气固反应的同步辐射X射线衍射原位表征装置研制  

Gas-solid reaction devices for in situ synchrotron X-ray diffraction characterization

作　　者：周靖添 陶亚军 罗震林[1] ZHOU Jingtian;TAO Yajun;LUO Zhenlin(National Synchrotron Radiation Laboratory,University of Science and Technology of China,Hefei 230026,China)

机构地区：[1]中国科学技术大学国家同步辐射实验室,合肥230026

出　　处：《核技术》2022年第3期13-20,共8页Nuclear Techniques

基　　金：国家自然科学基金(No.12175235)资助。

摘　　要：腐蚀性气体参与的气固反应,其同步辐射原位X射线衍射(X-ray Diffraction,XRD)表征需要使用防腐蚀和泄露的装置。为此研发了两种用于气固反应XRD表征的原位装置,分别通过液体挥发和固体热处理来产生反应气体,具有装置结构紧凑、可拆卸和重复利用等优点,解决了特定气固反应原位XRD表征的需求。其中,基于液体挥发产生反应气体的原位装置适用于室温近常压气固反应,气体与固态样品发生反应可以通过精确控制液体的注入来控制反应的起始时间;基于固体热处理的原位反应装置主体采用石英材料制作,包括石英反应池和石英X窗等,适用于光子能量在18 keV以上的原位X射线衍射表征,工作温度可达450℃。这些实验装置有助于推动同步辐射技术在化学反应原位表征中的应用。[Background]Characterizing the microstructure evolution of materials during the gas-solid reaction is crucial for the comprehensive understanding of the reaction mechanism.In situ synchrotron X-ray diffraction(XRD)is a powerful tool for this purpose.For the reactions involving corrosive gases,unique devices need to be designed for the in situ experiments.[Purpose]The study aims to develop two kinds of in situ synchrotron XRD devices for characterizing gas-solid reaction.[Methods]Liquid volatilization and solid heat treatment were applied respectively to the generation of reaction gas for two kinds of in situ synchrotron XRD devices.The gas-solid reaction in liquid volatilization was triggered and precisely controlled by injecting liquid into the cell,suitable for gas-solid reaction at room temperature and near atmospheric pressure.For in situ XRD characterization device with reaction gas generated by heat treatment of solid,both the cell and the X-ray window were made of quartz glass,hence suitable for the gassolid reaction temperature up to 450℃and X-ray photon energy above 18 keV.[Results&Conclusions]The two in situ devices have the advantages of compact,disassemble and reusable.These devices help to facilitate the application of synchrotron experimental techniques for in situ characterization of chemical reaction processes.

关 键 词：同步辐射 X射线衍射 原位装置 气固反应 

分 类 号：TL99[核科学技术—核技术及应用]