Nanostructured CuO thin films were prepared by spray pyrolysis of aqueous copper acetate solutions at temperatures over 200-300 degreesC range. The textural and structural properties of the films were determined by scanning electron microscopy, atomic force microscopy, X-ray diffraction spectroscopy and X-ray photoelectron spectroscopy (XPS). Although the sole crystalline phase detected in the film was CuO, XPS spectra revealed a more complex surface structure due to the presence of undecomposed copper acetate that can be easily removed by Ar+ ion sputtering. The heating temperature was found to have little limited effect on the particle size and thickness of the films, which, however, increased significantly increasing deposition time. The film with the smallest grain size exhibited an excellent electrochemical response in Li battery electrodes and was capable of supplying sustained specific capacity as high as 625 A h kg(-1) (50% greater than that delivered by bulk CuO and close to the theoretical capacity for the CuOdouble left right arrowCu reaction) upon extensive cycling. (C) 2004 Elsevier B.V. All rights reserved.