The TiO2 microspheres, ZnO microspheres and TiO2/ZnO composite microspheres were obtained by Sol-gel method and hydrothermal method with Carbon microspheres as a template. The samples were characterized by SEM and X-ray diffractometer. The result indicates that TiO2 microspheres, ZnO microspheres and TiO2/ZnO composite microspheres were obtained and the diameter of them were 5-10 μm. The photocatalytic properties of the obtained photocatalyst on methylene blue solution and lake water were studied under UV light and the sunlight. Photocatalytic experiments have shown that among the three microspheres, the TiO2 / ZnO composite microspheres have better photocatalytic activity.