In this work, preparation of nanocrystalline Ni₃Al-based alloys by mechanical alloying process followed by hot-pressing consolidation is reported. Ni75Al20Co5 and Ni70Al25Co5 elemental powder mixtures were subjected to ball milling. Subsequently, the milling products were sintered at 1000^oC under a pressure of 7.7 GPa. The powders and the consolidated pellets were investigated by X-ray diffraction. The results obtained show that the milling products were in both cases supersaturated solid solutions Ni(Al,Co) and that during hot-pressing consolidation they had transformed into nanocrystalline Ni₃Al-based intermetallic compounds. The microhardness of the produced Ni₃Al-based alloys is 920 HV0.1 in the case of Ni₇₅Al₂₀Co₅ composition and 1030 HV0.1 in the second case. The density of compacted materials is close to the theoretical value and their open porosity is negligible.

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