In this work, B4C-TiB2 nanocomposite powders were synthesized by mechanochemical method of B, C and Ti elements. Mixed powders with a theoretical composition were milled for 6, 10, 14, 20, 26, 32, 50 and 70 h. In order to complete the reactions, milled powders were heat treated at 800o, 1000o and 1200oC for 1 h. The morphology of powders was studied by SEM. Phase characterization, crystalline sizes were determined by XRD. Results showed that titanium diboride forms during the early stage of milling and after 70h of milling, the crystallite sizes become 7.5 nm. No boron carbide was detected in powders milled for 70h and after heating at 800oC and higher this phase appeared.