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Accelerated microwave-assisted synthesis and in situ X-ray scattering of tungsten-substituted vanadium dioxide (V1−xWxO2)
Journal of Materials Research ( IF 2.7 ) Pub Date : 2020-09-23 , DOI: 10.1557/jmr.2020.250
Catrina E. Wilson , Amanda E. Gibson , Joshua J. Argo , Patricia A. Loughney , Wenqian Xu , Graham King , Vicky Doan-Nguyen

Vanadium dioxide (VO2) has been widely studied due to its metal-insulator phase transition at 68 °C, below which it is a semiconducting monoclinic phase, P21/c, and above it is a metallic tetragonal phase, P42/mnm. Substituting vanadium with transition metals allows transition temperature tunability. An accelerated microwave-assisted synthesis for VO2 and 5d tungsten-substituted VO2 presented herein decreased synthesis time by three orders of magnitude while maintaining phase purity, particle size, and transition character. Tungsten substitution amount was determined using inductively coupled plasma-optical emission spectroscopy. Differential scanning calorimetry, superconducting quantum interference device measurements, and in situ heating and cooling experiments monitored through synchrotron X-ray diffraction (XRD) confirmed the transition temperature decreased with increased tungsten substitution. Scanning electron microscopy analyzed through the line-intercept method produced an average particle size of 3–5 μm. Average structure and local structure phase purity was determined through the Rietveld analysis of synchrotron XRD and the least-squares refinement of pair distribution function data.



中文翻译:

钨取代的二氧化钒(V 1- x W x O 2)的微波辅助加速合成和原位X射线散射

由于二氧化钒(VO 2)在68°C时具有金属-绝缘体相变,因此得到了广泛的研究,在其以下是半导体单斜晶相P2 1 / c,在其上方是金属四方相P4 2 / mnm。用过渡金属代替钒可实现过渡温度可调性。VO 25d钨取代的VO 2的加速微波辅助合成本文所述的化合物将合成时间减少了三个数量级,同时保持了相纯度,粒度和过渡特性。使用电感耦合等离子体发射光谱法确定钨取代量。差示扫描量热法,超导量子干涉仪测量以及原位通过同步加速器X射线衍射(XRD)进行的加热和冷却实验证实,过渡温度随着钨取代量的增加而降低。通过线截距法分析的扫描电子显微镜得出的平均粒径为3–5μm。通过同步加速器XRD的Rietveld分析和对分布函数数据的最小二乘优化确定平均结构和局部结构相的纯度。

更新日期:2020-09-23
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