In present study, the fabrication and structural characterization of nanocrystalline Al3Ti/Al-13(Fe, Ni)(4) intermetallic compound by means of melt spinning and subsequent annealing has been performed. For this purpose, melt spinning process was done in Al80Fe10Ti5Ni5 (at%) alloying system at different wheel speeds in the range of 20-50 m/s. To achieve the desired microstructure, the melt spun ribbons were annealed at temperatures between 300 and 600 degrees C. The prepared samples were characterized by X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM and TEM), differential scanning calorimetry (DSC) and nano-indentation (NI) techniques. During the melt spinning with a wheel speed of 50 m/s, a fully amorphous phase was formed in the Al80Fe10Ti5Ni5 alloying system. By annealing the produced amorphous phase, Al3Ti and Al-13(Fe, Ni)(4) intermetallic phases precipitated from the amorphous matrix. The fully amorphous phase has a hardness about 4.5 GPa, which increased to about 6.2 GPa after annealing process. (C) 2016 Elsevier B.V. All rights reserved.