This study investigates the microstructural evolution during mechanical alloying of Mg and Ni, and during subsequent heat treatments of SPEX milled powders. The mil領(lǐng) was performed under an inert argon atmosphere, employing two different ball-to-powder ratios (BPR): 10:1 and 20:1. It was observed that a large number of defects were produced during the ?rst hours of mil領(lǐng). These defects led to the amorphi- zation of part of the system, and promoted an extensive re?nement of the microstructure as well. Later on, the formation of the Mg2Ni compound due to the crystallization of the amorphous phase was observed. The microstructural details showed us that a possible complete sequence of phase transformations during mil領(lǐng) of pure Mg and Ni could be: Mgc +Nic Mgnc +Nic amorphous + Ninc +Mgnc amorphous +Ninc +Mg2Ninc Mg2Ninc, where c and nc stand for crystalline and nanocrystalline, respectively. On the other hand, subsequent heat treatments of the milled powder showed that the amorphous phase could also be transformed into Mg2Ni by heating. Finally, the knowledge of the evolution of the microstructure during mil領(lǐng) and annea領(lǐng) were combined to propose an optimal processing route to ef?ciently obtain the Mg2Ni compound.