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惰性气氛下热分解法制备M相二氧化钒超细颗粒

尹翔鹭 曾泽华 高荣荣 代宇 滕艾均

尹翔鹭, 曾泽华, 高荣荣, 代宇, 滕艾均. 惰性气氛下热分解法制备M相二氧化钒超细颗粒[J]. 钢铁钒钛, 2022, 43(1): 1-6. doi: 10.7513/j.issn.1004-7638.2022.01.001
引用本文: 尹翔鹭, 曾泽华, 高荣荣, 代宇, 滕艾均. 惰性气氛下热分解法制备M相二氧化钒超细颗粒[J]. 钢铁钒钛, 2022, 43(1): 1-6. doi: 10.7513/j.issn.1004-7638.2022.01.001
Yin Xianglu, Zeng Zehua, Gao Rongrong, Dai Yu, Teng Aijun. Thermolysis preparation of monoclinic phase vanadium dioxide with ultrafine particles under an inert gas atmosphere[J]. IRON STEEL VANADIUM TITANIUM, 2022, 43(1): 1-6. doi: 10.7513/j.issn.1004-7638.2022.01.001
Citation: Yin Xianglu, Zeng Zehua, Gao Rongrong, Dai Yu, Teng Aijun. Thermolysis preparation of monoclinic phase vanadium dioxide with ultrafine particles under an inert gas atmosphere[J]. IRON STEEL VANADIUM TITANIUM, 2022, 43(1): 1-6. doi: 10.7513/j.issn.1004-7638.2022.01.001

惰性气氛下热分解法制备M相二氧化钒超细颗粒

doi: 10.7513/j.issn.1004-7638.2022.01.001
详细信息
    作者简介:

    尹翔鹭(1990—),男,山东潍坊人,研究生,工程师,主要研究方向:纳米功能材料,E-mail:Xiangluyin@163.com

  • 中图分类号: TF841.3

Thermolysis preparation of monoclinic phase vanadium dioxide with ultrafine particles under an inert gas atmosphere

  • 摘要: M相二氧化钒(VO2)是一种主要的热致相变材料,相变温度为68 ℃。由于相变前后会发生明显的物理化学性质的变化,M相VO2可以广泛应用在相变节能和传感等领域。采用草酸氧钒作为前驱体,在惰性气氛中直接热分解制备M相VO2超细颗粒。探究了主要反应条件:热解温度、热解时间和气体流速对产物物相纯度的影响。在最优的制备条件(热解温度450 ℃,热解时间30 min,氩气流速2.0 L/min)下,制备了较纯的M相VO2超细颗粒。采用扫描电镜、差示热分析仪表征了产物的形貌和相变性能。制备的M相VO2颗粒主要为类长方体形的微米级颗粒,在其表面附着大量不规则形貌的纳米级细小颗粒,微米级颗粒平均尺寸为5.76 μm,纳米级颗粒平均尺寸为177.21 nm,相变温度为65 ℃。该方法简单高效、易于放大制备M相VO2超细颗粒。
  • 图  1  草酸氧钒的热重曲线

    Figure  1.  TG curve of vanadyl oxalate

    图  2  不同热分解时间下产物的XRD谱

    Figure  2.  XRD spectra of prepared samples in different pyrolysis time

    图  3  不同温度下热分解产物的XRD谱

    Figure  3.  XRD spectra of prepared samples in different pyrolysis temperature

    (a) 350 ℃;(b) 400 ℃;(c) 450 ℃;(d) 500 ℃

    图  4  不同气流速度下热分解产物的XRD谱

    Figure  4.  XRD spectra of prepared samples in different gas velocity

    (a) 0.5 L/min;(b) 1.5 L/min;(c) 2.0 L/min;(d) 2.5 L/min

    图  5  M相VO2的扫描电镜形貌和相应的元素分布

    (a) M相VO2的SEM形貌;(b) 氧元素分布;(c) 钒元素分布

    Figure  5.  SEM images of M-phase VO2(a) and relevant elements distribution maps(b-O, c-V)

    图  6  M相VO2超细颗粒的SEM形貌及尺寸分布

    (a) 1 000倍;(b) 5 000倍;(c) 微米级颗粒的尺寸分布;(d) 纳米级颗粒的尺寸分布

    Figure  6.  SEM images of M-phase VO2 nanoparticles and size distribution

    图  7  产品的差示热分析曲线

    Figure  7.  DSC curve of prepared sample

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出版历程
  • 收稿日期:  2021-12-01
  • 网络出版日期:  2022-04-24
  • 刊出日期:  2022-02-28

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