N, Cd-codoped TiO2 has been synthesized by sol-gel method coupling with thermolysis. The products were characterized by XRD, SEM, UV-visible DRS, XPS and BET analysis, respectively. The photocatalytic activities of samples were evaluated on the degradation of methyl orange (MO). It was showed that particle sizes of anatase photacatalysts were about 10-15 nm. The maximum specific surface area of the products was 102.7 m2⋅g-1. N atoms were incorporated into the TiO2 crystal lattice, while Cd atoms existed on the crystal surface. The optical absorption edge of N, Cd-codoped TiO2 was 435 nm, which illustrated that the product represented photoactivity in the visible region. It indicated a strong N-Cd synergistic interaction appeared to play a decisive role in driving the excellent photoactivity performance of N,Cd-codoped TiO2.