The MoS2 powders was coated with Al2O3 ratio varying 5wt.% to 50wt.% content. Ni–MoS2/Al2O3 composite coatings were prepared by means of pulse electrodeposition in a nickel-plating bath containing MoS2/Al2O3 powder to be co-deposited. The dependence of surface morphology, microhardness and tribological properties of the composite coatings was investigated in relation to the Al2O3 ratio in MoS2/Al2O3 powder. The results demonstrate that the coating co-deposited with MoS2/50wt.%Al2O3 showed a compact and fine granular surface morphology; the highest microhardness and wear resistance. The hardness of Al2O3 is responsible for this improvement.