Hybrid Metal Matrix Composites (HMMCs) have gained wide applications in aerospace, marine, and domestic areas because of its significant properties relative to external forces and enabling environment. In present research work, Ni-alloy selected as a matrix and Al2O3 of 40–80 μm and TiO2 of 1–5 μm were selected as reinforcements. The composites were prepared by keeping 9 wt. % of TiO2 as unvarying and Al2O3 is varied from 3 weight % to 12 weight % in steps of 3 weight %. Induction furnace is used for the casting of composites and mixing is done by using mechanical stirring at 160 rpm for a time period of 5 min. The prepared composites are then tested for their tensile and hardness as per the ASTM standards. The Scanning Electron Microscopy was used for microstructural study. From experimentation, it was observed that increment in the weight percentage of Al2O3 with constant TiO2 increases the mechanical properties of hybrid composites and proper stirring improves homogeneity in the composite material. The test results show that the addition of Al2O3 up to 9 weight percent increases in tensile strength compared to Ni alloy and tensile strength slowly decreases with the addition of Al2O3 and that the hardness values are directly proportional to the weight percent of the addition of Al2O3 / TiO2.