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The use of advanced electron microscopy techniques to characterize both the bulk and near-atomic level microstructural evolution of catalyst materials during different dynamometer/vehicle aging cycles is an integral part of understanding catalyst deactivation. The study described here was undertaken to evaluate thermally-induced microstructural changes which caused the progressive loss of catalyst performance in a three-way automotive catalyst. Several different catalyst processing variables, for example changing the washcoat ceria content, were also evaluated as a function of aging cycle and thermal history. A number of thermally-induced microstructural changes were identified using high resolution electron microscopy techniques that contributed to the deactivation of the catalyst, including sintering of all washcoat constituents, γ-alumina transforming to α-, β-, and δ-alumina, precious metal redistribution, and constituent encapsulation.