Sb2O3/TiO2 nanoparticles were synthesized by a facile hydrothermal method, and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transfer infrared (FT-IR) spectroscopy and X-ray photoelectron spectroscopy (XPS). The photocatalytic activities of Sb2O3/TiO2 nanoparticles were evaluated by the degradation of methyl orange. The results show that the Sb2O3 doping enhanced the photocatalytic activity of TiO2, and the 0.5%Sb2O3/TiO2 nanoparticles show the best photocatalytic activity. The separation of photoinduced electron-hole pairs on the Sb2O3/TiO2 photocatalyst surface is an important step in the photocatalytic reaction because of the Sb2O3 coupling. (c) 2012 Elsevier B.V. All rights reserved.