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In this study, we used the adsorption-induced segregation to control the performance of Pd–Ag2/Al2O3 catalyst. The main idea was to study the possibility to tune the structure of active sites and, consequently, the catalytic characteristics of Pd-Ag catalysts by using CO and O2 adsorption-induced surface segregation. The catalytic effect of this treatment was investigated in liquid-phase diphenylacetylene (DPA) hydrogenation.