A feasible approach to fabricate an Al(Cu)-based hybrid nanocomposite reinforced with TiC and Al2O3 based on mechanical activation and post heat treatment was proposed. Structural and phase evolution during mechanical alloying were studied by employing X-ray diffraction (XRD), transmission electron microscopy (TEM), filed emission scanning electron microscopy (FESEM) and differential thermal analysis (DTA) techniques. Mechanical alloying method was used in order to formation of Al(Cu), TiO2/Al3Ti, Al4C3 powder. It was found that a powder mixture of Al(Cu), TiO2/Al3Ti, Al4C3 is formed after 30 h of milling. The XRD analysis showed that Al(Cu)/TiC-Al2O3 is synthesized after heat treating of powder mixture at 1000 °C for 1 h via reaction between Al3Ti, Al4C3 and TiO2. DTA analysis showed that Al(Cu)/TiC-Al2O3 cannot be synthesized without mechanical activation and only based on heat treating. It was shown that heat treating of the as-milled powder mixture for 50 h at 500 °C doesn’t lead to formation of Al(Cu)/ TiC-Al2O3 composite and a minimum temperature of about 1000 °C is needed for synthesis of Al(Cu)/ TiC-Al2O3 hybrid composite.