In this work, mechanochemical reduction of CuO/ZnO powder mixture by Al and C has been investigated. Powder mixture was milled up to 2011 in a planetary ball mill. X-ray diffraction, transmission electron microscopy, thermo gravimetric analyzer, and differential scanning calorimeter have been used to study products phases and activation of redox reactions took place during ball milling. Results showed that the highly exothermic reduction reaction caused by aluminum provided the required heat for the endothermic reduction reactions by carbon. Consequently, the oxide powders were entirely reduced during ball-milling process and alpha-brass Al2O3 nanostructured composite was obtained after 3 h milling. By utilizing the Scherrer's method, the mean grain size of the brass was found to be in the nanometer range which was later confirmed by TEM observations. (C) 2010 Elsevier B.V. All rights reserved.