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固态电解质界面的X射线光电子能谱(XPS)测试方法

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固态电解质界面(SEI)对二次电池的性能至关重要,其成分及化学态通常使用X射线光电子能谱(XPS)来测定.然而,由于SEI组成复杂且稳定性差,其化学态极易受到外界条件的影响,带来错误的电池机理解释,这对XPS测试方法提出了更高要求,常规XPS测试获得的SEI成分信息的真实性、准确性值得探究.此外,由于离子溅射时存在择优溅射,XPS深度剖析测试时SEI是否存在组分还原的情况仍未可知.以锂金属电池的SEI为例,结合实际测试情况,详细研究测试位置、X射线、真空静置时间以及溅射条件对谱图的影响.结果表明,不同测试位置获得的SEI组成不同,真空静置时SEI也不稳定,成分发生变化,离子溅射导致SEI成分发生分解,而SEI在X射线辐照下可以保持稳定.基于此,建立了适用于锂金属电池中SEI组分研究的XPS测试方法,并为其他二次电池体系中的界面研究提供参考与借鉴.
Study on X-ray Photoelectron Spectroscopy Testing Method of Solid Electrolyte Interphase
The solid electrolyte interphase(SEI)is crucial to the performance of secondary batteries.The composition and chemical state of SEI are usually determined using X-ray photoelectron spectroscopy(XPS).However,due to the complex composition and poor stability of SEI,its chemical state is highly susceptible to external conditions,leading to incorrect interpretations of battery mechanisms.This poses higher demands on the XPS testing method,and the authenticity of the SEI composition obtained by XPS tests are worth exploring.Moreover,during in-depth analysis,preferential sputtering can easily occur.It remains unknown whether the SEI composition remains stable during the sputtering process.In this paper,taking the SEI of lithium metal batteries as an example,combined with the actual test conditions,the influence of test location,X-ray,vacuum standing time and sputtering conditions on the XPS spectra was studied in detail.The results showed that different test locations yielded different SEI compositions.And the composition of SEI changed under vacuum.The sputtering caused the decomposition of SEI components,but SEI could remain stable under X-ray irradiation.Based on this,an XPS testing method suitable for the study of SEI in lithium metal batteries was proposed.It provides references and insights for interface research in other secondary battery systems.

lithium-metal batteriessolid electrolyte interphaseX-ray photoelectron spectroscopychemical state

赵利媛、方岩、王珊珊、陈艳、宋廷鲁

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北京理工大学材料学院,北京 100081

北京理工大学分析测试中心,北京 102401

锂金属电池 固态电解质界面 X射线光电子能谱 化学态

2025

中国无机分析化学
北京矿冶研究总院

中国无机分析化学

北大核心
影响因子:1.306
ISSN:2095-1035
年,卷(期):2025.15(1)