On latest years, an emergency requirement for clean methods to improvement of environment worth has attracted attention in several researches’ fields. The use of films on photocatalysis process is one of the most interesting alternatives due to its easily on separation of residual water and recovery of photocatalyst. In this study, CuO/TiO2:ZrO2 catalysts with various molar ratios of CuO were synthesized by sol-gel dip-coating process. The dip-coated thin films have been examined at different annealing temperatures 500, 800 and 1000 °C. The crystalline structures, morphology, constituent contents, optical and photocatalytic properties of the as-prepared catalysts were analyzed by X–ray diffraction (XRD), Raman spectroscopy, FT-IR spectra, UV-VIS, Photoluminescence spectroscopy (PL) techniques. X-ray diffraction (XRD) and Raman results indicated that an increase in annealing temperature from 500°C to 1000°C caused a transformation of crystallinity from anatase and brookite at 500°C to rutile and monoclinic CuO phases at 1000°C, accompanied by an increase in the particle sizes. The optical transmittance of the films, increased to over 90% in the visible region, indicate that copper loading decreases the band gap from 3.53 to 3.39eV. The PL experiments revealed that the recombination of photoinduced electrons and holes is hindered by copper adding effectively, which is favorable for photocatalytic performance. 5%CuO/TiO2:ZrO2 exhibits the highest photocatalytic activity and the degradation degree of methyl orange (MO) reaches more than 99% after 3h. Photocatalytic experiments confirmed that our catalysts displayed highly efficient and durable activity for the photodegradation of methyl orange under visible light.