Preparation of titanium diboride (TiB2) nanoparticles was carried out by volume combustion synthesis. TiO2. B2O3 and elemental Mg were mixed with 0-60% salt mixture of KCl, NaCl and CaCl2 with increment of 15% as a low melting temperature diluent. Compressed samples were synthesized in a tubular furnace at a constant heating rate under argon atmosphere. Thermal analysis of the process showed that the addition of the low melting temperature salts mixture led to a significant decrease in ignition and combustion temperatures. Synthesized samples were then leached by nitric and hydrochloric acids to remove impurities. The samples were examined by XRD, SEM and DLS analysis. The results showed the formation of fine deagglomerated particles with the addition of the salts mixture. The results revealed that 45% salts mixture had the smallest average particle size of about 90 nm. (C) 2011 Elsevier Ltd. All rights reserved.