VO2(B)热转化为VO2(R)和V2O3的高温XRD原位表征  

In Situ Characterization on Thermal Transitions of VO_2（B）：Toward VO_2（R） and V_2O_3

作　　者：张少鸿 付娟 苏秋成 吴梁鹏 李新军 

出　　处：《稀有金属材料与工程》2016年第6期1374-1380,共7页Rare Metal Materials and Engineering

基　　金：National Natural Science Foundation of China(51172233);the Development of Instrument&Equipment Function and Technical Innovation Project of CAS and the Analytical&Testing Fund of Guangzhou Area,China(201212)

摘　　要：以草酸和V_2O_5为原料,采用水热法制备VO_2（B）。通过高温原位X射线衍射技术研究VO_2（B）在氮气保护下升高温度过程中的相变特性,采用X射线衍射仪（XRD）、场发射扫描电子显微镜（FE-SEM）和激光拉曼光谱技术分析所制备样品及其在不同温度热相变产物的微观形貌、晶体结构和物相组成。结果表明：以草酸和V_2O_5为原料,用水热法可制得单斜晶系VO_2（B）,颗粒呈纳米片状;升温至430-700℃之间,VO_2（B）不可逆转化为四方晶系VO_2（R）,形貌由纳米片状变为亚微米及微米近球形;升温至1000℃左右,VO_2（R）开始分解形成Magnéli相系列化合物（V_nO_（2n-1）,3≤n≤9）;升温至约1200℃完全转变为具有刚玉结构的V_2O_3烧结块。VO_2（B） was synthesized via a facile hydrothermal process using V_2O_5 and oxalic acid. The crystal structure and the phase transition of VO_2（B） during elevated temperatures in N_2 were investigated by in situ X-ray diffraction（XRD）. Meanwhile, the morphologies and the crystal structures of the samples obtained by annealing at different temperatures were characterized by Field emission scanning electron microscopy（FE-SEM）, XRD and Raman spectroscopy, respectively. The results show that the as-synthesized nano platelet-like monoclinic VO_2（B） irreversibly transforms into submicron and micron subsphaeroidal tetragonal VO_2（R） between 430 and 700℃. The as-obtained VO_2（R） starts to decompose and form Magnéli phases V_nO_（2n-1）（3≤n≤9） series compounds at -1000 ℃, and totally transfers into a corundum V_2O_3 sintered block at ca. 1200 ℃.

关 键 词：水热法 氧化钒 原位XRD 热相变 拉曼光谱 

分 类 号：O643.36[理学—物理化学]