Nanocrystalline titanium carbonitride (TiCN) was successfully synthesized at low temperature (420 degrees C) via a chemical metathesis route using the source materials of TiCl4, CCl4 and NaN3, which are readily attainable. X-ray powder diffraction (XRD) indicated that the product was cubic TiCN with a lattice constant a = 4.244 angstrom. Transmission electron microscopy revealed that the crystals were composed of spherical particles with an average diameter of 13 nm. X-ray photoemission spectra analysed that the atomic ratio was in good agreement with the TiC0.2N0.8 stoichiometry. (c) 2005 Published by Elsevier B.V.