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This paper explores phase formation and phase stability in free nanoparticles of binary alloys. A procedure for estimating the size and composition dependent free energies incorporating the contributions from the interfaces has been presented. Both single phase solid solution and two phase morphology containing interphase interfaces have been considered. A free energy scenario has been evaluated for two binary alloy systems Ag–Ni and Ag–Cu to predict the microstructure of the alloy nanoparticles at different size ranges as a function of composition. Both Ag–Cu and Ag–Ni systems exhibit wide bulk immiscibility. Ag–Ni nanoparticles were synthesized using the wet chemical synthesis technique whereas Ag–Cu nanoparticles were synthesized using laser ablation of a Ag–Cu target immersed in distilled water. Microstructural and compositional characterization of Ag–Ni and Ag–Cu nanoparticles on a single …