The present work is aimed at preparation and detailed characterization of the Pd-Rh/γ-Al2O3-ZrO2 composition used as a component of three-way catalysts. Physicochemical properties, such as specific surface area, morphology, secondary structure, dispersity and chemical state of active components, and thermal stability along with catalytic activity were studied within this research. Textural parameters of the samples were examined using low-temperature nitrogen adsorption. Analysis of the morphology and secondary structure was performed by means of electron microscopy. Concentration of metals located on the surface and accessible for the reagents was estimated using test reaction of ethane hydrogenolysis. Method of X-ray photoelectron spectroscopy was applied to investigate the chemical state of active components. Catalytic performance and thermal stability of the samples were tested in a prompt thermal aging regime using CO oxidation reaction as a criterion for in situ characterization of the catalyst state. It was found that both these characteristics strongly depend on the nature and composition of the precursors used.