Cobalt alkoxide suspension is obtained by heating a mixed polyalcohol solution of cobalt acetate in an oil bath at 170 degrees C. Thermogravimetric analysis is adopted to determine the chemical formula of the alkoxide powder in the suspension. With the suspension precursors, CoO/Co composite thin films are fabricated by electrostatic spray deposition and subsequent heat treatment in nitrogen. They are characterized by scanning electron microscopy, transmission electron microscopy and X-ray diffraction. Electron energy loss spectroscopy mapping is applied to determine the lateral two-dimensional chemical distribution of metallic Co in the nanocomposites. The thin film can deliver a high reversible capacity of 1182.1 mAh g(-1) at 70th cycle and retain 69.5% of the initial capacity at 10C. The in situ production of metallic cobalt and the unique hollow structure of the particles can account for the good electrochemical performance. (C) 2012 Elsevier B. V. All rights reserved.