This article presents the results of laboratory testing of the technology for the synthesis of composite carbon—titanium carbide/titanium diboride (C—TiC/TiB
2) 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 TiO
2, boron oxide B
2
O
3 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/TiB
2 and titanium oxycarbide TiC
x
O
1-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/МеВ
2 system.