Mechanical alloying of Al - 25 at% X (X = Hf, Nb, Ta, Ti, Zr, and V) elemental powders was studied to synthesize L1(2) phase-trialuminides with nanocrystalline structure. The microstructural evolution and mechanical properties of the synthesized powders were investigated in order to correlate the possibility of the formation of L1(2) and nanocrystalline structures with the synthesizing techniques. Effects of ternary elements on the formation of L1(2) phase and the thermal stability were also examined.