The synthesis of the delafossite phase CuAlO2 using the Pechini method was investigated. Powder X-ray diffraction data showed that pure, single-phase samples were obtained after only 3 h heating at 1100 degrees C. CuAl2O4, which contains Cu(II) rather than Cu(I), was the dominant phase between 700 and 1100 degrees C. Conversion to CuAlO2 is promoted by the positive entropy change associated with the evolution of oxygen. No mixed Cu-Al oxide was formed below 700 degrees C. (c) 2013 Elsevier Ltd. All rights reserved.