An attempt was made to produce nickel aluminides with fine microstructure from nanoscale nickel and aluminum powders produced by wire electric explosion (WEE). The powders were mixed and spark plasma sintered (SPS) for simultaneous reaction and densification of the material. Various mixing methods were tested to give the best homogeneity of the nanopowders mixtures. Utrasonic pre-treatment of the powders did not result in any positive effect on mixing homogeneity. Sintered compact contained NiAl and Ni3Al phases, showed fine grain size and unexpectedly high hardness possibly due to the presence of aluminum oxide in the starting nanopowders.