Research progress on vanadium nitride preparation technology
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摘要: 氮化钒是一种性能优异的微合金化添加剂，同时，也在超级电容器、硬质涂层、工业催化等领域有着重要应用价值，其制备工艺的优化与创新一直是冶金及材料领域的研究热点。对现有氮化钒制备工艺进行分类介绍，包括碳热还原氮化法、氨气还原氮化法、含碳气体还原氮化法、前驱体法、金属钒直接氮化法、镁热还原氮化法以及化学气相沉积法，其中碳热还原氮化法按两步法和一步法进行探讨，对比总结了各种制备方法在原料和工艺参数选择以及产物元素含量上的差异，分析了各种方法的优势、不足以及应用场景，提出氮化钒的制备工艺，呈现出以碳热还原氮化法为核心，氨气还原氮化法、含碳气体还原氮化法及前驱体法稳步发展，其他研究方法处于小规模探索阶段的特点，并结合成本、环保、产品性能等要素，为氮化钒制备工艺的发展提供了参考方向。Abstract: Vanadium nitride is a kind of microalloying additive with excellent performance, and it also possesses significant practical value in other fields such as supercapacitors, hard coatings, and industrial catalysis. The optimization and innovation of its preparation technology have attracted continuous research attention in the fields of metallurgy and materials science. In this paper, a classified introduction to the existing vanadium nitride preparation methods was provided, including carbothermal reduction-nitridation, ammonia reduction-nitridation, carbonaceous gas reduction-nitridation, precursor method, direct nitridation of metallic vanadium, magnesiothermic reduction-nitridation, and chemical vapor deposition (CVD). Among these, the carbothermal reduction-nitridation method was discussed in terms of the two-step method and one-step method. A comparative analysis of raw material selection, process parameter configuration, and product element content was additionally presented, with a systematic evaluation of the advantages, disadvantages as well as application scale and scenarios of each process. It was proposed that the preparation processes of vanadium nitride were characterized by taking the carbothermal reduction-nitridation method as the core, with the ammonia reduction-nitridation method, carbonaceous gas reduction-nitridation method and precursor method developing steadily, while other research methods were still in the stage of small-scale exploration. In addition, considering factors such as cost, environmental protection and product performance, this paper presented the possible directions for the future development of vanadium nitride preparation technology.
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表 1 氮化钒制备工艺对比
Table 1. Comparison of VN preparation technologies
VN preparation technology Main V/C/N sources Reaction temperature/℃ Element
content /%Advantages Disadvantages Application scale and scenario References Two-step carbothermal reduction-nitridation V2O3, V2O5/C powder/N2 ~ 1 400* V: 72.99～78.7
N: 7.3～13
C: 0.95～10.5Controllable process parameters and product quality Long reaction process, strict reaction conditions (vacuum) Small-scale industrial application [11-15] One-step carbothermal reduction-nitridation V2O3, V2O5, NH4VO3/C powder/N2 ~1 450 V: 77～82
N: 10.19～20.98
C: 1.123～7Short reaction process, simple operation, continuous production feasibility High temperature, precise parameter regulation required for high quality products Industrial-scale high-volume production [16-35] Ammonia reduction- nitridation V2O3, V2O5/ without C/NH3 600～850 N: 15.83～17.4 Low temperature, short time, no residual C High cost, corrosiveness to equipment, environmental pollution Lab scale [39-42] Carbonaceous gas reduction-nitridation V2O3/CH4/N2 900～1 150 N: 14.2～16.2
C: 3.35～4.87Low temperature, short reaction process, low cost Precise parameter regulation required for avoiding residual C Lab scale [43-44] Precursor of V-containing compounds or composites V-precursors and NH3 700～850 Low temperature, nanoscale product particle size Complicated process in precursor preparation Lab scale production for specific fields [45-48] Precursor of mixture of V source and C V, C-precursors and N2 1 100～1 150 V: 78.93～79.32
N: 16.38～17.91Sufficient contact between V source and C, low temperature, short time Complicated operation required for avoiding C agglomeration Lab scale [49-52] Direct nitridation V metal V metal/without C/N2 1 650** Simple reaction routes, no impurity elements High cost, strict reaction conditions Lab scale [53-54] Magnesiothermic reduction-nitridation V2O3, V2O5/ without C/N2 675～900 (in molten salt) No residual C, low temperature High cost, complicated process in post-treatment Lab scale [55-56] Chemical vapor deposition VCl4, V2O5/ without C/ N2, NH3 350～650 (VCl4) or 900～1 300 (V2O5) High hardness and high stability of VN products High cost, complicated process Lab scale production for specific fields [57-58] * The first step was mainly conducted under vacuum；** Mechanical grinding in room temperature was also possible. 
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