This research reports on the microstructural characterization and nanomechanical evaluation of hybrid aluminium-based composite, fabricated by reinforcing pure aluminium matrix with zirconia (ZrO2) and ferrotitanium (TiFe) particles. The composites were consolidated using the spark plasma sintering technique, and the properties of the reinforced composites were examined and compared with pure aluminium samples fabricated using the same sintering parameters. The formation of new phases in the hybrid composites was ascertained using the X-ray diffraction technique, while the morphologies of the starting powders and as-sintered specimens were analysed using optical and scanning electron microscopes. Mechanical tests such as Vickers microhardness and frictional coefficient were determined to ascertain the respective strength and tribological performance. Nanoindentation test was also carried out to evaluate the nanomechanical properties such as penetration depth, elastic modulus, work indentation, and indentation creep. The results from this study revealed that mixing and sintering the admixed powders at sufficiently high temperature resulted in the formation of new phases which contributed to improved mechanical performance of the hybrid composites. The absence of pinning effect in loading and unloading curves from the nanoindentation test conducted confirmed the homogeneous dispersion of the reinforcement particles. Overall, the sample reinforced with 5% TiFe and 5% ZrO2 exhibited the most improved mechanical properties, while the unreinforced aluminium sample recorded the least mechanical and nanomechanical performance.