This study focused on synthesizing AlNiCo and CoNi materials using a low-energy milling process. The aim was to explore the formation of low-energy phases in both systems, contrasting with the typical research on phases formed under high-energy conditions. In the Co-20 wt% Ni system, the phases Co0.75Ni0.25 and Ni were identified, as well as the FCC cubic phase of CoNi, using X-ray diffraction (XRD) with a molybdenum radiation source. The observed behavior aligned closely with the miscibility curve in the equilibrium phase diagram, which included a region of alloys with varying structures and similar compositions. A notable feature was the presence of a predominantly dispersed hexagonal Ni zone, consisting of nanoparticles. Transmission electron microscopy (TEM) was employed to observe the FCC CoNi phase, which displayed a specific arrangement. AlNiCo and CoNi alloys were successfully synthesized through mechanical alloying, incorporating equilibrium and non-equilibrium phases.