Highly pure Ti2SC powder was synthesized by microwave hybrid heating a Ti/TiS2/C powder system in the temperature range of 200-1100 ℃. The effect of sintering temperature on the synthesis of Ti2SC was studied. For comparison, pressureless sintering (PLS) was used to synthesize Ti2SC powder from 1000 ℃ to 1400 ℃ for 15 min. By XRD, SEM, DSC and thermodynamics, the phase assembly, microstructure and reaction mechanism of samples were analyzed. The results indicate that the main phase graphite with small amount of Ti2SC was synthesized at 1400 ℃ by pressureless sintering. However, by microwave hybrid heating，at 400 ℃, Ti2SC phase was detected as a major phase and large amount of graphite existed. The peak of Ti2SC phase became strong together with weakening the peak of graphite at 800 ℃. At 1100 ℃, single-phase Ti2SC powder with the average size of 2-5 μm was achieved. In TiS2-Ti-C system, TiS2 reacted with Ti to form Ti-S compounds below 400 ℃, and Ti-S compounds reacted with Ti and graphite to produce Ti2SC at 400 ℃ and above.