The synthesis of nanocomposite coatings is described in this paper. The nanocomposite feedstock powders are synthesized using mechanical milling, and the characteristics of the milled powders, i.e., morphology, agglomeration behavior, powder size, grain size and structural evolution during milling, are analyzed using X-ray diffraction, SEM and TEM. Using high velocity oxygen fuel (HVOF) spraying, the nanocomposite coatings are sprayed, and the microstructures and properties of the resulting coatings are characterized.