A bias application system for tracking electrochemical reactions by x-ray photoelectron spectroscopy (XPS) is constructed using a laboratory-based apparatus. A specialized sample holder and stage with three electrical terminals provide contacts to a potentio-galvanostat on the outside, allowing bias application to an electrochemical device in the analysis chamber under vacuum conditions. The application of a direct current bias voltage to the sample holder is confirmed using metal Au samples. The Au 4f peaks from the Au grounded to the analyzer are identical, while those from the Au insulated from the analyzer shift due to the applied bias voltage. Furthermore, galvanostatic lithiation/delithiation processes and in situ XPS measurements are performed on a Si thin-film electrode after transferring the sample into the XPS apparatus without exposure to open air using a newly developed transfer vessel. After the initial lithiation process, a Li 1s peak containing a lithium-silicide component appears, and the Si 2p peaks shift to a lower binding energy due to the lithiation of the Si electrode. After the subsequent delithiation process, the Si 2p peak from the lithium silicide partially shifts back to a higher binding energy. As a result, in situ XPS measurements of the lithiation/delithiation reactions are successfully performed using the developed system.

使用基于实验室的设备构建用于通过X射线光电子能谱（XPS）跟踪电化学反应的偏压施加系统。带有三个电端子的专用样品架和载物台可提供与外部恒电位仪的接触，从而允许在真空条件下将偏压施加到分析室中的电化学装置上。使用金属金样品，可以确认在样品架上施加了直流偏置电压。从Au接地到分析仪的Au 4f峰是相同的，而与Au绝缘的Au 4f峰则由于施加的偏置电压而发生偏移。此外，恒电流锂化/去锂化过程和原位在使用新开发的转移容器将样品转移到XPS设备中而不暴露于空气之后，在Si薄膜电极上执行XPS测量。在最初的锂化过程之后，出现了包含锂硅化物成分的Li 1s峰，并且由于Si电极的锂化，Si 2p峰移向了较低的结合能。在随后的脱锂过程之后，来自硅化锂的Si 2p峰部分移回更高的结合能。结果，使用所开发的系统成功地进行了锂化/脱锂反应的原位XPS测量。