A gas‐ and vapour‐pressure control system synchronized with the continuous data acquisition of millisecond high‐resolution powder diffraction measurements was developed to study structural change processes in gas storage and reaction materials such as metal organic framework compounds, zeolite and layered double hydroxide. The apparatus, which can be set up on beamline BL02B2 at SPring‐8, mainly comprises a pressure control system of gases and vapour, a gas cell for a capillary sample, and six one‐dimensional solid‐state (MYTHEN) detectors. The pressure control system can be remotely controlled via developed software connected to a diffraction measurement system and can be operated in the closed gas and vapour line system. By using the temperature‐control system on the sample, high‐resolution powder diffraction data can be obtained under gas and vapour pressures ranging from 1 Pa to 130 kPa in temperatures ranging from 30 to 1473 K. This system enables one to perform automatic and high‐throughput in situ X‐ray powder diffraction experiments even at extremely low pressures. Furthermore, this developed system is useful for studying crystal structures during the adsorption/desorption processes, as acquired by millisecond and continuous powder diffraction measurements. The acquisition of diffraction data can be synchronized with the control of the pressure with a high frame rate of up to 100 Hz. In situ and time‐resolved powder diffraction measurements are demonstrated for nanoporous Cu coordination polymer in various gas and vapour atmospheres.

中文翻译：

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同步加速器粉末衍射的快速连续测量与控制 SPring-8 光束线 BL02B2 处的气体和蒸汽压力同步。

开发了一种与毫秒高分辨率粉末衍射测量的连续数据采集同步的气体和蒸气压控制系统，用于研究气体储存和反应材料（例如金属有机骨架化合物、沸石和层状双氢氧化物）的结构变化过程。该装置可安装在 SPring-8 的光束线 BL02B2 上，主要包括气体和蒸汽压力控制系统、毛细管样品气室和六个一维固态（MYTHEN）探测器。压力控制系统可以通过连接到衍射测量系统的开发软件进行远程控制，并且可以在封闭的气体和蒸汽管线系统中操作。通过在样品上使用温度控制系统，可以在 1 Pa 至 130 kPa 的气体和蒸汽压力、30 至 1473 K 的温度范围内获得高分辨率粉末衍射数据。该系统使人们能够自动执行高精度粉末衍射数据。‐即使在极低压力下也可进行原位X射线粉末衍射实验。此外，该开发的系统可用于研究吸附/解吸过程中的晶体结构，如通过毫秒和连续粉末衍射测量获得的。衍射数据的采集可以与压力控制同步，帧速率高达 100 Hz。演示了纳米多孔铜配位聚合物在各种气体和蒸汽气氛中的原位和时间分辨粉末衍射测量。