Operando Study Insights into Lithiation/Delithiation Processes in a Poly(ethylene oxide) Electrolyte of All-Solid-State Lithium Batteries by Grazing-Incidence X-ray Scattering

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Abstract
Poly(ethylene oxide) (PEO)-based composite electrolytes (PCEs) are considered as promising candidates for next-generation lithium-metal batteries (LMBs) due to their high safety, easy fabrication, and good electrochemical stability. Here, we utilize operando grazing-incidence small-angle and wide-angle X-ray scattering to probe the correlation of electrochemically induced changes and the buried morphology and crystalline structure of the PCE. Results show that the two irreversible reactions, PEO-Li+ reduction and TFSI- decomposition, cause changes in the crystalline structure, array orientation, and morphology of the PCE. In addition, the reversible Li plating/stripping process alters the inner morphology, especially the PEO-LiTFSI domain radius and distance between PEO-LiTFSI domains, rather than causing crystalline structure and orientation changes. This work provides a new path to monitor a working battery in real time and to a detailed understanding of the Li+ diffusion mechanism, which is essential for developing highly transferable and interface-stable PCE-based LMBs.
Funding Information
  • Deutsche Forschungsgemeinschaft (EXC 2089/1390776260, MU1487/32)
  • Center for NanoScience, Ludwig-Maximilians-Universit?t M?nchen
  • Bayerisches Staatsministerium f?r Bildung und Kultus, Wissenschaft und Kunst
  • China Scholarship Council
  • National Natural Science Foundation of China (52061135110)
  • International Research Training Group 2022 Alberta/Technical University of Munich International Graduate School for Environmentally Responsible Functional Hybrid Materials
  • Center for NanoScience

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