Development of a Raman spectroscopy system for in situ monitoring of microwave‐assisted inorganic transformations
Development of a Raman spectroscopy system for in situ monitoring of microwave‐assisted inorganic transformations
复制标题
开发用于原位监测微波辅助无机转化的拉曼光谱系统
DOI：
10.1002/jrs.6478
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发表时间：
2022
影响因子：
2.5
通讯作者：
Birkel, Christina S.
中科院分区：
文献类型：
--
作者：
Jamboretz, John;Reitz, Andreas;Birkel, Christina S.
由于加热速率高、潜在的选择性加热以及时间/能量减少，微波加热方法在无机固体的制备中具有独特的优势。由于缺乏可用且易于应用的原位监测方法，特别是对于固态样品，对这些增强功能以及所涉及的机制的了解还很薄弱。现有的现场研究通常依赖于光束线设施以及定制的微波系统，这在最好的情况下是不方便的，在最坏的情况下是无法实现的。原位拉曼光谱是一种理想的技术，因为它通过非接触方法提供快速、明确的物相识别。此外，仪器部件简单紧凑，便于在典型的合成实验室中使用。关于在微波加热期间使用拉曼光谱进行原位测量的报告很少，而且它们都利用专门的定制反应器设置。在这项工作中，描述了一种新的拉曼测量系统，旨在观察原位无机转变，该系统可轻松部署在标准的商用实验室规模微波反应器中。作为一个简单的演示，在微波和传统炉加热下监测了 TiO2 中锐钛矿到金红石的相变。所实现的出色时间分辨率证明了该系统在理解微波辅助制备无机化合物的方法方面的实用性。这种简单性将鼓励非专业人士进行整合，以了解合成制剂的微波加热并促进该技术的更广泛应用。
Microwave heating methods offer unique advantages in preparations of inorganic solids due to the high heating rates, potentially selective heating, and time/energy reductions. Understanding of these enhancements as well as involved mechanisms is poor due to the lack of available and easily applicable in situ monitoring methods, particularly for samples in the solid state. Existing in situ studies typically rely on access to beamline facilities as well as custom‐built microwave systems, which is in the best case inconvenient and in the worst case not achievable. In situ Raman spectroscopy is an ideal technique as it provides rapid and unambiguous phase identification by a noncontact method. Further, the instrument components are simple and compact, facilitating use in the typical synthetic laboratory. Only a few reports on using Raman spectroscopy for in situ measurements during microwave heating exist, and they all utilize specialized custom reactor setups. In this work, a new Raman measurement system designed to observe inorganic transformations in situ that is readily deployable in a standard, commercially available laboratory scale microwave reactor is described. As a simple demonstration, the anatase‐to‐rutile phase transition in TiO2is monitored under both microwave and conventional furnace heating. The excellent time resolution achieved demonstrates the utility of the system in understanding microwave‐assisted methods for the preparation of inorganic compounds. The simplicity will encourage integration by the non‐specialist to understand microwave heating for synthetic preparations and promote wider application of the technique.