In this work, the powder of nano structured Fe3Al intermetallic compound was mechanically alloyed from pure iron and aluminum powders using ball milling technique. The synthesized Fe3Al powder was full characterized using X-ray and selected area electron diffractometers, transmission electron microscope and laser light scattering method. The results show that after 50 h milling, aluminum is completely dissolved in iron and then forms disordered Fe3Al intermetallic with bcc structure. Through analyzing of X-ray diffraction patterns using modified Williamson-Hall technique, the crystallite size and lattice strain of 60 h milled Fe3Al powder were calculated as 8 nm and 2%, respectively. These results demonstrated good agreement with TEM microstructural observations from the particles. (C) 2015 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.