Simultaneous neutron powder diffraction and microwave characterisation at elevated temperatures.
Simultaneous neutron powder diffraction and microwave characterisation at elevated temperatures.
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在高温下同时进行中子粉末衍射和微波表征。
DOI：
10.1039/d1cp03658k
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发表时间：
2021
期刊：
影响因子：
--
通讯作者：
Barter M
中科院分区：
文献类型：
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作者：
Barter M
同时使用中子粉末衍射（NPD）和微波表征可以提供更多的信息，而不是单独使用任何一种技术;例如，它可以区分物理吸附和金属配位的物种。使用这些组合技术的许多可能的实验可以受益于添加用于样品加热的热源，例如溶剂去除或化学和催化反应的实时测量。本文记录了在高温下同时进行NPD和2.5 GHz微波腔共振技术的设备设计，并证实了该设备在150 °C下成功地对金属有机框架（MOF）样品进行去溶剂化。高灵敏度的微波表征的损耗和极性材料的水平比那些可以检测到使用晶体学技术低得多。
The use of simultaneous neutron powder diffraction (NPD) and microwave characterisation can provide more information than the use of either technique individually; for example, it enables the differentiation of physisorbed and metal-coordinated species. Many possible experiments using these combined techniques can benefit from the addition of a heat source for sample heating, such as real-time measurements of solvent removal, or chemical and catalytic reactions. This paper documents the design of equipment to conduct simultaneous NPD and 2.5 GHz microwave cavity resonance techniques at elevated temperatures and confirms the use of this equipment for successful desolvation of a metal–organic framework (MOF) sample at 150 °C. The high sensitivity of microwave characterisation of lossy and polar materials is demonstrated at levels much lower than those that can be detected using crystallographic techniques.