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High-resolution real-space mapping of Li-ion diffusion in the LiNi(1/3)Co(1/3)Mn(1/3)O₂ cathode within an all-solid-state thin film Li-ion battery has been conducted using advanced scanning probe microscopy techniques, namely, band excitation electrochemical strain microscopy (BE-ESM) and conductive atomic force microscopy. In addition, local variations of the electrochemical response in the LiNi(1/3)Co(1/3)Mn(1/3)O₂ thin film cathode at different cycling stages have been investigated. This work demonstrates the unique feature and applications of the BE-ESM technique on battery research. The results allow us to establish a direct relationship of the changes in ionic mobility as well as the electrochemical activity at the nanoscale with the numbers of charge/discharge cycles. Furthermore, various factors influencing the BE-ESM measurements, including sample mechanical properties (e.g., elastic and dissipative properties) as well as surface electrical properties, have also been studied to investigate the coupling effects on the electrochemical strain. The study on the relationships between the Li-ion redistribution and microstructure of the electrode materials within thin film Li-ion battery will provide further understanding of the electrochemical degradation mechanisms of Li-ion rechargeable batteries at the nanoscale.

This paper presents in situ characterization of lithium-ion diffusion at nano- to micro-meter scales in a Li-rich layered oxide thin film cathode under external bias by using Electrochemical Strain Microscopy (ESM) and Atomic Force Microscopy (AFM) techniques. The local variations of the diffusion coefficient are calculated and visualized from the ESM images. The results indicate that the Li-ion movement is closely correlated with the changes in the surface topography when the Li-rich cathode is subjected to an external bias. Furthermore, bias-induced Li-ion redistribution is partially reversible. Topography evolution due to Li-ion diffusion and relaxation behaviour are observed. The results from this in situ study provide the insight into the Li-ion diffusion mechanism in the cathode material and pave the way for studying the details of the diffusion-related phenomenon in Li-ion battery materials.

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