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首页> 外文期刊>Journal of synchrotron radiation >Design and development of a controlled pressure/temperature set-up for in situ studies of solid-gas processes and reactions in a synchrotron X-ray powder diffraction station
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Design and development of a controlled pressure/temperature set-up for in situ studies of solid-gas processes and reactions in a synchrotron X-ray powder diffraction station

机译：设计和开发可控压力/温度装置，用于在同步加速器X射线粉末衍射站中对固体气体过程和反应进行原位研究

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摘要

A novel set-up has been designed and used for synchrotron radiation X-ray high-resolution powder diffraction (SR-HRPD) in transmission geometry (spinning capillary) for in situ solid-gas reactions and processes in an isobaric and isothermal environment. The pressure and temperature of the sample are controlled from 10(-3) to 1000 mbar and from 80 to 1000 K, respectively. To test the capacities of this novel experimental set-up, structure deformation in the porous material zeolitic imidazole framework (ZIF-8) by gas adsorption at cryogenic temperature has been studied under isothermal and isobaric conditions. Direct structure deformations by the adsorption of Ar and N-2 gases have been observed in situ, demonstrating that this set-up is perfectly suitable for direct structural analysis under in operando conditions. The presented results prove the feasibility of this novel experimental station for the characterization in real time of solid-gas reactions and other solid-gas processes by SR-HRPD.
机译：设计了一种新颖的装置并将其用于透射几何学（纺丝毛细管）中的同步辐射X射线高分辨率粉末衍射（SR-HRPD），用于在等压和等温环境中进行原位固体气体反应和过程。样品的压力和温度分别控制在10（-3）至1000 mbar和80至1000K。为了测试这种新型实验装置的能力，在等温和等压条件下，研究了低温条件下气体吸附在多孔材料沸石咪唑骨架（ZIF-8）中的结构变形。现场观察到由于Ar和N-2气体的吸附而导致的直接结构变形，这表明该装置非常适合在操作条件下进行直接结构分析。所提出的结果证明了该新型实验站通过SR-HRPD实时表征固体气体反应和其他固体气体过程的可行性。

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