Nanocomposite films of titanium nitride in either boron nitride or silicon nitride matrices were prepared by reactive sputtering of titanium diboride or titanium disilicide targets in a nitrogen plasma. These films were expected to have high dielectric constants and in the case of the silicon nitride matrix high hardness. The films were characterized by a variety of physicochemical techniques including photoelectron spectroscopy, Rutherford backscattering spectroscopy, RBS, and transmission electron microscopy. The films derived from titanium diboride incorporated oxygen as an inadvertent impurity in the form of titanium monoxide and dioxide. A silicon oxynitride underlayer is suggested by the RBS analysis of the silicon nitride based film, apparently arising from exposure of the native oxide on silicon to the nitrogen plasma. Capacitance measurements of the films showed moderately high dielectric constants of about 30–60 and a hardness of 11 GPa for the silicon nitride nanocomposite.