Characterization and Formation Mechanism of (Ni, Fe)3Al –Al2O3 Nanocomposite by Mechanical Alloying According researches, the nickel aluminides exhibits advantageous properties including high melting temperature, high tensile strength and yield point, low density, high hardness, good thermal stability and high creep resistance, good corrosion and oxidation resistance at elevated temperatures. These materials are particularly ideal as high temperature structural materials. The major barriers for the use of them as structural materials are their low toughness and ductility at ambient temperature. Recently much attention has been given to the investigation of ternary systems and ternary nanocomposites by mechanical alloying. It leads to the improvement of low ductility and toughness at ambient temperature.The aim of this research was to synthesis and characterization (Ni, Fe)3Al–Al2O3 nanocomposite by mechanical alloying (MA) and evaluating its formation mechanism. In first step (Ni, Fe)3Al intermetallic compound by mechanical alloying (MA) of Ni, Fe and Al elemental powder mixtures with composition Ni50Fe25Al25 was successfully synthesized. .