4為原料,然后通過碳熱還原-碳化獲得超細(xì)WC的方法。以PbWO4為鎢中間產(chǎn)品,避免了氨氮試劑的引入;采用碳還原的方式可避免水蒸氣的產(chǎn)生,抑制了鎢粉的長大。結(jié)果表明:在初始pH為7.0、反應(yīng)溫度為160 ℃,反應(yīng)時(shí)間為4.5 h的條件下,Na2WO4溶液中99.9%(質(zhì)量分?jǐn)?shù))以上的W以PbWO4的形式回收。然后采用低溫碳還原PbWO4,在C:W摩爾比為5、950 ℃的條件下還原3 h,獲得了W和C的混合物,該混合物中預(yù)加富余的C有助于抑制鎢粉的團(tuán)聚。然后將W和C混合物高溫碳化,在1200 ℃下反應(yīng)6 h,獲得了粒徑約為60 nm的WC粉末。"/>

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水熱合成鎢前驅(qū)體-碳熱還原-碳化制備超細(xì)納米級(jí)碳化鎢
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1.中南大學(xué) 冶金與環(huán)境學(xué)院,湖南 長沙 410083;2.稀有金屬冶金與材料制備湖南省重點(diǎn)實(shí)驗(yàn)室,湖南 長沙 410083;3.上海交通大學(xué) 材料科學(xué)與工程學(xué)院,上海 200240

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Preparation of Ultrafine Nanosized Tungsten Carbide by Hydrothermal Synthesis of Tungsten Precursor, Carbother-mic Reduction, and Carburization
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1.School of Metallurgy and Environment, Central South University, Changsha 410083, China;2.Key Laboratory of Hunan Province for Metallurgy and Material Processing of Rare Metals, Changsha 410083, China;3.School of Materials Science and Engineering, Shanghai Jiao Tong University, Shanghai 200240, China

Fund Project:

National Natural Science Foundation of China (51334008); National Key Research and Development Program of China (2022YFC2904505); Project of Basic Science Center of the National Natural Science Foundation (72088101)

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    摘要:

    提出了一種以水熱合成的PbWO4為原料,然后通過碳熱還原-碳化獲得超細(xì)WC的方法。以PbWO4為鎢中間產(chǎn)品,避免了氨氮試劑的引入;采用碳還原的方式可避免水蒸氣的產(chǎn)生,抑制了鎢粉的長大。結(jié)果表明:在初始pH為7.0、反應(yīng)溫度為160 ℃,反應(yīng)時(shí)間為4.5 h的條件下,Na2WO4溶液中99.9%(質(zhì)量分?jǐn)?shù))以上的W以PbWO4的形式回收。然后采用低溫碳還原PbWO4,在C:W摩爾比為5、950 ℃的條件下還原3 h,獲得了W和C的混合物,該混合物中預(yù)加富余的C有助于抑制鎢粉的團(tuán)聚。然后將W和C混合物高溫碳化,在1200 ℃下反應(yīng)6 h,獲得了粒徑約為60 nm的WC粉末。

    Abstract:

    A novel method to prepare ultrafine WC was proposed: the PbWO4 prepared by hydrothermal synthesis was used as raw material, and WC was obtained through the carbothermic reduction-carburization process. PbWO4 was used as the tungsten intermediate product to avoid the introduction of ammonia nitrogen reagent. The carbon reduction method can avoid the generation of water vapor and inhibit the growth of tungsten powder. Results show that more than 99.9wt% of W is extracted in the form of PbWO4 from the Na2WO4 solution under the conditions of initial pH value of 7.0, reaction temperature of 160 °C, and reaction time of 4.5 h. Then, the homogeneous mixture of W and C is obtained by the carbothermic reduction of PbWO4 at 950 °C for 3 h with the molar ratio of carbon:tungsten as 5. Pre-adding excessive carbon in the mixture can inhibit the agglomeration of tungsten powder. Subsequ-ently, the WC powder with particle size of about 60 nm is obtained by the carburization of the W and C mixture at 1200 °C for 6 h.

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李江濤,羅勇進(jìn),蘇準(zhǔn),趙中偉,陳愛良,劉旭恒,何利華,孫豐龍,陳星宇.水熱合成鎢前驅(qū)體-碳熱還原-碳化制備超細(xì)納米級(jí)碳化鎢[J].稀有金屬材料與工程,2024,53(2):321~329.[Li Jiangtao, Luo Yongjin, Su Zhun, Zhao Zhongwei, Chen Ailiang, Liu Xuheng, He Lihua, Sun Fenglong, Chen Xingyu. Preparation of Ultrafine Nanosized Tungsten Carbide by Hydrothermal Synthesis of Tungsten Precursor, Carbother-mic Reduction, and Carburization[J]. Rare Metal Materials and Engineering,2024,53(2):321~329.]
DOI:10.12442/j. issn.1002-185X. E20230018

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  • 收稿日期:2023-07-05
  • 最后修改日期:2023-09-22
  • 錄用日期:2023-10-07
  • 在線發(fā)布日期: 2024-02-27
  • 出版日期: 2024-02-23