In the present work, TiAl-based intermetallic matrix composite with second phase reinforcement as Ni-P-coated carbon and graphite powders were synthesized by mechanical alloying route. Graphite powder (20-30 mu m) and elemental carbon powders (1-5 mu m) were coated with Ni-P by the electroless coating technique, which was added to the elemental powder mixtures of Ti-48Al-1%Cr -1%Nb with 1% composition of either of the two. The powder mixtures were subjected to mechanical alloying at 300rpm up to 250h using toluene as a process control agent. The samples were collected after 25h duration and characterized. The formation of TiAl () and Ti3Al ( (2)) phases are confirmed by x-ray diffraction. The formations of these phases were found after milling for 75h in case of graphite addition and 100h in case of carbon addition in the intermetallic matrix. The mechanically alloyed samples milled for different extents of time were examined by a field emission scanning electron microscope (FESEM) and energy dispersive x-ray (EDAX) spectroscopy; the grain size was determined to be in the size range of 140-189nm for the mechanically alloyed mixture.