Aluminide intermetallics are potentially useful structural materials-provided their brittleness can be reduced. One possible method is the refinement of grain size to the nanometer level. Measurements of the mechanical properties are required in order to confirm this. The preparation described here is a general solution-based strategy for the chemical synthesis of nanocrystalline aluminide intermetallics. The results of sample characterization are presented and a two-step formation of the aluminide phase proposed.