This article presents the results of laboratory testing of the technology for the synthesis of composite carbon—titanium carbide/titanium diboride (C—TiC/TiB2) material directly in course of electrolytic reduction of cryolite-alumina melts. After the preliminary standard treatment purposing the mixing of initial components—petroleum coke of different fractions, rutile titanium oxide TiO2, boron oxide B2O3 and binding agent—the cathode specimens were pressed to the specified sizes and thermally treated at the temperature of 1050 °С. Experiments with holding time of 5, 15 and 24 h during the electrolytic reduction process have demonstrated the acceptable wettability of cathode specimen surface. X-ray phase analysis and SEM-EDS-analysis have detected the presence of TiC/TiB2 and titanium oxycarbide TiCxO1-x within the volume of cathodes and on their surface. After 15 and 24 h experiments the aluminium layer with good adhesion to the surface was noticed on the cathode surface; which is indicative of wettability of the electrode with metal. This tested technology can be extended to the creation of wide range of composite products in the С—МеС/МеВ2 system.