Silicon nitride nanofibers coated with titanium nitride particles are formed by deposition of TiO(OH)2 and Ti(O)2(OH)2 using controlled hydrolysis of TiCl4 followed by nitriding in an NH3 flow. The nitriding at 700–900°C permits the formation of 5 to 15 nm titanium nitride particles. The amorphous layer on Si3N4 fibers limits the nucleation of titanium nitride and thus the formation of continuous coatings. Titanium peroxyhydroxide Ti(O)2(OH)2 as a precursor is preferable for depositing titanium nitride coatings on silicon nitride fibers.