In the present work, a new micro- spherical SnO2/Zn2SnO4 via a refluxing method has been synthesized. The heat treatment of the product was carried out at 500 and 900oC for 1 h. The sample was characterized by X-ray diffraction (XRD), UV-Vis spectrophotometer and field emission scanning electron microscopy (FE-SEM). The SnO2/Zn2SnO4 sample was formed after heat treatment at 900oC for 1h. The average diameter of micro- spheres of about ~2.7 mm were obtained. The photocatalytic activity of the sample by decolorization of two dye mixture- methylene blue (M.B.) and methyl orange (M.O.) was evaluated under UV-Vis. irradiation. The result showed that the SnO2/Zn2SnO4 sample is capable to decolorize (M.B.) and (M.O.) in dye mixture solution.