Controllable structure of TiO2 powders were prepared using sulfate ion, and mesoporous TiO2 nanoparticles were prepared by hydrothermal method using surfactant Pluronic-F68. The samples were characterized by XRD, TEM, N2-sorption, and UV-Vis diffuse reflectance spectra. Photocatalytic activity of TiO2 materials was investigated by measuring the photodecomposition of congo red. In result, mesoprous TiO2 which has large surface area was found to exhibit better photocatalytic acticity.