Abstract: The deposition capability of nickel on the surface of poly-α-methylstyrene microspheres was improved by combined treatment of ozone aeration and UV irradiation in aqueous ammonia. Surface properties of the treated film were investigated by X-ray photoelectron spectroscopy(XPS) and Fourier transform infrared(FT-TR) measurements. The samples were characterized by SEM. The results indicate that after ultraviolet joint ozone treatment, the surfaces of microspheres were oxidized, and the amine and amide groups are introduced on their surface. The images of SEM show the adhesion between microspheres and nickel-phosphorus films was improved after surface modification. This was attributed to amide which could chemisorb palladium ions to catalyze electroless nickel plating on the pretreated surfac