In this study, FeAl2 and Fe2Al5 intermetallic alloys were prepared by conventional casting technique. In order to study their structural stability the alloys were subjected to high-energy ball milling process for 1, 2.5, 5 and 10 h. The structural and chemical characterizations were conducted by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and differential scanning calorimetry. After 10 h of milling, the experimental results indicated a phase transformation from FeAl2-triclinic phase to Fe2Al5-ortorrombic structure. This phase transformation is characterized by a change from low to high symmetry systems.