Due to the increasing demand for lighter materials with enhanced properties, the upgrade of techniques to improve the production of high-performance composite materials is of great interest in modern technology. The microstructural and mechanical properties of spark plasma sintered aluminium based composites with ferrotitanium (TiFe) and silicon carbide (SiC) reinforcements were investigated. High energy ball milling technique was adopted to effectively disperse the particles SiC and TiFe reinforcements into the matrix of aluminium, and the admixed powders were compacted using spark plasma sintering technique. The specimens sectioned from the sintered compacts were analysed using an X-ray diffractometer (XRD), optical microscope (OM), and field emission scanning electron microscope (FESEM) to understand the microstructural features and phase evolution of the sintered composites. The mechanical properties of the composites were also investigated through hardness, nanomechanical and tribology tests. Results from the microstructural examinations conducted shows that the reinforcement particles were evenly dispersed within the aluminium matrix, as a result of the milling process. Furthermore, all the sintered composites had their microstructural features enhanced, but properties such as hardness, frictional coefficient, and elastic modulus were more enhanced in specimen reinforced with 2%SiC+2%TiFe particles. The reduced crystallite size recorded by the sintered specimens confirmed the effectiveness of the milling process, and powder metallurgy route adopted for fabrication.