Abstract: ZnTiO₃-TiO₂ nano-composite photocatalytic materials were prepared via a Sol-Gel method and characterized by transmission electron microscope(TEM), X-ray diffractometry(XRD), UV-Vis spectrum and zeta(ζ) potential. The influences of light source and calcination temperature on the photocatalytic property of the nano-composite materials was investigated by decolorizing degradation of methylene blue(MB) solution as a probe. The results exhibit that the catalytic activity of the as-prepared material depends on the particle size, dispersibility in solution as well as the superficial charge. On the surface of the ZnTiO₃-TiO₂ obtained by calcinin at 600℃ for 3 h, which can disperse well in solution and has an average particle size of 60 nm and highest negative charge, decolorizing efficiency of MB solution was up to 93% under sunlight radiation for 7 h while the efficiency was just 82% under ultraviolet light radiation for same time radiation. Such efficiency can be maintained higher than 80% when the catalyst is repeatedly used for 4 times. The nano-composite material shows higher photocatalytic activity than pure TiO₂ and ZnO, and has preferable photocatalytic stabilization property under sunlight.