The present study characterized NbS i2–Al2O3 nanocomposite powders plasma-sprayed on Ti–6Al–4Vsubstrates. The powders were agglomerated to obtain suitable particle sizes for spraying. The agglomerated powders were then plasma-sprayed using atmospheric plasma spraying. The structural transformations of the powders along with the morphological and mechanical changes of the coatings were examined by X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy, transmission electron microscopy, and hardness testing. The results showed that after plasma spraying, the grain size increased, and the lattice strain decreased. However, the grain size of this compound after spraying was still in the nanometer range. The coating was uniform and exhibited good adhesion to the substrate. The microhardness and fracture toughness of the nanocomposite coating were higher than those of a nanostructured NbS i2 coating. The present study studied characterized as NbS i2-Al2O3 nanocomposite powders plasma-sprayed on Ti-6Al-4Vsubstrates. The structural units of the blast have been obtained as particle sizes for spraying. The structural transformations of the agglomerated powders were then plasma-sprayed powders along with the morphological and mechanical changes of the coatings were examined by X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy, transmission electron microscopy, and hardness testing. The results was that after plasma spraying, the grain size increased, and the However, the grain size of this compound after spraying was still in the nanometer range. The coating was uniform and cited good adhesion to the substrate. The microhardness and fracture toughness of the nanocomposite coating were higher than those of a nanostructured NbS i2 coating.