In this study, the fabrication and structural characterization of amorphous/nanocrystalline Al9FeNi/Al3Ti phase has been performed. In this regards, milling and annealing processes were applied on Al80Fe10Ti5Ni5 (at. %) powder mixture for different periods of time. The prepared samples were characterized using X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM and TEM) and differential scanning calorimetery (DSC). According to the results, supersaturated solid solution, nano crystalline Al9FeNi/Al3Ti (with average crystallite size of about 7 nm) and amorphous phases indicated three different microstructures which can be formed in Al80Fe10Ti5Ni5 system during milling process. The formed supersaturated solid solution and amorphous phases were unstable and transformed to Al9FeNi/ Al3Ti intermetallic compound during annealing process. It is shown that, Al9FeNi phase in Al9FeNi/Al3Ti intermetallic compound can decompose into Al3Ni, Al13Fe4 and liquid phases during a reversible peritectic reaction at 809 degrees C. (C) 2016 Elsevier B.V. All rights reserved.