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 N adsorption isotherm changed significantly, indicating the decrease of the Brunauer-Emmett-Teller surface area from 743 to 283 m/g and of the pore volume from 1.27 to 0.26 cm/g, respectively. After the crystallization to anatase, the TiO 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.