A copper(II) and iron(III) co-modified titanium dioxide nano material was prepared by a simple sol-gel process using titanium(IV) isopropoxide plus copper(II) and iron(III) nitrates as raw materials. The as-prepared nanocomposites were characterized by X-ray diffraction (XRD), diffuse reflectance spectroscopy and photoluminescence spectra. The XRD results showed that the undoped TiO 2 nanoparticles mainly include anatase phase while the Cu, Fe-codoped TiO 2 nanoparticles showed a mixture of anatase phase with a small fraction of rutile phase displaying higher activity than the pure anatase phase. Optical characterization showed that the codoping with copper(II) and iron(III) resulted in a red shift of adsorption and lower recombination probability between electrons and holes, which were associated with high photocatalytic activity of the Cu, Fe-codoped TiO 2 nanoparticles under visible light (k [ 400 nm). The photocatalytic activity of the samples was tested by aqueous methyl orange degradation. The capability of the codoped catalyst was much higher than that of the pure TiO 2 catalyst under visible irradiation. A mechanism is proposed in order to account for the enhanced catalytic activity.