Atmospheric Plasma Spray (APS) is one of the most leading industrial techniques for protective coating, by improving the performance of parts in the thermal barrier, and wear resistance. Ni-Al alloys are very effective players in the field of design of protective coatings. Accordingly, mixed Al, Ni/Al, and Ni5Al powders were applied on 304stainless steel substrate to develop plasma sprayed coatings. The effect of different compositions on microstructure, microhardness, and porosity was measured. The microstructures of the as-deposited films were characterized utilizing X-ray diffraction (XRD), scanning electron microscopy (SEM), and microhardness measurements. The results showed the formation of two intermetallic compounds, namely: NiAl and Ni3Al. The existence of NiAl is inevitable in all samples, despite the amount of Ni-based alloys in mixtures, or even the atomic percentage of nickel, where the appearance of Ni3Al depends only on increasing the amount of the Ni-based alloy to 50 % percent in mixtures. As regards the steel substrate, the microhardness of the interdiffusion zone of the substrate has been significantly enhanced. Results have shown that the microhardness of the different tested coatings is increased directly with the increment of Ni-based percentage in the coating mixture. The average porosity of the plasma sprayed coatings has proven to be within the normal range.