TiB 2 reinforced in-situ titanium aluminide matrix composite was made through reaction synthesis process using high purity elemental powders of Ti, Al, Cr, Nb and B. XRD of the synthesized block showed presence of mainly Al 3 Ti and TiB 2 phases. To obtain γ Ti aluminide based matrix, the material was homogenized in two phase region (α 2 +γ). Presence of γ phase matrix alongwith α 2 was confirmed through XRD, SEM and TEM. Uniform distribution of TiB 2 phase was confirmed through elemental mapping and by analyzing specimens of different locations. Differential scanning calorimetry of powder mixture showed presence of endothermic peak for Al melting and exothermic peak of Ti aluminide and TiB 2 formation.