Mesoporous silica (SBA-15 with the BJH pore size of 8 nm) containing anatase nanoparticles in the pore with two different titania contents (28 and 65 mass%), which were prepared by the infiltration of the amorphous precursor derived from tetraisopropyl orthotitanate into the pore, were heat treated in air to investigate the structural changes (both mesostructure of the SBA-15 and the phase and size of the anatase in the pore). The mesostructure of the mesoporous silica and the particle size of anatase unchanged by the heat treatment up to 800 °C. The heat treatment at the temperature higher than 1000 °C resulted in the collapse of the mesostructure and the growth of anatase nanoparticles as well as the transformation to rutile, while the transformation of anatase to rutile was suppressed especially for the sample with the lower titania content (28 mass%). The resulting mesoporous silica-anatase hybrids exhibited higher benzene adsorption capacity (adsorption from water) over those heated at lower temperature, probably due to the dehydroxylation of the silanol group on the pore surface. The photocatalytic decomposition of benzene in water by the present hybrid heated at 1100 °C was efficient as that by P25, a benchmark photocatalyst.

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.

Precise and systematic structural design of host–guest complexes of mesoporous silica and immobilized anatase nanoparticles was achieved by carefully designed syntheses.

Well-defined nanoparticles of rutile (with the size of 5 nm) were successfully prepared by the unusual solid-state transformation of an amorphous precursor in well-defined nanospace of a mesoporous silica template (SBA-15) at room temperature. An aqueous colloidal suspension of the rutile nanoparticles was successfully obtained by dissolution of SBA-15 and subsequent pH adjustment. The isolated rutile nanoparticles were used for H 2 evolution from an aqueous methanol solution by UV irradiation.

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Crystallization of well-defined anatase nanoparticles (5 nm) in the mesopore (6 nm) of SBA-15 over 400 °C, results the high photocatalytic activity for decomposition of acetic acid compared with other commercial titanium dioxides.

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