Titanium diboride is one of the candidate materials for high temperature applications and also for control rod elements in high temperature reactors. This paper presents the experimental data on the composites of B 4 C-nano TiB 2 that were synthesized successfully by co-precipitation method at temperatures between 973 and 1523K. Titanium tetraisopropoxide, boron carbide and isopropanol were used as the precursor materials. The phase constitution and microstructure of B 4 C-nano TiB 2 during synthesis were investigated. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to determine phase and microstructure of TiB 2 -B 4 C composites. The DTA/DDTA and TG/ DTG results improve that the first exothermic reaction is TiO 2 phase and second exothermic reaction takes place at 1523K which is TiB 2 phase.