This paper presents the experimental data on the synthesis of titanium diboride (TiB2) fine dispersed powder carried out in laboratory scale. TiB2 powder was prepared by the reduction of titanium dioxide with boron carbide and nanofibrous carbon in an argon atmosphere. The powders of TiB2 were characterized by X-ray diffraction (XRD), elemental analyses, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), low-temperature nitrogen adsorption, particle size analysis, simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC). The resulting material contains a single phase – titanium diboride. The particles of the powder were predominantly aggregated. The average size of the particles and the aggregates were 7.4–8.0 µm with a wide size of distribution. The specific surface values of samples obtained were 2.4–5.8 m2/g. The oxidation of titanium diboride began from the temperature of 450 °C. In this work, the optimal synthesis conditions were estimated: the molar ratio was TiO2:B4C:C=2:1:3 (according to stoichiometry), the temperature was 1600 °C, the process duration was 20–30 min.