In Al-25Nb binary system, it was observed only formation of D0 22 Al 3 Nb intermetallic compound after 5hr milling but it was not observed formation of meta stable phase like L1 2 phase. In this state, D0 22 Al 3 Nb fabricated had nano sized grain of approximately 20nm. Ternary systems, transition metals such as Cr, Cu, Fe, Mn were added 6~12at.% as substitution of Al, showed formation of D0 22 Al 3 Nb like Al-25Nb binary system. In Al- l2Cu-25Nb system, it was observed that broad XRD pattern like amorphization of Al and not observed formation of D0 22 Al 3 Nb after 5hr milling. But there was mixed phase of a lot of amorphous Al and little D0 22 Al 3 Nb through TEM. In the states of unalloyed, 5~7hr milling time, those showed exothermic reaction at 35 0 ? C , which was formation of D0 22 Al 3 Nb like Al-25Nb binary system. With increasing milling time to 10hr, D0 22 Al 3 Nb was transformed to mixed phase of amorphous and nanocryatlline, having approximately 10nm grain but the meta stable Al 3 Nb was not fabricated by adding transition metals.