Fe 3 Al intermetallic compound is an important class of materials because of a combination of its high tensile strength, low density, good wear resistance, ease of fabrication and low cost. It also has excellent oxidation, sulfidation and corrosion resistance at high temperature. These properties have led to the identification of several potential usages including structural applications and protective coatings in hostile environments. Two major problems that restrict the application of Fe 3 Al are poor low-temperature ductility and inadequate high-temperature creep resistance. These limitations can be overcome by introducing ceramic particles as reinforcements. The goal of this work is fabrication of Fe 3 Al intermetallic compound with Al 2 O 3 reinforcement via mechanochemical process. The phase transformation and microstructural characterization during mechanochemical reaction were investigated by X-ray diffractometery (XRD), scanning electron microscopy (SEM), Transmission electron microscopy (TEM) with an energy dispersive spectrometer (EDS) attached, and thermal analysis (DTA).Mechanochemical behavior of different Fe, Al, and Fe 2 O 3 powder mixtures to fabrication of Fe–Al 2 O 3 , Fe 3 Al–57 vol.% Al 2 O 3, Fe 3 Al–30 vol.% Al 2 O 3 was studied according to the calculated adiabatic temperature of reactions, vial temperature measurement during milling, and structural investigations. Fe 3 Al–57 vol.% Al 2 O 3 and Fe 3 Al–30 vol.% Al 2 O 3 nanocomposite powders were compacted and then sintered at 1400 ? C for 1 h. The consolidated Fe 3 Al–57 vol.% Al 2 O 3 art had an ultrafine and homogeneous structure without "core-rim" feature consisting of Fe 3 Al and Al 2 O 3 phases. The consolidated Fe 3 Al–30 vol.% Al 2 O 3 art had a homogeneous and interconnected network of Fe 3 Al matrix. In addition, Fe 3 Al–30 vol.% Al 2 O 3 was also fabricated by mechanical alloying of Fe, Al, and nano-Al 2 O 3 in order to compare the effect of the addition route of Al 2 O 3 phase in Fe 3 Al matrix on sintering behavior and mechanical properties. The results showed that the Fe 3 Al–30 vol.% Al 2 O 3 fabricated through mechanochemical process had higher three-point fracture stress and hardness than Fe 3 Al–30 vol.% Al 2 O 3 fabricated by addition of Al 2 O 3 nanopowders