In situ intermetallic matrix composites were fabricated by an MA–PDS process with a matrix of Fe–28 at% Al and volume fractions of particle TiB 2 formulated at 0, 5, 15, and 25%. Mechanical alloying was carried out using a vibratory mill. During the mechanical alloying, Al, Ti, and B became fully embedded to the Fe lattice. Mechanically alloyed powders were sintered in a plasma discharge sintering system. As a result, Fe 3Al matrix and TiB 2 particles were successfully synthesized by this in situ process. The tensile properties of the binary alloy were significantly improved without any loss in tensile elongation. The composite also had improved tensile strength. However, composites that contained a high volume fraction showed poor tensile properties due to the presence of micro pores existed within the microstructure.