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以聚苯乙烯微球胶体晶体为硬模板、四氯化钛为氧化钛前驱体,结合控制浸渍-煅烧工艺制备了三维有序TiO2薄膜材料,重点考察了浸渍液中TiCl4的浓度对最终TiO2薄膜样品结构的影响。利用X射线衍射(XRD)、热重分析(TGA)、扫描电子显微镜(SEM)、能谱仪(EDS)、透射电子显微镜(TEM)、选区电子衍射(SAED)和N2吸附/脱附等手段对样品的结构特征进行表征。XRD分析表明,经500℃煅烧2 h后所得样品为锐钛矿相TiO2;SEM结果显示,在本实验条件下随着前驱体溶液中TiCl4浓度的增大,TiO2薄膜的微观结构逐步由三维有序大孔TiO2(three-dimensional ordered macro-porous TiO2,3DOM-TiO2)演变为三维有序TiO2中空球(three-dimensional ordered TiO2hollow-spheres,3DOH-TiO2);TEM结果表明,3DOM-TiO2和3DOH-TiO2薄膜样品骨架由氧化钛纳米颗粒组成,大孔孔壁和中空球壳壁上存在由TiO2纳米颗粒堆积形成的不规则介孔。
Three-dimensionally ordered TiO2 thin films were prepared by using polystyrene microsphere colloidal crystals as hard template and titanium tetrachloride as titanium oxide precursors in combination with controlled impregnation-calcination process. The effects of TiCl4 concentration in immersion solution on the final TiO2 film Effect of sample structure. XRD, TGA, EDS, TEM, SAED and N2 adsorption / desorption methods were used to investigate the thermal stability of the composites. The structural characteristics of the samples were characterized. The results of XRD showed that the samples obtained after calcination at 500 ℃ for 2 h were anatase TiO2. The SEM results showed that with the increase of TiCl4 concentration in the precursor solution under the experimental conditions, the microstructure of TiO2 films was gradually changed from three-dimensional The 3DOM-TiO2 and 3DOH-TiO2 were evolved into three-dimensional ordered TiO2hollow-spheres (3DOH-TiO2). TEM results showed that 3DOM-TiO2 and 3DOH- The TiO2 thin film sample framework consists of titanium oxide nanoparticles with irregular mesopores formed by the deposition of TiO2 nanoparticles on the walls of macropore and hollow spheres.