Bulk specimen containing Ti 3 SiC 2 , TiSi 2 and TiC was prepared through an in situ spark plasma sintering/solid-liquid reaction powder metallurgy method using the Maxthal 312 (nominally-Ti 3 SiC 2 ) powder as starting material. The reaction mechanism, phase constituents and evolution of microstructure were systematically investigated by X-ray diffraction (XRD), optical microscopy, scanning electron microscopy (SEM) equipped with energy dispersive spectroscopy (EDS) system, transmission electron microscopy (TEM), Raman spectroscopy, differential scanning calorimetry (DSC) and Vickers microhardness testing. Phase analysis and microstructural characterization revealed that the bulk sample contained binary ancillary phases possibly due to incomplete reaction and/or Si evaporation. The deformed microstructure around the indents revealed evidence of plasticity, intrinsic lubricity and toughening. The Microstructural and orientation relationships between the phases contained in the bulk sample are reported.