Ordered mesoporous TiO(2) materials with an anatase frameworks have been synthesized by using a cationic surfactant cetyltrimethylammonium bromide (C(16)TMABr) as a structure-directing agent and soluble peroxytitanates as Ti precursor through a self-assembly between the positive charged surfactant S(+) and the negatively charged inorganic framework I(-) (S(+)I(-) type). The low-angle X-ray diffraction (XRD) pattern of the as-prepared mesoporous TiO(2) materials indicates a hexagonal mesostructure. XRD and transmission electron microscopy results and nitrogen adsorption-desorption isotherms measurements indicate that the calcined mesoporous TiO(2) possesses an anatase crystalline framework having a maximum pore size of 6.9 nm and a maximum Brunauer-Emmett-Teller specific surface area of 284 m(2) g(-1). This ordered mesoporous anatase TiO(2) also demonstrates a high photocatalytic activity for degradation of methylene blue under ultraviolet irradiation.