: In this research, Nickel-Aluminum-Silicon Carbide powder was produced using ball mill for thermal spray process. For this, 1 Kg of mixture of powder was mixed with 20 Kg steel ball, and milled. For determining the optimum conditions of powder for thermal spray process X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) were employed. These powders were coated on CK45 substrate by plasma spray process in different distances and current intensities. With microstructure and morphology study of coating, the optimum conditions of coating were determined. Results showed that Nickel-Aluminum obtained from ball mill, reacted during plasma spraying and Ni 2 Al 3 intermetallic compound and ?-Ni solid solution were formed. For more studies in microstructure transformation, the samples were heat treated. Cohesive strength of coating on substrate evaluated with “Interfacial Indentation Test” and then the results were compared with Cr 3 C 2 -NiCr coating. Results of microhardness tests showed that existing phases in plasma spray coatings, Had high hardnesses