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柠檬酸溶胶法制备Bi2WO6粉体及其表征
引用本文:蔡宗英,周若,孙文龙,曹卫刚.柠檬酸溶胶法制备Bi2WO6粉体及其表征[J].有色金属科学与工程,2018,9(2):30.
作者姓名:蔡宗英  周若  孙文龙  曹卫刚
作者单位:华北理工大学冶金与能源学院,河北 唐山 063210
基金项目:河北省杰出青年培育基金资助项目E2015209021国家自然科学基金资助项目51274082国家自然科学基金资助项目51474088
摘    要:利用钨酸铵、硝酸铋、柠檬酸和硝酸为原料,柠檬酸溶胶法制备了Bi2WO6粉体.热重-差热(TG-DTA)和红外光谱(FT-IR)分析Bi2WO6前驱体的热分解过程,X射线衍射(XRD)、场发射扫描电镜(FE-SEM)对Bi2WO6粉体结构、形貌进行表征.结果表明,Bi2WO6前驱体热分解分为4个阶段,其中Bi2WO6粉体开始形成发生在367 ℃. Bi2WO6前驱体在400~700 ℃煅烧5 h获得了单一的Bi2WO6粉体,当温度低于600 ℃时,产物为球形颗粒,晶粒尺寸随温度升高变化不大,当温度达到700 ℃时,晶粒迅速长大,最终发展成为规则的正交晶系.这表明晶体生长过程发生了由扩散机制向界面反应控制机制的转变,因此通过调整煅烧反应温度和保温时间可以控制产物的尺寸和形貌. 

关 键 词:Bi2WO6    粉体    柠檬酸溶胶    制备
收稿时间:2017-12-06

Preparation and characteristics of Bi2WO6 powders by citrate sol process
Affiliation:College of Metallurgy and Energy, North China University of Science and Technology, Tangshan 063210, China
Abstract:Bismuth tungsten oxide (Bi2WO6) powders were synthesized by citrate sol process using ammonium tungstate, bismuth nitrate, citrate and nitric acid as the starting materials. The structure and morphology of as-synthesized Bi2WO6 samples were characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM). Thermogravimetry and differential thermal analysis (TG-DTA) and Fourier transform infrared spectroscopy (FT-IR) were applied to analyze the thermal behavior of the Bi2WO6 precursor. There are four stages were found in the TG-DTA curves of the Bi2WO6 precursor, and the Bi2WO6 started to be formed at 367 ℃ in the third stage. The pure bismuth tungsten oxide powders were prepared by calcination of the precursors at 400~700 ℃ for 5 h. The spherical particle size of Bi2WO6 powders does not change apparently with increasing temperature below 600 ℃. The grain grow up rapidly and orthogonal crystal system obtained when the temperature at above 700 ℃. The crystal grow process of Bi2WO6 undergoes a transition from a diffusion control mechanism to an interfacial reaction controlled mechanism as the temperature increasing. The morphology and size can be controlled by setting the calcination temperature and the soaking time. 
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