In this study, the authors prepared a series of technologically significant Fe1 -xAlx (0.2 ≤ x ≤ 0.6) alloys by two distinct methods: (a) arc melting and (b) ball milling and compared their structural and magnetic characteristics using XRD and VSM. Regardless of the synthesis method, structural analyses show that a FeAl alloy phase forms in both situations. Although FeAl alloy is formed using both processes, the diffraction patterns are indeed very different. In samples prepared by ball milling, the peaks are substantially wider than in samples obtained by arc melting. This is mostly due to the development of nanostructured disordered FeAl alloy during ball milling of the material. Aside from this, the existence of an Aluminum peak in a sample obtained by arc melting shows an unequal distribution of Al into the Iron matrix, whereas in a sample prepared by ball milling, Al is completely dissolved into the Fe lattice. Magnetic data indicate that the arc melted process favors the nonmagnetic FeAl alloy phase, whereas the ball milled method favors the weakly magnetic FeAl alloy phase. The existence of weak magnetism in a ball-milled sample is explained by considering the system's degree of nanocrystallization and disorder.