Abstract A Fe 32 Cu 64 B 4 (FeCuB) alloy was obtained by using an induction furnace under an argon atmosphere. Parameters suitable in the casting processes like voltage, temperature and cooling times were optimized. Once the FeCuB alloy was melted and solidified, X-ray diffraction (XRD) and surface morphology analysis were performed through optical and scanning electron microscopy (SEM-EDX). The results showed that complete diffusion of the precursor elements (Fe, Fe2B, Cu) requires thermal homogenization treatments (2 and 4 hours) at 750° as suggested from phase diagram of FeCuB simulation. The XRD analysis revealed that the primary crystallization consists of a mixture of the fcc-FeCuB (79%) and bcc-FeCuB (21%), with a = 3.62Å, spatial group Fm-3m and a = 2.86Å, spatial group Im-3m respectively. Micrographic images show an average grain distribution of ∼ 135 µ m. Finally, long times of homogenization (4 hours) allow a greater uniformity and redistribution of grain boundaries, resulting in the formation of an equiaxed grain structure in the alloy.