氢气还原制备一氧化钒试验研究

于杰; 黄青云; 钟大鹏; 裴贵尚; 苏丽佳; 徐海铭; 向俊一

doi:10.7513/j.issn.1004-7638.2026.01.002

氢气还原制备一氧化钒试验研究

doi: 10.7513/j.issn.1004-7638.2026.01.002

1.
重庆科技大学冶金与动力工程学院, 重庆 401331
2.
重庆大学材料科学与工程学院, 重庆 400044
3.
首尔国立大学材料科学与工程系, 韩国首尔 08826

基金项目: 国家自然科学基金（52404314, 52425408）；重庆市自然科学基金（cstc2021jcyj-msxmX0882）；重庆科技大学硕士研究生创新计划项目（YKJCX2420208）。

详细信息

作者简介:
于杰，2000年出生，男，山西大同人，硕士研究生，研究方向为高纯金属钒制备，E-mail：2023202007@cqust.edu.cn

通讯作者:
黄青云，1982年出生，女，博士，长期从事冶金物化基础研究工作，E-mail：qyhuang08@126.com

中图分类号: TF841.3
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出版历程
- 收稿日期: 2025-04-16
- 录用日期: 2025-05-30
- 修回日期: 2025-05-25
- 网络出版日期: 2026-02-28
- 刊出日期: 2026-02-28

Experimental study of vanadium monoxide synthesis via hydrogen reduction

1.
School of Metallurgical and Power Engineering, Chongqing University of Science and Technology, Chongqing 401331, China
2.
College of Materials Science and Engineering, Chongqing University, Chongqing 400044, China
3.
Department of Materials Science and Engineering, Seoul National University, Seoul 08826, South Korea

摘要

摘要: 一氧化钒（VO）作为高能量和高功率锂离子电池（LIBs）的潜在负极材料，其现有合成方法存在纯度低、成本高、工艺复杂等问题，限制了其在电极材料上的应用。笔者提出了采用氢气还原V₂O₃制备VO新工艺，以V₂O₃为原料、H₂为还原剂，系统研究了还原温度、还原时间等因素的影响。通过V-H-O多相反应实现VO的制备，制得的VO粉体颗粒表面较为平整，呈现出近似球或椭球的形状；XRD衍射图谱与标准衍射图谱呈现高度一致性，峰位对应精准，峰形尖锐且半峰宽较窄，表明其结晶程度优良。通过优化参数，确定最佳VO还原条件，当还原温度1500 ℃、还原时间5.5 h、氢气流速0.264 cm/s时，钒含量约78.27%，符合VO_0.80-VO_1.20。
- H₂ /
- VO /
- 负极材料 /
- 热还原
Abstract: Vanadium monoxide (VO), recognized as a potential anode material for high-energy and high-power lithium-ion batteries (LIBs), is limited in its application as an electrode material due to its low purity, high cost and complex process in existing synthesis process. The authors propose a novel hydrogen reduction process for VO synthesis using V₂O₃ as the raw material and H₂ as the reducing agent. The key parameters such as reduction temperature, reaction duration, and others were systematically investigated. The preparation of VO is achieved through the V-H-O multiphase reaction, and the resulting VO powder particles have relatively smooth surfaces, presenting an approximating spherical or ellipsoidal shape. The XRD diffraction pattern closely matches with the reference diffraction pattern, with accurate peak positions, sharp profiles, and narrow full widths at half maximum, indicating excellent crystallinity. By optimizing parameters, the optimal reduction conditions were determined. When the reduction temperature is 1500 ℃, the reaction time is 5.5 h, hydrogen flow rate is 0.264 cm/s, the vanadium content is about 78.27%, which is consistent with VO_0.80-VO_1.20.
- H₂ /
- VO /
- anode material /
- thermal reduction

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图 1 以V₂O₃粉末为原料的XRD谱图

Figure 1. XRD pattern with V₂O₃ powder as the raw material

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图 2 VO制备试验装置

Figure 2. Schematic diagram of the experimental device for the preparation of vanadium monoxide

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图 3 钒氧化物氧势^[22]

Figure 3. Oxygen potential diagram of vanadium oxide^[22]

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图 4 不同反应温度下还原产物的XRD谱图

Figure 4. XRD patterns of reduction products at different reaction temperatures

(a) 1450 ℃, Rwp=3.66%，Rp=2.63%，χ²=1.92； (b) 1475 ℃，Rwp=7.04%，Rp=4.43%，χ²=2.62； (c) 1500 ℃，Rwp=3.08%，Rp=2.53%，χ²=1.32； (d) 1525 ℃，Rwp=3.29%，Rp=2.87%，χ²=1.46。

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图 5 不同反应温度的VO还原度

Figure 5. Reduction degree of VO at different reaction temperatures

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图 6 不同反应时间下还原产物的XRD谱图

Figure 6. XRD patterns of reduction products under different reaction time

(a)4.5 h，Rwp=6.01%，Rp=4.77%，χ²=3.12； (b)5 h，Rwp=6.22%，Rp=4.86%，χ²=2.89； (c)5.5 h，Rwp=4.52%，Rp=2.34%，χ²=1.87；(d)6 h，Rwp=3.08%，Rp=2.53%，χ²=1.32

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图 7 不同保温时间的VO还原度

Figure 7. Reduction degree of VO under different heat preservation times

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图 8 不同氢气流速下还原产物的XRD谱图

Figure 8. XRD patterns of reduction products at different hydrogen flow rates

(a) 0.15 cm/s，Rwp=7.53%，Rp=4.30%，χ²=3.07； (b) 0.188 cm/s，Rwp=6.14%，Rp=3.95%，χ²=1.99；(c) 0.226 cm/s，Rwp=6.71%，Rp=4.44%，χ²=2.28；(d) 0.264 cm/s，Rwp=4.52%，Rp=2.34%，χ²=1.87。

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图 9 不同氢气流速的VO还原度

Figure 9. Reduction degree of VO at different hydrogen flow rates

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图 10 不同放大倍数下VO粉末的SEM-EDS图

Figure 10. SEM-EDS analysis of VO powder at different magnification levels

(a)10 μm；(b) 20 μm；(c) 50 μm

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表 1 VO粉末中钒含量分析

Table 1. Analysis of vanadium content in vanadium monoxide (powder)

Sample number Element content/%

1 78.27
2 78.22
3 79.97
4 79.89

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