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微孔–介孔钛硅氧化物复合材料的合成与表征
SYNTHESIS AND CHARACTERIZATION OF MICRO- AND MESO-POROUS TITANIA–SILICA COMPOSITE MATERIALS
【摘要】 以十六烷基三甲基溴化铵为模板剂诱导硅酸钠水解形成的多孔二氧化硅为硫酸钛水解的“模板”,用溶胶–凝胶技术和水热处理工艺合成钛硅复合材料前驱体。通过两步灼烧法可脱除前驱体中的有机模板。通过X射线衍射、差热分析和低温氮吸附等测试技术对产物进行表征。结果表明:硅浓度约为0.1mol/L,起始钛浓度约为0.125mol/L,pH值为1时,硫酸钛于室温下水解制备的前驱体具有较好的孔结构。前驱体首先在350℃灼烧4h,再在750℃灼烧4h后的产物为晶体结构趋于规整的锐钛矿型二氧化钛,比表面积高达369m2/g,并具有良好的热稳定性。通过t–曲线计算出微孔和介孔对比表面及孔体积的贡献。
【Abstract】 Using cetyl trimethyl ammonium bromide as the template to induce hydrolysis of sodium silicate, and the obtained hydro- lytic product porous silica as the template for the hydrolysis of titanium sulfate, titania–silica composite precursor was synthesized via sol–gel and hydrothermal process. A heat treatment of the two-step calcination was used to remove the organic template. The products were characterized by X-ray diffraction, differential thermal analysis, and N2 absorption measurements. The results show that the synthesized precursor has an ordered pore structure when the Ti(SO4)2 hydrolysis pH value is 1, the hydrolysis temperature is at an ambient temperature, the concentration of sodium silicate is approximately 0.1 mol/L, and the initial concentration of titanium sulfate is approximately 0.125 mol/L. The product obtained after the first calcination at 350 ℃ for 4 h and the second calcination at 750 ℃ for 4 h has a regular crystal structure of anatase, and still has a large specific surface area of 369 m2/g and has good thermal stability. Based on the t–plot method, the specific surface area and pore volume from the micropore and mesopore contribution are calculated, respectively.
【Key words】 titania–silica composite; micro-and mesoporous; specific surface area; thermal stability;
- 【文献出处】 硅酸盐学报 ,Journal of the Chinese Ceramic Society , 编辑部邮箱 ,2007年04期
- 【分类号】TN304
- 【被引频次】7
- 【下载频次】606