Titania-silica mixed metal oxide materials with a mesostructure have been prepared by a novel method in which hydrolysis and condensation of titanium tetraisopropoxide (TTIP) and tetraethoxysilane (TEOS) were controlled by the pH change of acidic solution using cetyltrimethylammonium bromide (CTAB) as the structure-directing agent. The prepared materials were characterized by TEM, XRD, XPS, FT-IR and nitrogen sorption. The resulting materials showed a short-range ordered mesoporous structure with the nanoparticles (8 nm) of TiO2, dispersed uniformly on SiO2, Supports. These TiO2-SiO2 mesoporous materials were also found to have a higher photocatalytic activity than that of commercial pure TiO2, nanoparticles at the same titanium loading for the degradation of methyl orange. (c) 2005 Elsevier B.V. All rights reserved.