The analysis results show that by the selection of appropriate conditions, a metastable Ni- Ti-C powder could be obtained by nominal compositions of 50wt. %Ni, 40wt.% Ti, and 10wt.% C. A powder, suitable for HVOF spraying, with particle sizes ranging from -38 to 8 mm was sieved and classified. Coatings with an approximate thickness of 250 mm were deposited by HVOF spraying on to mild steel substrates, and the resultant microstructures were investigated. XRD showed that a self-propagating high-temperature synthesis (SHS) reaction had occurred in the powder particles during spraying. It also revealed that the principal phases involved in the coating were TiC and a Ni-rich solid solution; small quantities of NiTi, TiO2, and NiTiO3 were also present. SEM revealed that the coating had a splat-like morphology characteristic and that TiC was formed by nanoscale dispersion, with particle sizes ranging from 50 to 200 nm, with in solidified splats.