Nanocrystalline TiN, VN and CrN have been synthesized by a thermal nitridation reaction between the corresponding metal powder and NH(4)Cl at 600 degreesC in an autoclave. X-ray powders diffraction (XRD) indicated that these nanocystallites had a NaCl-type structure with lattice parameters: a = 4.236 Angstrom for TiN, 4.133 Angstrom for VN, 4.145 Angstrom for CrN. Transmission electron microscopy (TEM) showed these products consisted of cubic nanocrystals. X-ray photoelectron spectroscopy (XPS) and thermogravimetric analysis (TGA) techniques revealed that all the products were almost pure nitrides. (C) 2004 Elsevier Ltd. All rights reserved.