微波辅热-甲醇还原法制备M相二氧化钒粉体  

Preparation of M-phase vanadium dioxide powder by microwave assisted thermal reduction of methanol

作　　者：陈益超[1,2] 颜文斌 石爱华[1,3] 易静 CHEN Yichao;YAN Wenbin;SHI Aihua;YI Jing(College of Chemistry and Chemical Engineering,Jishou University,Jishou 416000,China;Manganese and Zinc Product Quality Supervision and Inspection Center of Hunan Province,Jishou 416000,China;Key Laboratory of Mineral Cleaner Production and Green Functional Materials in Hunan Province,Jishou 416000,China)

机构地区：[1]吉首大学化学化工学院,湖南吉首416000 [2]湖南省锰锌产品质量监督检验中心,湖南吉首416000 [3]矿物清洁生产与绿色功能材料开发湖南省重点实验室,湖南吉首416000

出　　处：《材料科学与工艺》2019年第3期41-46,共6页Materials Science and Technology

基　　金：国家自然科学基金资助项目(21566010);吉首大学研究生项目(14JDY051);湖南省高校科技创新团队支持计划资助

摘　　要：为获得具有良好相变特性的M相VO2粉体,本文以V2O5为原料、甲醇作还原剂,采用微波辅热制备M相VO2粉体.探讨了微波辅热功率、填充度、反应温度、反应时间、甲醇用量因素对制备VO2的影响,采用X射线衍射(XRD)、差示扫描量热法(DSC)和扫描电子显微镜(SEM),对产物进行了物相、相变和形貌特征的表征.结果表明:在微波辅热功率为1000kW,填充度为0.7,反应温度为250℃时,反应时间为60min,V2O5质量与甲醇体积比为5∶3时,得到B相的VO2粉体;B相的VO2再经过800℃高温热处理后完全转化为具有相变功能的M相,M相VO2粉体纯度为99.20%,产率为92.30%,相变点温度为68.6℃,晶体形貌呈现较匀称的棒状结构,长度为1~2μm.By adopting microwave assisted heating, we used vanadium pentoxide as raw material and methanol as reducing agent to prepare M-phase vanadium dioxide powder with good phase transformation characteristics. Effects of microwave heating power, fullness, reaction temperature, reaction time, and methanol dosage on the preparation of vanadium dioxide powder were discussed. The phase, phase transition, and morphology of vanadium oxides were characterized by XRD, DSC, and SEM. Results show that the powder was B phase vanadium dioxide when the microwave heating power was 1 000 kW, fullness was 0.7, reaction temperature was 250 ℃, reaction time was 60 min, and the mass/volume ratio of vanadium pentoxide to methanol was 5∶3. In addition, the obtained B phase transferred to M-phase after the heat treatment at 800 K. The purity of the M-phase vanadium dioxide was 99.20%, yield was 92.30%, and the phase transformation point was 68.6 ℃. The crystal morphology showed a more symmetrical rod-shaped structure, whose length was about 1~2 μm.

关 键 词：微波辅热 甲醇还原法 制备 二氧化钒 粉体 

分 类 号：TB34[一般工业技术—材料科学与工程]