Full dense and highly pure TiAl/Ti5Si3 in situ composite was successfully synthesized by reactive synthesis from the powder mixtures of Ti, Al and Si. The reaction process was investigated in detail by the X-ray diffraction analysis (XRD) and differential scanning calorimetry (DSC). The microstructural characteristics of the TiAl/Ti5Si3 in situ composite were also studied by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The results show that the as fabricated composite possesses three phases, namely, TiAl, Ti3Al and Ti5Si3. The matrix phases are mainly equiaxed TiAl with a minor lamellar Ti3Al phase. Ti5Si3 particles with size less than 1 μm are distributed uniformly in matrix grains as a reinforcing phase.