ZnO, CuO, and Cu0.05Zn0.95O nanoparticles have been prepared by a sol-gel method using poly(vinyl alcohol) aqueous solutions and metal nitrate precursors. The precursor powders were analyzed by thermogravimetry (TG) and differential scanning calorimetry (DSC). X-ray powder diffractometry (XRD), infrared spectroscopy (FTIR), and scanning electron microscopy (SEM) were used to characterize the structural and the chemical features of the nanoparticles. An average nanocrystallite size of 25-30 nm was obtained for ZnO and Cu0.05Zn0.95O and of 40 nm for CuO, as estimated by the Scherrer's equation. (C) 2008 Elsevier B.V. All rights reserved.