The ceramic particle reinforcement process is one of the most utilized techniques to enhance the metal surface. The current investigation uses vanadium and niobium carbides to reinforce the AA6061 alloy using the friction stir process (FSP). The mechanical properties are evaluated using ultrasound and conventional compressive tests; furthermore, the microstructure and physical properties are carried out to show the effect of single and hybrid additives of ceramic particles on the surface composites of aluminum alloy. Scanning electron microscopy (SEM) is utilized to examine the presence and distribution of the reinforcement VC and NbC particles inside the composite matrix. The microstructure examination revealed a good dispersion and homogenized distribution of the reinforcement particles. The results indicated that reinforcement particles significantly enhanced the mechanical and physical properties. The VC and NbC particles play an important role in improving the surface hardening behavior and grain refinement by restricting grain growth during the dynamic recrystallization process in the FSP action. The hybrid composited AA6061/NbC + VC recorded an increase in the compressive stress, yield stress, and hardness of 25%, 20%, and 50%, respectively, relative to the base metal, in addition to a 55% decrease in the coefficient of the thermal expansion (CTE) was reported. Moreover, the hybrid composite AA6061/NbC + VC significantly affected the corrosion rate with a reduction of 45%.