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Herein, a combinatorial approach is developed to conduct high‐throughput studies on the nanosecond pulsed laser‐induced dewetting phenomenon of bilayer Ag–Co metallic thin films. Laser irradiation results in the spontaneous rupture of these films in nanosecond timescale, forming bimetallic nanoparticles (NPs) through intermediate stages of hole formation and bicontinuous nanostructures. This approach utilizes bilayer thin films with thickness gradients in both Ag and Co layers (referred to as bigradient samples) while maintaining a constant overall thickness. The laser irradiation on such bigradient bilayer films facilitates control on Ag and Co ratio in the thin films, thus enabling material libraries of Ag–Co NPs covering a large compositional variation. The evolution of NPs with a correlation between NP diameter and interparticle spacings is further studied. The study reveals monotonic increase in NP size and interparticle spacing in Co/Ag bilayer arrangement, while an increase and subsequent decrease in the NP size is observed at 50% Ag in Ag/Co bigradient films. A transition from intermediate stage hole formation to bicontinuous nanostructures with changing composition is also observed. These changes in intermediate stage morphologies and dewetting mechanism are attributed to variation of the free energy of the bilayer system dominated by intermolecular interaction forces.