This paper presents a synthesis of TiB2 powder via self-propagating high-temperature synthesis (SHS) method using a mixture of TiO2, B2O3 and Mg followed by acid leaching. In the acid leaching step, the MgO content in the SHS product was leached in different HCl concentrations. X-ray diffraction (XRD) analysis showed that when 9.3 M HCl was used, the leached SHS product was found similar to that of the commercial TiB2 powder. However, scanning electron microscopy (SEM) and BET surface area analysis revealed that the leached product was agglomerated and exhibited very high surface area. (c) 2006 Elsevier Ltd. All rights reserved.