The PS microspheres with the smooth surface and uniform size were prepared by the dispersion polymerization technique in the presence of PVP, using 2-methylpropionitrile as initiator, anhydrous alcohol as the dispersion medium . After surface treatment, PS / Ni composite particles with characteristic of high conductivity were prepared by chemical plating process. The results show that the surface morphology and phase change of PS microspheres before and after nickel plating were studied and the effect of preparaction process on conductivity of composite was analyzed. The results show that the optimized process is: PS / NiCl₂ ·6 H₂O = 4 : 7 ( mass ratio) ,complexing agent dosage is 2 g, NH₃ ·H₂O dosage is 30 mL.