The MoS2 powders were coated with Al2O3 (5 wt.%) through controlling hydrolysis of Al (NO3)3•9H2O. MoS2 powder coated with Al2O3 waswritten as MoS2/Al2O3 hereinafter. MoS2/Al2O3 powders were put into Ni plating electrolyte bath. Cetyltrimethylammonium bromide (CTAB)—the surfactant was also put into the bath. The experiment proves that MoS2/Al2O3 particles were absorbed onto the Ni plate. The amount of MoS2/Al2O3 deposited on Ni plate rises with the increasing concentration of MoS2/Al2O3 in the bath. The microhardness, micro-surface, phase and thetribological property of the MoS2/Al2O3 multi-plating coating were measured and analyzed. The performances of microhardness and wearresistance of the Ni-MoS2/Al2O3 composite are better than those of Ni-MoS2 composite.