In this paper, live types of ceria-zirconia modified alumina (CZA) were prepared by co-precipitation with supercritical drying (CPS), co-precipitation with common drying (CPC), sol-gel (SG), micro-emulsion (ME) and impregnation (IM) methods, respectively. The corresponding supported Pd-only three-way catalysts (TWC) were also prepared and evaluated in the simulative gasoline engine exhaust. The influence of different preparation methods on the physicochemical properties of CZA mixed oxide and its supported TWC was characterized by X-ray diffraction (XRD), N(2) adsorption/desorption and transmission electron microscopy (TEM) techniques. The redox behavior was investigated with H(2) temperature-programmed reduction (H(2)-TPR) experiments. The results reveal that the CZA mixed oxides derived from CPS and ME methods exhibit the relatively higher textural and structural properties as well as better redox behavior, which lead to the better catalytic activity and wider air-to-fuel operation window of the corresponding Pd-only three-way catalysts. Crown Copyright (C) 2011 Published by Elsevier B.V. All rights reserved.