In order to produce Mo-Si intermetallic compounds, pure molybdenum and silicone powders were mechanically milled. Furthermore, X-ray diffraction, heat treatment and mean particle size calculation, the optimum of milling time was obtained which it is 15 hour for this system. Due to small particle size, which is not suitable for thermal spray processing, chemical agglomeration with carboxy methyl cellulose (CMC) was carried out. Different concentrations of CMC was examined and 1wt% CMC chosen as the best concentration. By utilizing atmospheric plasma spray processing, feed stock powders sprayed on a copper substrate. Results indicate that during thermal spray process, MoSi 2 , Mo 5 Si 3 , SiO 2 and MoO 2 were synthesized. Tribological behavior evolution of coating was evaluated