Transactions of Nonferrous Metals Society of China The Chinese Journal of Nonferrous Metals

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中国有色金属学报

ZHONGGUO YOUSEJINSHU XUEBAO

第22卷    第2期    总第155期    2012年2月

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文章编号:1004-0609(2012)02-0579-06
水热法制备超细焦绿石型三氧化钨及其表征
彭志宏,吴  旭,周秋生,喻晓剑,齐天贵,刘桂华,李小斌

(中南大学 冶金科学与工程学院,长沙 410083)

摘 要: 在水热条件下利用纯WO3作为添加剂能够直接从钨酸钠溶液中制备出超细焦绿石型三氧化钨(WO3·0.5H2O)粉体。结果表明:往100 g/L的钨酸钠溶液中添加WO3,在密闭压力容器内,在140 ℃下反应24 h,反应率能达到80%左右。采用XRD和SEM等测试手段对水热产物进行表征,产物为结晶良好的立方体结构,颗粒的平均尺寸小于1 μm。EDS检测表明:所得产品含微量的Na元素,经盐酸洗涤后可得到几乎不含杂质Na的WO3·0.5H2O粉体。利用IR光谱测定水热条件下钨酸钠溶液的离子结构变化,初步认为制备WO3·0.5H2O的生长基元为WO42−

 

关键字: 钨酸钠溶液;水热处理;焦绿石型三氧化钨;超细粉体

Preparation of ultrafine pyrochlore-type tungsten trioxide powder by hydrothermal method and its characterization
PENG Zhi-hong, WU Xu, ZHOU Qiu-sheng, YU Xiao-jian, QI Tian-gui, LIU Gui-hua, LI Xiao-bin

School of Metallurgical Science and Engineering, Central South University, Changsha 410083, China

Abstract:The ultrafine pyrochlore-type tungsten trioxide powders were hydrothermally synthesized from sodium tungstate solution by adding pure WO3 powders to the reaction system. The results show that the precipitation rate of tungsten species in solution can reach 80%. XRD analyses results indicate that the precipitates are powders with cubic crystal structure. EDS analyses results reveal that a small amount of impurity of sodium is present in the precipitates and it can be completely removed by washing in the diluted hydrochloric acid. SEM micrographs show that the average diameter of the precipitates is less than 1.0 μm. Based upon IR technique, a new reaction mechanism is proposed that WO42 may be the growth unit of pyrochlore-type tungsten trioxide during the hydrothermal precipitation process of sodium tungstate solution.

 

Key words: sodium tungstate solution; hydrothermal process; pyrochlore-type tungsten trioxide; ultrafine powder

ISSN 1004-0609
CN 43-1238/TG
CODEN: ZYJXFK

ISSN 1003-6326
CN 43-1239/TG
CODEN: TNMCEW

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