The quest for lightweight, oxidation-resistant, high temperature materials for applications in the aerospace industry has led to numerous investigations of aluminum-rich intermetallics of the type Al[sub 3]X (commonly referred to as the trialuminides), where X is usually Ti, Zr, Hf, V, Nb, or Ta. Metastable cubic L1[sub 2] phases have been synthesized in ternary Al-25Zr-xFe and Al-25Zr-xNi (x = 3 and 8) powders by MA starting from blended elemental powders. The degree of order increased with increasing MA time in both the alloy systems. Some differences in behavior were observed with variations in the amount of the ternary solute element. In the Fe-containing alloys, the degree of order was higher for the 3% Fe than the 8% Fe sample at all milling times. However, in the Ni-containing alloys, the degree of ordering was lower for the 3% Ni sample up to 10 h, and at longer milling times, the degree of ordering was higher for the 3% Ni sample than the 8% Ni sample. The degree of order increased significantly on annealing the powders at 500 C. The L1[sub 2] phases in all the four compositions investigated transformed to the equilibrium phases on annealing the powders at 900 C.