A visible light responsive N, Mo co-doped TiO 2 were prepared by sol-gel method. X-ray diffraction, TEM, N 2 adsorption, UV-vis spectroscopy, photoluminescence, and X-ray photoelectron spectroscopy were used to characterize the prepared TiO 2 samples. Doping restrained the phase transformation from anatase to rutile and reduced the particle sizes. The band gap was much narrowed after N, Mo co-doping. The photocatalytic activities were tested in the degradation of an aqueous solution of a reactive dyestuff, methylene blue, under visible light. The photocatalytic activities of doped TiO 2 were much higher than that of neat TiO 2 . The photocatalytic stability of N, Mo co-doped TiO 2 was much better than that of N doped TiO 2 .