高等学校化学学报

高等学校化学学报 ›› 2003, Vol. 24 ›› Issue (5): 761.

• 论文 • 上一篇    下一篇

不同整比性VO2纳米粉体的合成

何山1, 林晨2, 雷德铭1, 郑臣谋2   

  1. 1. 中山大学物理系, 广州 510275;
    2. 中山大学化学系, 广州 510275
  • 收稿日期:2002-07-24 出版日期:2003-05-24 发布日期:2003-05-24
  • 通讯作者: 郑臣谋(1946年出生),男,副教授,从事无机功能材料研究.E-mail:cedc46@zsu.edu.cn E-mail:cedc46@zsu.edu.cn
  • 基金资助:

    国家自然科学基金(批准号:59972045);广州市科技局基金(批准号:2002J1-C0371)

Synthesis of Various Stoichiometry Nano-powder of VO2

HE Shan1, LIN Chen2, LEI De-Ming1, ZHENG Chen-Mou2   

  1. 1. Department of Physics., Guangzhou 510275, China;
    2. Department of Chemistry, SUN Yat-Sen University, Guangzhou 510275, China
  • Received:2002-07-24 Online:2003-05-24 Published:2003-05-24

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摘要： 以V2O5,HCl,N2H4·2HCl和NH4HCO3为原料合成了紫红色多晶(NH4)5[(VO)6(CO3)4(OH)9]·10H2O(I),产率80％～95％.在N2气流中对前体I进行了TG/DTG和DTA热分析.研究了前体I在N2-空气气流中热解时氧分压(po2)和反应温度对产物VO2整比性的影响.结果表明,在500℃条件下,VOx中的x值与po2呈正比关系,在po2=30.3Pa条件下,在450～520℃区间,产物为缺氧VO2;在t<450℃和t>520℃时,产物为富氧VO2.在合适的条件下,成功地合成了从VO1.927到VO2.080之间不同整比性的VO2粉体.产物组成均匀,其XRD谱未观察到非VO2的杂质峰.VO2粉体颗粒的平均粒径为20nm,粒度分布均匀并呈球形.

关键词: 二氧化钒, 纳米粉体, 整比性, 前体制备路线

Abstract: The violet polycrystalline (NH4)5[(VO)6(CO2)4(OH)9]·10H2O(Ⅰ) was synthesized by using V2O5, HCl, N2H4·2HCl and NH4HCO3as the starting materials. The yield was 80%-95%. The TG/DTG and DTA of Iwere studied in a flow of N2. The effects of partial pressure of oxygen(po2) in N2-air flow and temperature of reaction on VO2stoichiometry were investigated in the pyrolysis of Ⅰ in a silica tube. The results show that x value of VOxis proportional to po2at pyrolysis temperature of 500 ℃ At po2= 30.3 Pa and in the temperature range from 450 to 520 ℃ the products are oxygen-deficient VO2, and when the temperature is lower than 450℃ or higher than 520℃ the products are oxygen-rich VO2In this paper, various stoichiometry VO2powders from VO1.927to VO2.080were successfully synthesized by pyrolysizing the precursor. XRD patterns of VO2show that none of the impurity peaks was observed. The SEM micrograph of sample indicates that as-prepared VO2is spherical particles with mean size 20 nm and is homogeneous in distribution. Further experiments testify that the composition of nano-powders is homogeneous.

Key words: Vanadium dioxide, Nano-powder, Stoichiometry, Preparative route of the precursor

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