物理化学学报 >> 2009, Vol. 25 >> Issue (09): 1890-1894.doi: 10.3866/PKU.WHXB20090914

研究论文 上一篇    下一篇

氧化钨介孔材料的制备与表征

余勇, 刘士军, 李洁, 陈启元   

  1. 中南大学化学化工院, 长沙 410083
  • 收稿日期:2009-02-26 修回日期:2009-05-14 发布日期:2009-09-03
  • 通讯作者: 刘士军 E-mail:liushijun@hotmail.com

Preparation and Characterization ofMesoporous Tungsten Oxides

YU Yong, LIU Shi-Jun, LI Jie, CHEN Qi-Yuan   

  1. College of Chemistry and Chemical Engineering, Central South University, Changsha 410083, P. R. China
  • Received:2009-02-26 Revised:2009-05-14 Published:2009-09-03
  • Contact: LIU Shi-Jun E-mail:liushijun@hotmail.com

摘要:

以介孔二氧化硅(KIT-6)为硬模板, 硅钨酸为钨源, 用硬模板法制备WO3-SiO2复合材料, 再利用HF除去二氧化硅, 得到了介孔三氧化钨材料. 用X射线衍射(XRD)、能量扩散X射线(EDX)、高分辨透射电镜(HRTEM)、N2吸附-脱附等表征手段, 对制备复合材料的物料比、煅烧温度以及不同分散剂等条件进行了考察. 结果表明, 硅钨酸与硅介孔的物料比(m(WO3)/m(SiO2))在3:1到4:1之间, 在600-750 ℃下煅烧, 能制备结构较好的介孔氧化钨. 乙醇和蒸馏水为分散剂时, 用乙醇为分散剂所得的介孔WO3材料具有更高的比表面积和孔体积.

关键词: 介孔材料, 氧化钨, 二氧化硅, 硬模板法

Abstract:

Mesoporous tungsten oxides were prepared by a hard templating method using mesoporous silica dioxide (KIT-6) as the hard template, silicotungstic acid (H4O40SiW12·nH2O) as the source of tungsten and by removing silica dioxide with HF. The mesoporous tungsten oxides were characterized by X-ray diffraction (XRD), energy dispersive X-ray(EDX), high resolution transmission electron microscopy (HRTEM), and nitrogen adsorption-desorption isotherms. The influences of the mixing ratio of the silicotungstic acid and mesoporous silica, the calcination temperature of the mixture, and different dispersants on the preparation of the mesoporous tungsten oxides was investigated. Results showed that mesoporous tungsten oxides could be obtained at calcination temperatures of 600-750 ℃ and that mixing mass ratios of silicotungstic acid and mesoporous silica (m(WO3)/m(SiO2)) should be 3:1-4:1. Larger surface area and pore volume were obtained for the mesoporous tungsten oxide when using ethanol instead of distilled water as dispersant.

Key words: Mesoporous material, Tungsten oxide, Silicon dioxide, Hard templating method

MSC2000: 

  • O643