A complete range of mesoporous Ce1-xZrxO2 beads (x = 0-1) were synthesized by the nanocasting approach using porous polymeric beads as templates and crystalline Ce1-xZrxO2 nanoparticle sols as filling agent. The final beads obtained after calcination at 500 °C showed surface areas as large as 113 m2 g-1. According to scanning electron microscopy (SEM) and transmission electron microscopy (TEM) investigations the morphological features of the template beads are transferred to the oxide spheres. Wide-angle X-ray scattering (XRD) data and Raman studies of the samples calcined at 500 °C and 900 °C, respectively, indicate the compositional homogeneity as well as a systematic variation of the crystal properties. The ceria zirconia samples with intermediate compositions (x ∼ 0.5) were more stable towards crystal growth and loss of surface area. © 2006 Elsevier Inc. All rights reserved.