In this study, Al–Ni–Ce–Fe–Cu alloy powders with composition of Al 87 Ni 8.5 Ce 3 Fe 1 Cu 0.5 (at%) were atomized and then subjected to mechanical milling for different hours. The consolidation of the mechanical milled powders was performed by using spark plasma sintering followed by hot extrusion. Microstructure analysis and mechanical properties test were employed to the powders and the bulk samples, respectively. XRD patterns and DSC curves indicated that amorphous and nanocrystalline microstructure was obtained after milling for 170h. Room temperature compression test showed that the as-extruded bulk sample made from 170h milled Al–Ni–Ce–Fe–Cu powders had fracture strength of about 780MPa, however, without any visible fracture deformation. In addition, the ductility can be significantly optimized by introducing 20wt% pure Al powder. The strengthening mechanisms of the bulk samples were discussed.