准原位转移仓辅助空气敏感样品的X射线光电子能谱测试  

XPS test of air-sensitive samples assisted by quasi-insitu transfer cabin

作　　者：陈睿 章小余[2] 袁震[2] 陈铁红 李国然 CHEN Rui;ZHANG Xiaoyu;YUAN Zhen;CHEN Tiehong;LI Guoran(School of Materials Science and Engineering,Nankai University,Tianjin 300050,China;Institute of Chemistry,Chinese Academy of Sciences,Beijing 100190,China)

机构地区：[1]南开大学材料科学与工程学院,天津300350 [2]中国科学院化学研究所,北京100190

出　　处：《实验技术与管理》2021年第11期110-114,共5页Experimental Technology and Management

基　　金：国家重点研发计划新能源汽车专项(2016YFB0100200);南开大学2021年自制实验教学仪器设备项目(21NKZZYQ08)。

摘　　要：空气敏感样品的X射线光电子能谱(XPS)测试在样品制备过程中需要高纯度惰性气体保护,一般是使用高纯惰气保护的塑封袋密封,待仪器舱门打开后,迅速将待测样品从塑封袋中拿出,放入仪器进行测试。然而这种转移方式仍然无法完全避免样品接触空气。该文针对以上问题,以对空气活泼的金属锂电极为研究对象,自主设计了准原位转移仓。经与塑封转移方式对照,发现在XPS测试中,准原位微型转移仓可以对空气敏感样品起到很好的隔离保护作用,得到更真实、更科学的材料表面组分和价态信息,有助于对空气敏感材料中各个组分化学态的合理归属。X-ray photoelectron spectroscopy(XPS) measurement of air-sensitive samples requires high purity inert gas protection during the sample preparation process. The sample is usually sealed in a plastic bag filled with inert gas and placed into the preparation chamber from the plastic bag for test as soon as the door of preparation chamber is opened. However, this transfer method still can not completely prevent the sample from contacting air.In this paper, a home-made quasi-insitu-cabin transfer is used to protect the air active metal lithium electrode as the typical air-sensitive representative samples, and then transfer the samples to XPS instrument without exposure to the air. Compared with the normal plastic packaging transfer process, an effective protection is achieved when the home-made transfer cabin is employed. In this way, more scientific and reliable information of surface composition and valence state of the air-sensitive sample can be obtained,and more reasonable assignment of the chemical state of each component can be inferred.

关 键 词：锂电极 空气敏感 表面分析 准原位转移仓 X射线光电子能谱 

分 类 号：O647[理学—物理化学]