水热合成钨前驱体-碳热还原-碳化制备超细纳米级碳化钨  

Preparation of Ultrafine Nanosized Tungsten Carbide by Hydrothermal Synthesis of Tungsten Precursor,Carbothermic Reduction,and Carburization

作　　者：李江涛 罗勇进 苏准 赵中伟 陈爱良 刘旭恒 何利华 孙丰龙 陈星宇 Li Jiangtao;Luo Yongjin;Su Zhun;Zhao Zhongwei;Chen Ailiang;Liu Xuheng;He Lihua;Sun Fenglong;Chen Xingyu(School of Metallurgy and Environment,Central South University,Changsha 410083,China;Key Laboratory of Hunan Province for Metallurgy and Material Processing of Rare Metals,Changsha 410083,China;School of Materials Science and Engineering,Shanghai Jiao Tong University,Shanghai 200240,China)

机构地区：[1]中南大学冶金与环境学院,湖南长沙410083 [2]稀有金属冶金与材料制备湖南省重点实验室,湖南长沙410083 [3]上海交通大学材料科学与工程学院,上海200240

出　　处：《稀有金属材料与工程》2024年第2期321-329,共9页Rare Metal Materials and Engineering

基　　金：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)。

摘　　要：提出了一种以水热合成的PbWO_(4)为原料,然后通过碳热还原-碳化获得超细WC的方法。以PbWO_(4)为钨中间产品,避免了氨氮试剂的引入;采用碳还原的方式可避免水蒸气的产生,抑制了钨粉的长大。结果表明:在初始pH为7.0、反应温度为160℃,反应时间为4.5h的条件下,Na_(2)WO_(4)溶液中99.9%(质量分数)以上的W以PbWO_(4)的形式回收。然后采用低温碳还原PbWO_(4),在C:W摩尔比为5、950℃的条件下还原3h,获得了W和C的混合物,该混合物中预加富余的C有助于抑制钨粉的团聚。然后将W和C混合物高温碳化,在1200℃下反应6h,获得了粒径约为60nm的WC粉末。A novel method to prepare ultrafine WC was proposed:the PbWO_(4)prepared by hydrothermal synthesis was used as raw material,and WC was obtained through the carbothermic reduction-carburization process.PbWO_(4)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 PbWO_(4)from the Na_(2)WO_(4)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 PbWO_(4)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.Subsequently,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.

关 键 词：钨酸铅 超细碳化钨 水热处理 还原碳化 

分 类 号：TB383.1[一般工业技术—材料科学与工程] TQ136.13[化学工程—无机化工]