Air plasma spraying was utilized to deposit Ni 3 Al coatings on AISI-321 steel substrate. The deposited coatings were isothermally heat-treated at various temperatures from 500 to 800°C for 10, 30, 60, and 100 h. The x-ray diffraction analysis revealed NiO formation in Ni 3 Al at 500°C after 100 h, and the percentage of NiO increased with increasing exposure time and temperature. The hardness of the coating increased with the formation of NiO. The DSC test showed the formation of minor phases, Al 3 Ni and Al 3 Ni 2 , within the coating along with the major phase N i3 Al. TGA revealed a slowing down of the oxidation rate upon surface oxide formation. The pin-on-disk wear test on the as-sprayed and heat-treated coatings showed that wear rate and coefficient of friction decreased with an increase in the NiO phase content.