An Al58Cu25Fe17 alloy composition was produced by conventional casting technique. In order to take advantage from the hydrogen-environmental embrittlement reaction, which affects these alloys, this research was carried out subjecting prealloyed powders to wet-ball milling. Through these experiments it has been possible to evaluate the particle size reduction as consequence of hydrogen fracture and milling energy. The morphological and structural characteristics of the samples were performed using x-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and transmission electron microscopy (TEM). The experimental results indicate that the samples with higher contents of humidity have a good particle size reduction. With the increment of milling time, the particle size was diminished even more reaching nanometer size scale.