Titanium diboride (TiB2) has attracted great interests for its excellent mechanical properties, chemical resistance and good thermal and electrical conductivities. So it is widely applied as cutting tool composites, wear resistant parts, metal melting crucibles and electrode materials. This paper presents synthesis of nano titanium diboride powders via sol-gel method using a mixture of TTIP and B4C as precursors. In the hydrolysis step, B4C to TTIP molar ratio varied from 1.3 to 2.5. Solution samples stirred well and after aging and drying process, they were heat treated in an argon atmosphere. X-ray diffraction (XRD) patterns and Scanning electron microscopy (SEM) analysis showed that the percentage of synthesized TiB2 increased gradually as the molar ratio of B4C to TTIP reached to 2.3, afterward increasing the B4C to TTIP molar ratio caused decreasing of titanium diboride percentage.