Binary CuO/ZnO and ternary CuO/ZnO/Al2O3 Catalysts have been rapidly synthesized in a multimode microwave oven by the homogeneous precipitation of aurichalcite and hydrotalcite-like precursors using urea hydrolysis. For purposes of comparison, the same catalysts were prepared under conventional heating. The corresponding metal nitrates were mixed with various amounts of urea to yield different urea/(Sigma M+) molar ratios. The precipitation proceeded stepwise, copper being the first metal to be hydrolyzed. It was found that the higher the urea content, the higher the alkalinization of the solution, an effect which favored the precipitation of Zn (II) (the most pH dependent metal), and in turn, the synthesis of aurichalcite and hydrotalcite-like precursors. Microwave-synthesized catalysts presented similar characteristics to those obtained under conventional heating, but in considerably reduced aging times. Microwave radiation proved to be more efficient than conventional heating under harsh conditions of precipitation, i.e., lower molar ratios of urea with respect to the metal cations in the solution. (C) 2009 Elsevier B.V. All rights reserved.