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The study investigates the preparation of high surface area, three-way catalysts (TWC)-like, ceria–zirconia mixed oxide. It is shown that under basic conditions cationic surfactants effectively incorporate into hydrous oxides of cerium and zirconium. The presence of cerium inhibits the action of alkyl-trimethyl-ammonium salts as true templating agents and there is no formation of a regular pore structure. The elimination of surfactants upon calcination gives rise to the formation of high surface area, fluorite-structured CeO₂–ZrO₂ solid solution characterized by a fairly good compositional homogeneity. Surface areas in excess of 230m²/g were obtained after calcination at 723K, which drop to ca. 40m²/g following treatment at 1173K.