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Layered cathodes are essential for achieving a high energy density in rechargeable lithium-ion batteries, but they suffer from capacity fade due to local crystal phase transitions during charge−discharge cycles. Understanding these phase transitions is essential to minimizing their effects, but their nanometer size and sensitivity to experimental conditions make observation difficult. Here, we visualized nanometer-scale crystal phases within an epitaxial LiCoO2 cathode after 100 charge−discharge cycles by matching experimental and simulated cepstra derived from scanning nanobeam electron diffraction. While the LiCoO2 bulk remained a layered structure, spinel- and rocksalt-type phases were observed within 3 nm of the cathode−electrolyte interface. The developed method achieved a spatial resolution of 1.5 nm across a field of view of several hundred nanometers with minimal electron beam damage. The cepstral matching analysis offers valuable insights into the interfacial phase transitions and will aid in the design of high-performance lithium-ion batteries.

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• In Copyright
  

  This document is the Accepted Manuscript version of a Published Work that appeared in final form in Nano Letters, copyright © 2025 American Chemical Society after peer review and technical editing by the publisher. To access the final edited and published work see https://doi.org/10.1021/acs.nanolett.5c03692.

Keyword: All-solid-state batteries, TEM, Nanobeam electron diffraction, Cepstra

Date published: 2025-11-05

Publisher: American Chemical Society (ACS)

Journal:

• Nano Letters (ISSN: 15306984) vol. 25 issue. 44 p. 15840-15847

Funding:

• Asahi Glass Foundation
• Shibuya Science Culture and Sports Foundation
• Japan Society for the Promotion of Science JP22K14473
• Japan Society for the Promotion of Science JP24H00042
• Japan Society for the Promotion of Science JP25K18108
• Japan Science and Technology Agency JPMJGX23S5
• Japan Science and Technology Agency JPMJGX23S6
• Advanced Low Carbon Technology Research and Development Program
• Research Foundation for the Electrotechnology of Chubu
• National Institute for Materials Science
• Mitani Foundation for Research and Development
• Japan Advanced Institute of Science and Technology
• Iketani Science and Technology Foundation

Manuscript type: Author's version (Accepted manuscript)

MDR DOI: https://doi.org/10.48505/nims.6005

First published URL: https://doi.org/10.1021/acs.nanolett.5c03692

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Updated at: 2026-04-30 12:01:11 +0900

Published on MDR: 2026-10-23 02:59:57 +0900