Titanium diboride powders were prepared through a sol-gel and boron carbide reduction route by using TTIP and B4C as titanium and boron sources. The influence of TTIP concentration, reaction temperature and molar ratio of precursors on the synthesis of titanium diboride was investigated. Three different concentrations of TTIP solution, 0·033/0·05/0·1, were prepared and the molar ratio of B4C to TTIP varied from 1·3 to 2·5. The results indicated that as the TTIP concentration had an important role in gel formation, the reaction temperature and B 4C to TTIP molar ratio showed obvious effects on the formation of TiB2. Pure TiB2 was prepared using molar composition of Ti : B4C = 1 : 2·3 and the optimum synthesis temperature was 1200°C. © Indian Academy of Sciences.