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The NiO/TiO2 composite films with the NiO content of 3 %, 5 %, 10 %, 13 %, 15 % and 20 % were prepared by mechanical coating technology and subsequent oxidation process. The composition and microstructure of the films were analyzed by X-ray Diffraction (XRD), scanning electron microscope (SEM), and energy dispersive spectroscopy (EDS). The photocatalytic activity was evaluated and the effects of the content of NiO on microstructure and photocatalytic activity of the films were studied. The results show that NiO particles are dispersed in the Ti coatings, and the NiO concentration in the inner layer of the coatings is higher than in the outer layer. With the addition of NiO in the NiO/Ti coating, the ductility is deteriorated and the thickness is reduced of the NiO/Ti coatings. The films with NiO/TiO2/Ti composite microstructure are obtained by the oxidation of NiO/Ti coatings. Photocatalytic efficiency of the films is obviously enhanced with the help of the p-n junction heterostructure in the NiO/TiO2 films. The optimum content of NiO is about 13 %, and the degradation rate of methyl orange solution reaches the maximum value of 88.44 %. DOI: http://dx.doi.org/10.5755/j01.ms.24.4.19266