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Three-way catalysts with low content of Pd–Rh alloy particles used as active components were synthesized and studied. Monometallic and bimetallic mixed catalysts with corresponding precious metals loading were chosen as reference samples. The catalytic activity was tested in oxidation of carbon monoxide, hydrocarbons, and in nitrogen oxides reduction. The stability of the samples was estimated by prompt thermal aging in situ technique. Ethane hydrogenolysis testing reaction was used to determine the surface concentration of Pd and Rh, and to confirm the alloy formation. Photoluminescence and electron paramagnetic resonance spectroscopy were applied to clarify the possible reasons of deactivation and to elucidate the mechanism of stabilization. It was shown that Pd–Rh alloyed catalyst is characterized by comparable activity and enhanced stability. While the Pd and Rh particles of monometallic …