The aim of this research is to determine the proper concentration of Titanium Tetra IsoPropoxide (TTIP) and select the right temperature and time of calcinations for the synthesis of B4C-nano TiB2 composite Nano powder by the chemical precipitation method. For this purpose, first, solutions with TTIP molar concentrations of 0.1, 0.05 and 0.03 were prepared and the optimal molar concentration of TTIP was determined to be 0.05. Then, a diluted solution of distilled water and TTIP was mixed with Isopropanol Alcohol containing B4C micropowder. In this mixture, Titanium Hydroxide nanoparticles were initially synthesized and then, to convert the Ti(OH)4 to TiB2, the above mixture were calcined in a furnace, under Argon atmosphere. The calcination process was carried out at temperatures of 750, 1000 and 1250 ºC. It was observed that the most suitable temperature for the formation of the TiB2 phase is 1250 ºC and that the lower temperatures only lead to the formation of the TiO2 phase. It was also observed that, at the calcination temperature of 1250 ºC, the most appropriate time duration for the conversion of Ti(OH)4 nanoparticles to TiB2 nanoparticles is 30 minutes, during which B4C-nano TiB2 composite Nano powders form, with most of the TiB2 particle sizes being in the range of 30-60 nm.