A Novel Approach for Post-Mortem Analysis in All-Solid-State Batteries: Isolating Solid Polymer Electrolytes from Lithium Anodes

Ortal Breuer, Ido Rozen, Nicole Leifer, Gayathri Peta, Miryam Fayena-Greenstein, Doron Aurbach, Gil Goobes

Research output: Contribution to journalArticlepeer-review

Abstract

Polymeric electrolytes are currently at the forefront of research for the next generation of lithium all-solid-state batteries. Polyethylene oxide (PEO), a commonly used polymer for these batteries, operates at elevated temperatures at which it reacts with active metal electrodes (e.g., lithium). Rich surface chemistry is developed at the Li-PEO interfaces, thereby controlling these batteries’ electrochemical behavior. Interfacial studies are essential to comprehend batteries’ stabilization or capacity fading mechanisms. For that, post-mortem analysis with an emphasis on interfaces is a necessary approach to underpinning these mechanisms. While it can be readily done with liquid electrolytes, post-mortem characterization of similar interfaces with solid electrolytes is hampered by the Li-PEO stack firm adhesion, which is impossible to separate. Here, various methods were attempted to separate polymer electrolytes from metallic anodes after Li symmetric cells’ operation, which is a necessary step for solid-state NMR characterization. By a simple method involving exposure to N2(g) atmosphere, PEO-based solid electrolyte samples were successfully isolated from lithium anodes while preserving their morphology and chemical characteristics to enable their direct analysis. This method’s concept was approved by Solid-state NMR spectroscopy. This work opens the door for post-operative analysis of many kinds of solid-state Li batteries.

Original languageEnglish
Article number020532
JournalJournal of the Electrochemical Society
Volume171
Issue number2
DOIs
StatePublished - 1 Feb 2024

Bibliographical note

Publisher Copyright:
© 2024 The Author(s). Published on behalf of The Electrochemical Society by IOP Publishing Limited.

Funding

Partial financial support was provided by the Israel Science Foundation (ISF) and the U.S.-Israel Binational Industrial Research and Development (BIRD) Foundation. The authors declare no competing financial interests. OB thanks MOST for a STEM scholarship for PhD students. The authors thank Dr. Shay Tirosh for the helpful discussion.

FundersFunder number
U.S.-Israel Binational Industrial Research and Development
BIRD Foundation
Ministry of Science and Technology of the People's Republic of China
Israel Science Foundation

    Keywords

    • PEO
    • SS NMR spectroscopy
    • all-solid-state lithium batteries
    • polymer electrolytes
    • post-mortem analysis

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