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Development and Research of Inert-Gas/Vacuum Sealing Air-Free In-Situ Transfer Module of X-Ray Photoelectron Spectroscopy
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摘要: 针对空气敏感材料的表面分析，为了获得更加真实的表面组成与结构信息，需要提供一个可以保护样品从制备完成到分析表征过程中不接触大气环境的装置. 通过使用O圈密封和单向密封柱，提出一种简便且有效的设计概念，自主研制了正负压一体式无空气X射线光电子能谱（XPS）原位转移仓，用于空气敏感材料的XPS测试，利用单向密封柱实现不同工作需求下正负压两种模式的任意切换. 通过对空气敏感的金属Li片和CuCl粉末进行XPS分析表明，采用XPS原位转移仓正压和负压模式均可有效避免样品表面接触空气，保证测试结果准确可靠，而且采用正压密封方式转移样品可以提供更长的密封时效性. 研制的原位转移仓具有设计小巧、操作简便、成本低、密封效果好的特点，适合给有需求的用户开放使用.Abstract: For the surface analysis of air sensitive materials, and from the sample preparation to characterization, it is necessary to provide a device that can protect samples from exposing to the atmosphere environment so as to obtain accurate and impactful data of the surface chemistry. Through the use of O-ring and one-way sealing, a simple and effective design concept has been demonstrated, and an inert-gas/vacuum sealing air-free X-ray photoelectron spectroscopic (XPS) in-situ transfer module has been developed to realize the XPS analysis of air sensitive materials. The design of one-way sealing was achieved conveniently by switching between inert-gas and vacuum sealing modes in face of different working requirements. The XPS analysis of air-sensitive metal Li sheets and CuCl powders showed that both the sealing modes (an inert-gas/vacuum sealing) of the XPS in-situ transfer module can effectively avoid air contact on the sample surface, and consequently, can ensure the accuracy and reliability of XPS data. Furthmore, the inert gas sealing mode can keep the sample air-free for a longer time. The homemade XPS in-situ transfer module in this work is characterized by a compact design, convenient operation, low cost and effective sealing, which is suitable for the open access to the users who need it.
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图 1 正负压一体式无空气XPS原位转移仓系统装置
（a）样品台，（b）密封罩，（c）紧固挡板，（d）整体装配实物图，（e）整体装置分解示意图，（f）样品台与密封罩在进样室内对接完成，（g）样品台与密封罩在进样室内分离
Figure 1. System device of inert-gas/vacuum sealing air-free XPS in-situ transfer module
图 3 金属Li片通过两种（标准和负压密封）方式转移并在空气中放置不同时间的（a）Li 1s和（b）C 1s高分辨谱图
Figure 3. High-resolution spectra of (a) Li 1s and (b) C 1s of Li sheet samples transferred by two methods (standard and vacuum sealings) and placed in air for different times
图 4 金属Li片通过两种（标准和正压密封）方式转移并在空气中放置不同时间的Li 1s高分辨谱图
Figure 4. High-resolution spectra of Li 1s on Li sheet samples transferred by two methods (standard and inert gas sealings) and placed in air for different times
图 5 CuCl粉末通过两种（标准和负压密封）方式转移并在空气中放置不同时间的Cu 2p高分辨谱图
Figure 5. High-resolution spectra of Cu 2p on CuCl powder samples transferred by two methods (standard and vacuum sealings) and placed in air for different times
表 1 通过两种（标准和负压密封）方式转移并在空气中放置不同时间的Li 1s的半峰宽
Table 1. Full width at half maxima (FWHM) of Li 1s transferred by two methods (standard and vacuum sealings) and placed in air for different times
样品说明 进样方式 半峰宽/eV 密封放置0 h XPS原位转移仓负压
密封模式转移1.38 密封放置2 h 同上 1.39 密封放置4 h 同上 1.36 密封放置8 h 同上 1.32 密封放置18 h 同上 1.32 密封放置24 h 同上 1.62 暴露15 s 标准样品台进样
（封口袋密封）1.62 
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表 2 通过两种（标准和正压密封）方式转移并在空气中放置不同时间的Li 1s的半峰宽
Table 2. FWHM of Li 1s transferred by two methods (standard and inert gas sealings) and placed in air for different times
样品说明 进样方式 半峰宽/eV 密封放置0 h XPS原位转移仓正压
密封模式转移1.42 密封放置2 h 同上 1.35 密封放置4 h 同上 1.35 密封放置8 h 同上 1.34 密封放置18 h 同上 1.38 密封放置24 h 同上 1.39 密封放置48 h 同上 1.42 密封放置72 h 同上 1.38 暴露15 s 标准样品台进样
（封口袋密封）1.62
下载: 导出CSV
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