TiO2 nanopowders doped with Cu and Zr were prepared via process-controlled sol–gel method. The effects of Zr and Cu doping on the structural and photocatalytic properties of synthesized nanopowders have been studied by X-ray diffraction (XRD), scanning electron microscope, transmission electron microscope, FTIR, and UV–Vis absorption spectroscopy. XRD results suggested that adding dopants has a great effect on crystallinity and particle size of TiO2. Titania rutile phase formation was inhibited by Zr4? and promoted by Cu2? doping. The photocatalytic activity was evaluated by degradation kinetics of aqueous methyl orange under visible spectra radiation. The results showed that the photocatalytic activity of the 15 % Zr-doped TiO2 nanopowder has a larger degradation efficiency than 5 % Cu-doped and pure TiO2 under visible light.