TiO2-coupled NiTiO3 nanoparticles have been prepared by coprecipitation in aqueous medium followed by sintering. Powder X-ray diffraction (PXRD) and high-resolution transmission electron microscopy (HRTEM) were used to characterize the crystalline structure. The crystalline sizes of both TiO2 and NiTiO3 were estimated to be in the range of 40-50 nm. A noticeable optical absorbance in the visible range was observed by UV-vis diffuse reflection spectroscopy (DRS). The photocatalytic activities were evaluated in the degradation of methylene blue in aqueous solution. The results show that the TiO2-coupled NiTiO3 nanoparticles exhibit good photocatalytic activities under visible light irradiation. The NiTiO3 phase was found to be indispensable for photoabsorption and photocatalysis.