A powder blend of Ti, SiC and C at a molar ratio of Ti:SiC:C=3:1:1 was compacted into cylinder and sintered in vacuum for the synthesis of Ti 3 SiC 2 . The microstructure of synthesized Ti 3 SiC 2 showed unique morphology. Variation in phase and microstructural morphology with temperature during sintering was investigated by X-ray diffraction analysis and a scanning electron microscope equipped with an energy dispersive X-ray analyzer in order to elucidate reaction mechanism. Two kinds of powder blends, Ti/Si and Ti/C, were also compacted and sintered to confirm the effect of diffusion of Si and C atoms into Ti particles on the morphological change of Ti particles. As a result, we proposed the progress of synthesis as follows: (1) Si and C atoms start to diffuse into Ti particles from SiC and C particles over 1023K, (2) the diffusion of Si and C atoms is enhanced rapidly over α/β phase transition temperature of Ti, which results in the formation of shell structure having ruffled surface composed of Ti 5 Si 3 and TiC on Ti particle surfaces, (3) the shell grows and joins together with neighbor ones and pure Ti core in Ti particles reduces in size, (4) Ti 3 SiC 2 is formed by the reaction of Ti 5 Si 3 with TiC over 1623K, (5) finally, Ti 3 SiC 2 with TiC is synthesized over 1823K. The joined shell structure having ruffled surface formed during sintering remained after the formation of Ti 3 SiC 2 , which resulted in the formation of the unique morphology.