The NiO/SnO 2 nanocomposites have been prepared by the simple coprecipitation method and further characterized by the XRD, SEM, TEM, UV-Vis, and BET. X-ray diffraction (XRD) data analyses indicate the exclusive formation of nanosized particles with rutile-type phase (tetragonal SnO 2 ) for Ni contents below 10 mol%. Only above 10 mol% Ni, the formation of a second NiOrelated phase has been determined. The particle size is in the range from 12 to 6 nm. It decreases with increasing amounts of doping NiO. The morphology of NiO-doped SnO 2 nanocrystalline powders is spherical, and the distribution of particle size is uniform, as seen from transmission electron microscopy (TEM). The photocatalytic oxidation of CO over NiO/SnO 2 photocatalyst has been investigated under UV irradiation. Effects of NiO loading on SnO 2 , photocatalyst loading, and reaction time on photocatalytic oxidation of CO have been systematically studied. Compared with pure SnO 2 , the 33.3 mol% NiO/SnO 2 composite exhibited approximately twentyfold enhancement of photocatalytic oxidation of CO. Our results provide a method for pollutants removal. Due to simple preparation, high photocatalytic oxidation of CO, and low cost, the NiO/SnO 2 photocatalyst will find wide application in the coming future of photocatalytic oxidation of CO.