In this study, a new coating process was developed using mechanical milling. The new coating technique was named the pre-milling coating process and was used for the formation of Fe-Al intermetallic coating on lowcarbon steel substrates. In this new coating process, AA7075 aluminum-alloy powders were milled for various periods (4 h, 8 h, 12 h, 16 h, 20 h, and 24 h) in a vial and then milled onto low-carbon steel for another 4 h to form a coating on the steel substrate. Local interrnetallic formation was analyzed with scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS) and X-ray diffraction (XRD). The XRD and SEM observations indicated the presence of compounds such as FeAl, Fe2Al5 and FeAL(3) at distances of 6 mu m, 16 mu pm and 25 mu m from the substrate surface, respectively. The results revealed that the best coating thickness distribution, pore content and microhardness values were produced by the formation of Fe-Al intermetallics after 16 h of pre-milling and 4 h of coating (for a total of 20 h milling time). Crown Copyright 2014 (C) Published by Elsevier B.V. All rights reserved.