Nanocrystalline titanium carbonitride (TiCN) was successfully synthesized at low temperature (420°C) via a chemical metathesis route using the source materials of TiCl 4 , CCl 4 and NaN 3 , which are readily attainable. X-ray powder diffraction (XRD) indicated that the product was cubic TiCN with a lattice constant a=4.244Å. Transmission electron microscopy revealed that the crystals were composed of spherical particles with an average diameter of 13nm. X-ray photoemission spectra analysed that the atomic ratio was in good agreement with the TiC 0.2 N 0.8 stoichiometry.