[Analysis Case] Atmospheric Non-Exposure XPS Analysis of Lithium-Ion Battery Anodes

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last updated：Apr 20, 2024

カネカテクノリサーチ本社、東京営業所、名古屋営業所、大阪分析センター、高砂分析センター

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This study analyzes cases where the chemical state of the anode surface changed when exposed to the atmosphere compared to when it was not exposed, using an anode extracted from a lithium-ion battery.

【Analysis Sample】 Graphite anode of a commercially available lithium-ion battery used in electronic devices (discharged state) 【Analysis Equipment】 Glove box (purge type, manufactured by Miwa Seisakusho) XPS; monochromatic Al Kα radiation (ULVAC-PHI, PHI5000 VersaProbe II) 【Analysis Procedure】 Inside the glove box (Ar atmosphere), a cylindrical 18650 lithium-ion battery was disassembled to collect the anode. The collected anode was transported from the glove box to the XPS equipment (vacuum) via a transfer vessel, which was designated as the non-atmosphere exposed anode. In contrast, the anode that was temporarily taken out of the glove box (into the atmosphere) before being transported to the XPS equipment was designated as the atmosphere exposed anode, and XPS analysis was conducted on both.

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**Analysis Results** The C1s spectra of the atmosphere-exposed and non-exposed negative electrodes are shown. It is generally known that repeated charge and discharge cycles lead to the formation of a Solid Electrolyte Interphase (SEI) on the electrode surface, and both spectra reflect the state of the SEI, showing contributions from organic materials and lithium salts. The two spectra do not match; the spectrum of the atmosphere-exposed negative electrode shows a lower proportion of graphite and a higher proportion of components like O-C=O compared to the non-exposed electrode. This suggests that the SEI on the surface of the atmosphere-exposed negative electrode has reacted with atmospheric components and undergone changes due to exposure. **Summary** Using a non-exposed transport mechanism, it is possible to analyze samples that react with atmospheric components without altering them.