Single phase TiN and AlN films were prepared on a Si wafer from titanium tetra-etoxide and aluminum tri-butoxide solutions dissolved in ethanol and toluene, respectively, using an Ar/N 2 /H 2 radio-frequency (r.f.) inductive thermal plasma chemical vapor deposition (CVD) method. The films were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, measurement of electrical resistivity and Vickers microhardness. Factors affecting the formation of the films (lattice parameter, chemical composition, oxygen/carbon content, and deposition rate of the films) were examined in terms of the N 2 flow rate (2.5-4.5 slm), substrate temperature (300-700 o C), feed rate of the solution (0.025-0.3 ml/min), and the mole ratio of the alkoxide solution (1:1-1:3). The optimum conditions for preparation of TiN films produced a film 0.2-3 μm thick with an oxygen content of 8 at.% and a free carbon content of 4 at.%, showing an electrical resistivity of 370 μΩ cm. The optimum conditions for AlN films produced a film 0.3 μm thick containing 14 at.% oxygen and 8 wt.% carbon. The deposition rate of the TiN film was determined to be 30-35 nm/min. The Vickers microhardness of the TiN and AlN films was found to be 10+/-1 and 13+/-3 GPa, respectively.