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动态碳热还原法制备纳米级钨粉
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中南大学粉末冶金研究院

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国家重点研发计划项目2022YFB3806701、2022YFB3806700


Preparation of nanoscale tungsten powder by dynamic carbon-thermal reduction method
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Powder Metallurgy Research Institute,Central South University,Changsha

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    摘要:

    高品质纳米钨粉是制取高性能纳米晶钨合金和硬质合金的前提,氢还原制备钨粉因产生WO2(OH)2导致钨粉晶粒长大,碳热还原法可有效避免这一问题。本研究重点对碳热还原温度、气氛、时间以及动/静态工序对产物相结构和粒度等影响规律进行研究。结果发现:真空气氛下产物纯度高于氩气气氛;随还原温度升高,产物由高价氧化钨向低价氧化钨转变并最终转变为纯钨;保温时间为1h时,随还原温度从1000℃升至1100℃,钨粉平均粒度由67nm升至118nm,还原温度为1000℃时,随保温时间从1h延长至3h,钨粉平均粒度从67nm升至93nm;动态还原因反应物接触更均匀、反应更充分所得产物纯度高于静态还原;在优化的1000℃、保温1h的真空动态碳热还原下,制备出平均粒径为67nm的纳米钨粉。

    Abstract:

    High-quality nano-tungsten powder is the prerequisite for the preparation of high-performance nanocrystalline tungsten alloys and cemented carbides. The tungsten powder prepared by hydrogen reduction producesWO2(OH)2, which leads to the growth of tungsten powder grains. The carbothermal reduction method can effectively avoid this problem. This study focuses on the influence of carbothermal reduction temperature, atmosphere, time and dynamic/static process on the phase structure and particle size of the product. The results showed that the purity of the product in vacuum atmosphere was higher than that in argon atmosphere. With the increase of reduction temperature, the product changes from high valence tungsten oxide to low valence tungsten oxide and finally to pure tungsten. When the holding time is 1h, the average particle size of tungsten powder increases from 67 nm to 118 nm with the increase of reduction temperature from 1000 ℃ to 1100℃.When the reduction temperature is 1000 ℃, the average particle size of tungsten powder increases from 67 nm to 93 nm with the increase of holding time from 1h to 3h. The dynamic reduction is also due to the more uniform contact of the reactants and the higher purity of the product obtained by the more complete reaction than the static reduction. Nano-tungsten powder with an average particle size of 67 nm was prepared under the optimized vacuum dynamic carbothermal reduction at 1000 ℃ for 1 h.

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张博林,鲍阔阔,唐家玉,马运柱.动态碳热还原法制备纳米级钨粉[J].稀有金属材料与工程,,().[Bolin Zhang, Kuokuo Bao, Jiayu Tang, Yunzhu Ma. Preparation of nanoscale tungsten powder by dynamic carbon-thermal reduction method[J]. Rare Metal Materials and Engineering,,().]
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  • 收稿日期:2024-12-26
  • 最后修改日期:2025-02-27
  • 录用日期:2025-03-03
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