TiAl/Ti2AlC in situ composite was successfully fabricated by hot-press-assisted reaction process from the mixture of Ti, Al and carbon black. The phase formation and transformation were investigated in detail by X-ray diffraction (XRD) and the morphology characteristics were also studied by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The results show that when the mixed powders were hot pressed at 1300 °C for 1 h, full dense and highly pure TiAl/Ti2AlC composite was synthesized. The TiAl was the matrix phase and the in situ synthesized Ti2AlC was reinforcing phase. The reaction process was also discussed.