McFadzean Ross George Bell, Smith Ronald, Drysdale Timothy David, Gregory Duncan H
Chemistry, University of Glasgow, Glasgow, UK.
ISIS Pulsed Neutron and Muon Source, Didcot, Oxfordshire, UK.
Philos Trans A Math Phys Eng Sci. 2025 May 22;383(2297):20240065. doi: 10.1098/rsta.2024.0065.
Utilizing direct microwave- (MW)-induced heating in solid-state synthesis yields the clear benefits of greatly reduced reaction times and lower energy requirements as compared with conventional methods. Here, we describe a bespoke single-mode cavity (SMC) MW reactor designed to operate within a neutron beamline that allowed powder diffraction data to be collected from materials as they were heated using MWs. The unique set-up was used to investigate the rapid solid-state synthesis of the binary metal chalcogenide thermoelectric (TE) materials BiSe, BiTe, SbSe and SbTe. The resultant time-resolved diffraction data from each synthesis were time-sliced post-reaction into segments covering periods of tens of seconds, enabling the reaction progression to be visualized as colourmap plots. This technique enabled the accurate tracking of polycrystalline structure formation and a quantitative analysis of phase fractions during the accelerated heating and subsequent cooling stages of each reaction. Our investigations have also revealed some of the present limitations of rapid neutron diffraction techniques and how these might be remedied.This article is part of the discussion meeting issue 'Microwave science in sustainability'.
与传统方法相比，在固态合成中利用直接微波（MW）诱导加热具有显著优势，即反应时间大幅缩短且能量需求降低。在此，我们描述了一种定制的单模腔（SMC）微波反应器，其设计用于在中子束线内运行，使得能够在材料通过微波加热时收集粉末衍射数据。这种独特的装置被用于研究二元金属硫族化物热电（TE）材料BiSe、BiTe、SbSe和SbTe的快速固态合成。每次合成得到的时间分辨衍射数据在反应后被按时间切片成覆盖数十秒时间段的片段，从而能够将反应进程可视化为彩色图。该技术能够在每个反应的加速加热和随后的冷却阶段准确跟踪多晶结构的形成并对相分数进行定量分析。我们的研究还揭示了快速中子衍射技术目前存在的一些局限性以及如何加以弥补。本文是“可持续性中的微波科学”讨论会议文集的一部分。
