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溶胶-凝胶辅助水热法制备硼掺杂纳米VO2粉体
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深圳大学

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Synthesis of Boron-doped Monoclinic VO2 nanoparticles by sol-gel hydrothermal method
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Shenzhen University

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    摘要:

    采用溶胶-凝胶辅助水热法制备了硼掺杂纳米二氧化钒(VO2)粉体,探究了双氧水(H2O2)浓度、水热时间、退火温度、不同硼掺杂剂、硼掺杂量等工艺参数对合成硼掺杂纳米VO2(M)粉体的影响,并采用X-射线衍射仪(XRD)、X-射线光电子能谱分析仪(XPS)、电感耦合等离子体光谱仪(ICP)、场发射扫描电镜(SEM)、差示扫描量热仪(DSC)对硼掺杂纳米VO2粉体的结构、形貌和相变特性进行了表征。结果表明:H2O2浓度为15%,水热时间为72 h,退火温度为600 ℃,硼掺杂剂为硼酸、硼掺杂量≤10%为较优合成工艺条件;所制备出的硼掺杂纳米VO2粉体尺寸约为100 nm,形貌呈珊瑚状;硼原子成功替代了VO2(M)晶格中的钒原子,当实际掺杂量为0.6 at.%时,相变温度降低7.2 ℃。

    Abstract:

    Boron-doped vanadium dioxide (VO2) nanopowders were prepared by the sol-gel hydrothermal method. Effect of process parameters including the hydrogen peroxide (H2O2) concentration, hydrothermal time, annealing temperature, type of boron dopant and boron doping amount on the synthesis of boron-doped VO2 powders was investigated. The structure, morphology and phase transition properties of the boron-doped VO2 powders were characterized by the X-ray diffractometer (XRD), X-ray photoelectron spectroscopy (XPS), inductively coupled plasma (ICP), field emission scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). The results show that the superior synthesis process parameters are 15% for the H2O2 concentration, 72 h for the hydrothermal time, 600 °C for the annealing temperature, boric acid as the boron dopant, and less than 10 at.% for the boron doping amount. The obtained boron-doped VO2 powders have the size of around 100 nm with the morphology of coral-like structure. The boron atoms successfully replace the vanadium atoms in the VO2(M) lattice. The phase transition temperature is reduced by 7.2 °C, when the actual doping amount is 0.6 at.%.

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周俏婷,吕维忠.溶胶-凝胶辅助水热法制备硼掺杂纳米VO2粉体[J].稀有金属材料与工程,2020,49(4):1325~1330.[Qiaoting Zhou,,Weizhong Lv. Synthesis of Boron-doped Monoclinic VO2 nanoparticles by sol-gel hydrothermal method[J]. Rare Metal Materials and Engineering,2020,49(4):1325~1330.]
DOI:10.12442/j. issn.1002-185X. sg20190086

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  • 收稿日期:2019-05-20
  • 最后修改日期:2019-07-30
  • 录用日期:2019-10-14
  • 在线发布日期: 2020-05-07
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