Ti2AlC/TiAl composites with the addition of niobium were prepared by spark plasma sintering using titanium, aluminum, niobium elemental powers and TiC particles as reactants. The experimental and analytical studies on this kind of material concentrated on the relationship between reinforcement phase and mechanical properties. The Ti2AlC/TiAl composites with 5% niobium exhibit high mechanical properties. The three-point bending strength and fracture toughness reaches as high as 915MPa and 23 MPa·m1/2, respectively. It is found that the in-situ reaction occurs at 1100°C with the addition of niobium at the interface between the TiAl matrix and original reinforcement TiC. Further XRD results indicate that the difference in the reinforcement phase from TiC to Ti2AlC is one of the most important origins to the variation in mechanical properties.