Abstract-Present day three way catalysts operate in contact with exhaust gases whose temperature is as high as >1000°C, so the problem of developing thermally stable catalytic compositions is still topical. A series of Al 2 O 3 -Ce 0.75 Zr 0.25 O 2 composites containing 0, 10, 25, and 50 wt % Al 2 O 3 has been synthesized by direct precipitation. The as prepared composites and those calcined in air at 1000 and 1100°C have been charac terized by BET, X ray diffraction, transmission electron microscopy, and temperature programmed reduc tion methods. The composites aged at 1050°C in a 2% O 2 + 10% H 2 O + 88% N 2 atmosphere have been used to prepare monolith catalysts, and the oxygen storage capacity (OSC) of the latter has been measured using a gas analysis setup. As the proportion of Al 2 O 3 in the composite is raised, the mixing uniformity and degree of dispersion of Ce x Zr 1 -x O 2 -δ particles increase, their chemical composition becomes homogeneous, and the amount of cerium involved in oxidation and reduction increases.