Powder of Fe 63 Nb 10 Al 4 Si 3 B 20 (%at) alloy was processed by gas atomization to investigate the formation of novel microstructures due to the high cooling rates involved in this process. The ratio between the gas volumetric flow rate and the metal mass flow rate used was 0.23, and nitrogen was used as the atomization gas. The powder, with a median particle diameter about 120µm, was sieved in the granulometric size ranges of 5-20, 20-30, 30-45, 45-75, 75-106, 106-150, 150-180, >180µm, and then were characterized by X-ray diffratometry (XRD), differential scanning calorimetry (DSC), scanning and transmission electron microscopy (SEM and TEM, respectively) both equipped with energy dispersive spectroscopy (EDS). Powder in the range of 5-45µm contain α-Fe nanocrystals embedded in an amorphous matrix. In the size range of 45-150µm, the powder contains, besides α-Fe nanocrystals embedded in an amorphous matrix, particles of FeB and Fe 23 B 6 intermetallic phases. For the size range > 150µm, the powder showed particles with Fe-α nanocrystals embedded in an amorphous matrix and partially crystalline particles with Fe-α, FeNbB and FeB phases. The volume fraction of the amorphous phase decreased with the increase of the granulometric size range. The nanocrystallization of the powder in the smaller size ranges opens the possibility for the production of a bulk nanocrystalline deposit produced by spray forming and its application as a soft ferromagnet.