Abstract: The mixture of pure nickel and aluminum powders in the composition of Ni50AI50 was subjected to high energy ball milling. The high energy ball milling to 30 h resulted in the formation of a nanocrystalline NiAl with a grain size of about 10 nm. The as-milled NiAl powder was hot-pressed and the compact with a density of 90% was obtained. It was showed that heating to900℃ and holding for more than 2 h failed to induce the coarsening of the fine nanocrystalin the material, the tendency of grain growth was weak. Compression testing showed that thecompression ductility at room temperature reached about 7%. The ductility increased with theexperimental temperature while the strength decreased drastically at elevated temperature.