CuC/Fe2O3 hollow hybrid spheres with the size of 3-5 mu m were successfully synthesized by a convenient hydrothermal method, using FeSO4 center dot 7H(2)O and CUSO4 center dot 5H(2)O as the starting materials and urea as the homogeneous precipitant. The samples were characterized by XRD, TEM, ED, SEM, EDX, IR and XPS measurements. XRD and XPS analyses indicated that the nanostructured materials consisted of CuO and alpha-Fe2O3. TEM and SEM measurements showed that the morphology of binary metal oxide was in the shape of hollow sphere. Careful observation from SEM measurements could find that CuO/Fe2O3 hollow microsphere shell was composed of uniform and dense metal oxide nanorods with about 20-40 nm in diameter and 100-200 nm in length. Moreover. the influence of calcination temperature on the thermal stability of the hollow structures was investigated. It showed that the hollow structure was stable after being calcined at 300 degrees C for 2 h. The formation mechanism of the CuO/Fe2O3 hollow spheres under hydrothermal condition was discussed. (C) 2008 Elsevier B.V. All rights reserved.