Ce0.95Zr0.05O2 nanopowders have been prepared by a standard Pechini-type sal-gel process and by using polymethyl methacrylate (PMMA) colloidal crystals as template. The effects of these different synthesis routes, on the structure and microstructural features of the nanopowders, were evaluated by using X-ray diffraction (XRD), scanning electron microscopy (SEM) and specific surface area measurements. For both preparation routes, the XRD analysis has shown that a cubic fluorite structure is formed with a crystallite size of similar to 45-50 nm. The SEM images indicate that the powder obtained by the sol-gel Pechini-type process, is constituted by aggregated nanoparticles with relatively uniform shape and size, whereas the powder synthesized as inverse opal exhibits the formation of macropores with a mean size of similar to 130 nm. The specific surface areas of the powder samples obtained by the Pechini-type sal-gel and inverse opal methods are similar to 56 m(2) g(-1) and similar to 90 m(2) g(-1) respectively. Additionally, the thermoluminescence cm signal of the synthetized samples has been measured in order to examine its potential application in the field of dosimetry of ionizing radiations. (c) 2012 Elsevier B.V. All rights reserved.