In the present study, in situ reaction technique has been employed to prepare AA5052 matrix composites reinforced with different vol. % of ZrB2 particles (i.e., 0, 4.5, and 9 vol. %). Composites have been characterized by X-ray diffraction (XRD) to confirm the in situ formation of ZrB2 particles in the matrix. Optical Microscopy (OM) studies reveal the refinement of aluminum-rich phase due to the presence of ZrB2 particles. Scanning electron microscopy (SEM) studies reveal size and distribution of ZrB2 particles while transmission electron microscopy (TEM) reveals the presence of dislocations in the matrix around ZrB2 particles. Hardness and tensile testing of composites have been carried out at room temperature to evaluate the mechanical properties. The results reveal the improvement in hardness and strength with increased amount of ZrB2 particles. Strength of AA5052/ZrB2 in situ composites has been analyzed by various strengthening mechanism models. The analysis revealed that Orowan and Solid solution strengthening mechanisms are the predominant mechanism for high strength composites. Theoretical yield strength is about 6–10% higher than the experimental values due to clustering tendency of ZrB2 particles.