Intermetallic compounds have certain properties that distinguish them from other intermetallic compounds. These properties include shape memory, compatibility with body environment, super elasticity property, high toughness, appropriate tribology behavior and high corrosion resistance. Given their properties, Ni-Ti intermetallic compounds are extensively used in the medical industry, aerospace industry and surface engineering. Ni-Ti system has 3 intermetallic compounds including Ni3Ti, NiTi NiTi2. NiTi intermetallic compound has received sufficient attention in different studies but the other two compounds seem to be partially neglected in previous research. Several methods such as metallurgy powder, SHS, mechanical alloying and explosive shock are used to produce Ni-Ti intermetallic compound. Mechanical alloying has recently been introduced as one of the latest methods for producing Ni-Ti alloys in powder form and as an alternative to conventional melting and casting techniques and SHS. One advantage of this method is the production of nanostructure materials. Despite some limitation, because of low production cost and simple process, mechanical alloying (MA) is one of the best methods for making and production intermetallic compounds. Firstly, this study investigated production of nanostructure Ni75Ti25 powder through mechanical alloying using two kinds of high-energy planetary ball mill and attritor under argon atmosphere. Microstructure investigations were made by X-ray diffraction (XRD), Scanning Electron Microscope (SEM), thermal analysis and microhardness surveys. The results showed that alloying Ni75Ti25 powder mixture leads to the formation of solid solution and some Ni3Ti phase. The mechanism for the formation of this compound begins by the formation of layered structure of raw materials and titanium atoms in nickel dissolution. Continuing process of supersaturated solid solution Ni3Ti structure is provided. After heat treatment higher order Ni3Tiand greater presence of this compound will be observed. Super lattice peaks in structure of powder do not occur in any parts of the mechanical alloying and heat treatment process. Initial development of Nickel-Titanium compounds has been caused due to their shape memory property, super elastic behavior, energy absorption capability and biocompatibility. But research in the last two decades has indicated that these compounds resist abrasion, erosion, corrosion, cavitation and erosion corrosion resistant as well. As such, this study also investigated the coating of a powder mixture Ni75Ti25. Atmospheric plasma spraying (APS) method was used to create intermetallic coatings of nickel - titanium on carbon steel. The given powder was grinded for 2 hours prior to spraying. Spray process was used to perform 4 different currents (Amp). The results indicated that Ni3Ti, NiTi2 intermetallic phases, Nickel and small amounts of titanium oxide were found in all coatings. With higher current, fewer intermetallic compound formations were made leading to different properties in coatings. Moreover, the coating created with high current was denser than other coatings and having better adhesion in substrate. It was also found that harder coating had lower resistance against vickers intrusive and cracked sooner. Therefore, they have lower fracture toughness. Keywords: Ni-Ti intermetallic compounds, Mechanical alloying, Nanostructure Materials, APS