In the present work, hybrid surface composites (HSCs) were fabricated using aluminium 5052 alloy as base matrix and silicon carbide (SiC) and cerium oxide (CeO2) as reinforcement particles via friction stir processing (FSP) technique. Varying reinforcement ratios of SiC and CeO2 nano-powders, viz 100:0, 75:25, 50:50, 25:75, and 0:100 was used. Multi-pass FSP was employed to obtain improved dispersion of reinforcement particles. Results revealed the collaborative impact of SiC and CeO2 particles on the mechanical properties of the SCs, shedding light on the optimal ratios for achieving superior mechanical performance. The hybrid ratio of (SiC: CeO2) 75:25 was predominant in tensile strength enhancements with an ultimate tensile strength of 283 MPa compared to 269 MPa of BM while the percentage elongation increased to 21.6 compared to 18.8 in BM. The average microhardness also improved to 92 HV compared to 85 HV. These results emphasised on the importance of HSC fabricated using 75:25 ratio of SiC:CeO2 reinforcing particles.