplines will be further deepened. 88

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

CALL FOR PAPERS

240th ECS Meeting

ORLANDO, FL October 10-14, 2021

Orange County Convention Center

Abstract Submission Deadline: April 9, 2021

www.electrochem.org/240

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

240TH ECS MEETING General Information

The 240th ECS meeting will be held in Orlando, Florida, from October 10-14, 2021, at the Orange County Convention Center. This international conference will bring together scientists, engineers, and researchers from academia, industry, and government laboratories to share results and discuss issues on related topics through a variety of formats, such as oral presentations, poster sessions, panel discussions, tutorial sessions, short courses, professional development workshops, a career fair, and exhibits. The unique blend of electrochemical and solid state science and technology at an ECS meeting provides an opportunity and forum to learn and exchange information on the latest scientific and technical developments in a variety of interdisciplinary areas.

Abstract Submission

Technical Exhibit

The 240th ECS Meeting will include a Technical Exhibit, featuring presentations and displays by dozens of manufacturers of instruments, materials, systems, publications, and software of interest to meeting attendees. Coffee breaks are scheduled in the exhibit hall along with evening poster sessions. Interested in exhibiting at the meeting with your company? Exhibitor opportunities include unparalleled benefits and provide an extraordinary chance to present your scientific products and services to key constituents from around the world. Exhibit opportunities can be combined with sponsorship items and are customized to suit your needs. Please contact sponsorship@ electrochem.org for further details.

To give an oral or poster presentation at the 240th ECS Meeting, you must submit an original meeting abstract for consideration via the ECS website, https://ecs.confex.com/ecs/240/cfp.cgi no later than April 9, 2021. Faxed, e-mailed, and/or late abstracts will not be accepted. Meeting abstracts should explicitly state objectives, new results, and conclusions or significance of the work. Once the submission deadline has passed, the symposium organizers will evaluate all abstracts for content and relevance to the symposium topic, and will schedule all acceptable submissions as either oral or poster presentations. In June 2021, Letters of Acceptance/Invitation will be sent via email to the corresponding author of all accepted abstracts, notifying them of the date, time, and location of their presentation. Regardless of whether you requested a poster or an oral presentation, it is the symposium organizers’ discretion to decide how and when it is scheduled.

Meeting Registration

Paper Presentation

In June 2021, Letters of Invitation will be sent via email to the corresponding author of all accepted abstracts, notifying them of the date, time, and location of their presentation. Anyone else requiring an official letter of invitation should email abstracts@electrochem.org; such letters will not imply any financial responsibility of ECS.

Oral presentations must be in English; LCD projectors and laptops will be provided for all oral presentations. Presenting authors MUST bring their presentation on a USB flash drive to be used with the dedicated laptop that will be in each technical session room. Speakers requiring additional equipment must make written request to meetings@electrochem.org at least one month prior to the meeting so that appropriate arrangements may be worked out, subject to availability, and at the expense of the author. Poster presentations must be displayed in English, on a board approximately 3 feet 10 inches high by 3 feet 10 inches wide (1.17 meters high by 1.17 meters wide), corresponding to their abstract number and day of presentation in the final program.

Meeting Publications

ECS Meeting Abstracts—All meeting abstracts will be archived in the ECS Digital Library, copyrighted by ECS, and all abstracts become the property of ECS upon presentation. ECS Transactions—Select symposia will be publishing their proceedings in ECS Transactions (ECST). Authors presenting in these symposia are strongly encouraged to submit a full-text manuscript based on their presentation. Issues of ECST will be available for sale on a pre-order basis, as well as through the ECS Digital Library and the ECS Online Store. Please see each individual symposium listing in this call for papers to determine if your symposium will be publishing an ECST issue. Please visit the ECST website for additional information, including overall guidelines, author and editor instructions, a downloadable manuscript template, and more. ECSarXiv—All authors are encouraged to submit their full-text manuscripts, posters, slides, or data sets to ECS’s preprint service, ECSarXiv. For more information on this offering, visit the ECSarXiv website. Please note that submission to ECSarXiv does not preclude submission to ECST. ECS Journals–Authors presenting papers at ECS meetings, and submitting to ECST or ECSarXiv, are also encouraged to submit to the Society’s technical journals: Journal of The Electrochemical Society and ECS Journal of Solid State Science and Technology. Although there is no hard deadline for the submission of these papers, it is considered that six months from the date of the symposium is sufficient time to revise a paper to meet the stricter criteria of the journals. Author instructions are available on the ECS journals website.

Short Courses

Four short courses will be offered on Sunday, October 10, 2021, from 08001630h. Short courses require advanced registration and may be cancelled if enrollment is under 10 registrants in the respective course. The following short courses are scheduled: 1) Advanced Impedance Spectroscopy, 2) Fundamentals of Electrochemistry: Basic Theory and Kinetic Methods and 3) Battery Safety and Failure Modes, and 4) Operation and Exploitation of Electrochemical Capacity Technology. Registration opens June 2021. 90

All participants—including authors and invited speakers—are required to pay the appropriate registration fees. Meeting registration information will be posted on the ECS website as it becomes available. The deadline for discounted early registration is September 13, 2021.

Hotel Reservations

The 240th ECS meeting will be held at the Orange County Convention Center. Please refer to the meeting website for the most up-to date information on hotel availability and information about the blocks of rooms where special rates have been reserved for participants attending the meeting. The hotel block will be open until September 13, 2021 or until it sells out.

Letter of Invitation

Financial Assistance

ECS divisions and sections offer travel grants to students, postdoctoral researchers, and young professionals to attend ECS biannual meetings. Applications are available beginning April 9, 2021, at www.electrochem.org/ travel-grants and must be received no later than the submission deadline of June 29, 2021. Additional financial assistance is very limited and generally governed by symposium organizers. Individuals may inquire directly to organizers of the symposium in which they are presenting to see if funding is available. For general travel grant questions, please contact travelgrant@electrochem.org.

Sponsorship Opportunities

ECS biannual meetings offer a wonderful opportunity to market your organization through sponsorship. Sponsorship allows exposure to key industry decision makers, the development of collaborative partnerships, and potential business leads. ECS welcomes support in the form of general sponsorship at various levels. Sponsors will be recognized by level in the Meeting Program, meeting signage, and on the website. In addition, sponsorships are available for the plenary, meeting keepsakes, and other special events. Advertising opportunities for the Meeting Program as well as in Interface magazine are also available. Please contact sponsorship@ electrochem.org for further details. ECS also offers specific symposium sponsorship. By sponsoring a symposium your company can help offset travel expenses, registration fees, complimentary proceedings, and/or host receptions for invited speakers, researchers, and students. Please contact Francesca.Spagnuolo@electrochem.org for further details.

Contact Information

If you have any questions or require additional information, contact ECS. The Electrochemical Society 65 South Main Street, Pennington, NJ, 08534-2839, USA tel: 1.609.737.1902, fax: 1.609.737.2743 meetings@electrochem.org www.electrochem.org The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

SYMPOSIUM TOPICS A— Batteries and Energy Storage New Approaches and Advances in Electrochemical Energy A01— Systems A02—

Sodium and Lithium Intercalation Chemistry for Rechargeable Batteries - Special Symposium in Honor of Claude Delmas

A03— Lithium Ion Batteries Fast Charging in Electrochemical Systems - Batteries and A04— Supercapacitors B— Carbon Nanostructures and Devices B01—

Carbon Nanostructures: From Fundamental Studies to Applications and Devices Nanocarbons

C— Corrosion Science and Technology C01— Corrosion General Poster Session C02— Critical Factors in Localized Corrosion 9 C03— Corrosion Mechanisms and Methods D— Dielectric Science and Materials D01— Semiconductors, Dielectrics, and Metals for Nanoelectronics 18 D02—

Photovoltaics for the 21st Century 17: New Materials and Processes

Processing Materials and Integration of Damascene and 3D D03— Interconnects 10 D04—

The Science and Applications of Topological and Correlated Materials 2

D05—

Water-Energy Nexus Research Relating to Semiconducting Materials

D06— Atmospheric Pressure Plasma Processing E— Electrochemical/Electroless Deposition E01— Current Trends in Electrodeposition - An Invited Symposium E02— Additive Manufacturing by Electro- and Electroless Deposition E03—

Electrodeposition of Reactive Metals and Compounds 2 (No Water Allowed)

F— Electrochemical Engineering F01—

Advances in Industrial Electrochemistry and Electrochemical Engineering

F02— Electrochemical Separations and Sustainability 4 F03— Electrochemical Conversion of Biomass 3

I05— J—

Advanced Manufacturing for High-Temperature Materials and Devices Luminescence and Display Materials, Devices, and Processing

J01— Luminescence: Fundamentals and Applications J02—

Ultraviolet and Infrared Luminescent Materials: Development and Applications

K— Organic and Bioelectrochemistry K01— Advances in Organic and Biological Electrochemistry L— Physical and Analytical Electrochemistry, Electrocatalysis, and Photoelectrochemistry L01—

Physical and Analytical Electrochemistry, Electrocatalysis, and Photoelectrochemistry General Session

L02— Advanced Techniques for In Situ Electrochemical Systems 4 L03— The Brain and Electrochemistry 3 L04— Education in Electrochemistry 3 L05— Electrochemical Water Remediation L06— Nitrogen Reduction L07— Electrochemical Luminescence and Fluorescence L08— Pulsed Electroanalytical Techniques L09— Electrochemistry of Two-Dimensional Materials L10— Supramolecular Materials M— Sensors M01— Recent Advances in Sensors Systems M02—

Biosensors and Nanoscale Measurements: A Symposium in Honor of Professors Nongjian Tao and Stuart Lindsay

Z— General Z01— General Student Poster Session Z02— Electrochemistry in Space 2 Z03—

Electrochemical and Solid State Science and Engineering Applied to COVID Issues

Z04—

Electrochemical Recovery, Recycling, and Sustainability of Critical and Value Added Materials

Z05—

Electrochemical and Solid State Data Science Showcase and Software Sprint

F04— Pulse and Reverse Pulse Electrolytic Processes 3 F05— Reduction of CO2: From Laboratory to Industrial Scale 2 F06— Process Intensification Using Electrochemical Routes G— Electronic Materials and Processing G01— Atomic Layer Deposition Applications 17 G02— Semiconductor Process Integration 12 G03— Thermoelectric and Thermal Interface Materials 7 H— Electronic and Photonic Devices and Systems H01—

State-of-the-Art Program on Compound Semiconductors 64 (SOTAPOCS-64)

H02— Low-Dimensional Nanoscale Electronic and Photonic Devices 14 H03— Gallium Nitride and Silicon Carbide Power Technologies 11 I— Fuel Cells, Electrolyzers, and Energy Conversion I01— Polymer Electrolyte Fuel Cells & Electrolyzers 21 (PEFC&E 21) I02— Materials for Low Temperature Electrochemical Systems 7 I03— Renewable Fuels via Artificial Photosynthesis or Heterocatalysis 7 I04—

Important Dates and Deadlines Meeting abstracts submission deadline............................April 9, 2021 Notification to corresponding authors of abstract acceptance or rejection.................................June 14, 2021 Technical program published online.............................. May 10, 2021 Meeting registration opens...................................................June 2021 ECS Transactions submission site opens.........................June 18, 2021 Travel grant application deadline..................................June 28, 2021 Meeting sponsor and exhibitor deadline (for inclusion in printed materials).................................... July 30, 2021 ECS Transactions submission deadline............................ July 16, 2021 Travel grant approval notification................................August 23, 2021 Hotel and early meeting registration deadlines.......................................... September 13, 2021 Release date for ECS Transactions........ on or before October 1, 2021

Crosscutting Materials Innovation for Transformational Chemical and Electrochemical Energy Conversion Technologies 4

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

ECS MEEting AdvErtiSing DigitAl ExhibitOr AnD VEnDOr guiDE

• Strategic digital showcase for your organization and product(s) • Brings brand stories to customers— including video • Distributed to all live and online audiences Contact Anna.Olsen@electrochem.org for more information. 92

The Electrochemical Society Interface • Spring 2021 • www.electrochem.org

2021 ECS Institutional Members Benefactor Bio-Logic USA/Bio-Logic SAS (13)

Gelest, Inc. (12)

Duracell (64)

Hydro-Québec (14)

Gamry Instruments (14)

Pine Research Instrumentation (15)

Patron Energizer (76)

Lawrence Berkeley National Laboratory (17)

Faraday Technology, Inc. (15)

Scribner Associates, Inc. (25)

GE Global Research Center (69)

Toyota Research Institute of North America (13)

Sponsoring BASi (6)

Nissan Motor Co., Ltd. (14)

Central Electrochemical Research Institute (28)

Pacific Northwest National Laboratory (PNNL) (2)

DLR-Institut für Vernetzte Energiesysteme e.V. (13)

Panasonic Corporation (26)

EL-CELL GmbH (7)

Permascand AB (18)

Ford Motor Corporation (7)

Teledyne Energy Systems, Inc. (22)

GS Yuasa International Ltd. (41)

The Electrosynthesis Company, Inc. (25)

Honda R&D Co., Ltd. (14)

Center for Solar Energy and Hydrogen Research Baden-Württemberg (ZSW) (17)

Medtronic Inc. (41)

Sustaining General Motors Holdings LLC (69)

Occidental Chemical Corporation (79)

Giner, Inc./GES (35)

Sandia National Laboratories (45)

Cummins, Inc. (3)

Western Digital GK (7)

Ion Power Inc. (7)

Technic, Inc. (25)

Kanto Chemical Co., Inc. (9)

Westlake (26)

Los Alamos National Laboratory (13)

Yeager Center for Electrochemical Sciences (23)

Microsoft Corporation (4)

01/08/2021

Please help us continue the vital work of ECS by joining as an institutional member today. Contact Anna.Olsen@electrochem.org for more information.

Spring 2021

VOL. 30, NO. 1, S p r i n g 2 0 2 1

Solid State Aspects of Energy Conversion

VOL. 30, NO. 1

8 26

2020 Year in Review

Free Radicals: Winner Takes All

239th ECS Meeting Highlights

A Vision for Sustainable Energy