This work aims to describe the formation of intermetallics in Ti-Al and Fe-Al systems during ultra-high energy mechanical alloying process developed by authors. Although both systems tend to form aluminides, the formation of the phases during mechanical alloying is different. It was found that TiAl38 (in wt.%) powder mixture forms dual-phase TiAl/Ti3Al structure, which is consequently transformed to almost single-phase TiAl structure as the duration of mechanical alloying increases. On the other hand, FeAl32 (in wt.%) powder mixture formed ordered FeAl phase in the early steps, which was consequently changed to disordered solid solution after longer milling.