The effects of annealing on microstructure and mechanical properties of bulk nanocrystalline Fe3Al based alloy with 10 wt. % Ni prepared by aluminothermic reaction have been investigated. It was found that crystal structure of the alloy did not change after annealing at 600 and 800 °C, while it changed to ordered B2 and nanocrystalline grains orientations became random after annealing at 1000 °C. Average grain sizes of the alloy changed a little after annealing at different temperatures. The alloy after annealing had a large plastic deformation in compression at room temperature and the alloy annealed at 800 °C had the highest compressive yield strength of 1351 MPa. The alloy without annealing had much lower flow stress and good creep property in compression at 800 and 1000°C.