Size-Controlled Synthesis of Anatase in a Mesoporous Silica, SBA-15.

The preparation of anatase in the cylindrical mesopore of SBA-15 (pore size of 8 nm) was done by the impregnation of tetraisopropyl orthotitanate and its subsequent crystallization. The impregnation was done without a solvent. Hydrolysis and condensation were promoted by the HCl vapor to encapsulate a larger amount of titanium oxo species in the mesopore and to suppress the desorption of the titanium oxo species during crystallization to anatase. After the reaction, the shape of the N2 adsorption isotherm changed significantly, indicating the decrease of the Brunauer-Emmett-Teller surface area from 743 to 283 m2/g and of the pore volume from 1.27 to 0.26 cm3/g, respectively. After the crystallization to anatase, the TiO2 content in the product was estimated to be 62 mass %, filling 30% of the pore volume of SBA-15. The homogeneous distribution of titanium in the SBA-15 sample was confirmed by elemental mapping based on scanning electron microscopy/energy-dispersive X-ray spectrometry. The crystal size of the anatase was determined to be ca. 8.1 nm, which is consistent with the pore size of the used SBA-15 (8.0 nm, derived from the Barrett-Joyner-Halenda analysis of the nitrogen adsorption isotherm). The zeta potential measurements showed the absence of anatase as isolated particles or on the surface of SBA-15 particles. All of these characterizations confirmed the successful size-controlled synthesis of anatase in the mesopore of SBA-15.