The TiO2/ZnO was prepared by microwave heating method.Microstructure and catalytic properties of TiO2/ZnO were studied by using XRD and reaction test of photocatalytic degradation of methyl orange in solution.Using titania dioxide as activator,methyl red simulating waste water,and high voltage mercury lamp simulating sunlight,the degradation of methyl red by photocatalysis was studied and compared with that of TiO2/ZnO which was prepared by rubbing.The results indicated that TiO2/ZnO prepared by microwave heating method has the best photocatalytic properties.After 60 min illumination,at the recruitment of TiO2/ZnO was 0.5g/L,the decolouration rate of the methyl red could be arrived 100%.as the increase of initial concentration,the degradation ratio of methyl red was increased.