In this work we show that mechano-synthesis is a good method to prepare the FeSiB amorphous alloy starting from Fe, Si, B pure elements with relative atomic composition of 75, 15 and 10%, respectively. We have used a high-energy ball-milling system keeping the material under an Ar atmosphere. The evolution of the microstructure inside the grains is followed by X-ray diffraction and Mössbauer spectroscopy at room temperature. The dependence of crystalline size, lattice parameter and hyperfine parameters on milling time is discussed. Our results show that the milled samples obtained after 10 h of milling contained a bcc structure in the amorphous matrix. After 19 h of milling the sample became fully amorphous.