AbstractThe microstructural evolution during mechanical alloying of Ti and Al powders has been investigated by X-ray diffraction, scanning electron microscopy (SEM)–energy dispersive spectroscopy, and transmission electron microscopy (TEM). Observations by SEM showed a progressive change of the powders' morphology as a function of milling time. Observations by TEM, performed on a sample milled for 20 h, revealed the simultaneous occurrence of amorphous zones and nanocrystalline domains. The observed amorphous phase is not the final milling product. After 34 h of milling it was possible to identify by TEM fcc (a=0·41 nm) nanocrystalline zones, with a mean size of about 10 nm. By irradiating the powder milled for 20 h with high density electron beams, a suddenin situcrystallisation took place. The crystallite (fcc with a=0·41 nm) size was between 0·1 and 0·5μm.MST/1281