Ti 3 SiC 2 is synthesized by self-propagating high-temperature synthesis (SHS) of elemental titanium, silicon, and graphite powders. The reaction paths and structure evolution are studied in situ during the SHS of the 3Ti+Si+2C mixture by time-resolved X-ray diffraction coupled with infrared thermography. The proposed reaction mechanism suggests that Ti 3 SiC 2 might be formed from Ti-Si liquid phase and solid TiC x . Finally, the effect of the powders starting composition on the Ti 3 SiC 2 synthesis is studied. For the investigated initial mixtures, TiC x is always formed as a major impurity together with the Ti 3 SiC 2 phase.