. Carbon steels are largely used in various applicatio however, their wear, corrosion and oxidation resistance are weak. To improve these properties, NiAl intermetallic coating can be used. Several methods have been made to produce NiAl coatings on different substrate. In these study nanostructured NiAl intermetallics coatings were generated on carbon steel by using mechanical alloying in ambient temperature and effect of process parameters was studied on the MA and formation of coatings. In this regard, was used the balls with 2, 4, 7 and 10 diameter and ball-to-powder weight ratio 5:1, 10:1 and 20:1. Milling time was between 60 and 600 min. Also, prepared samples after ball milling were subjected to annealing treatment at temperatures range of 400 °C, 500 °C and 600 °C. The effect of the annealing treatment on the structure and mechanical properties, wear resistance and crystal size of the NiAl coatings has been investigated. In order to optimize the coating properties was used TiC reinforcing in different weight percent (1,2,3,4 and5) and reported the best percent of TiC. Coatings were examined using X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM), microhardness, micro Scratch tester, roughness measurements and wear resistance. The results showed that the best coating was formed by using balls with 4mm diameter and ball-to-powder weight ratio 10:1 and 480 min milling time. With increasing milling time, coating thickness increased up to 470µm and hardness up to 970Hv and decreased crystal size to 23 nm. Annealing treatment in 600°C/ 90min improved the coating wear resistance, adhesion and microhardness properties due to the formation of NiAl intermetallic compound. By using 2% reinforcement, the attainable thickness, adhesion and wear resistance of coating were increased. Keywords : Coating; NiAl Intermetallics; Mechanical alloying; Annealing treatment ; Nanostructured materials; Composite; Wear