The modified Pechini method has been applied to the preparation of nano-structured SnO 2 and SnO 2 :CuO. The sample characterization was carried out by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), infrared spectroscopy (IR) and nitrogen adsorption isotherms (BET). The CuO phase in SnO 2 :CuO samples was successfully characterized by XRD, XPS and IR. The highest degree of crystallinity and subsequently the maximum intensity and area of CuO (002) diffraction peaks were observed for the samples prepared with templates. The morphology and microstructure of the hybrid were studied using SEM. The core level binding energies of Cu 2p, Sn 3d, and O 1s were measured in these samples. The appearance of a satellite peak in the Cu 2p spectra provided definitive evidence for the presence of Cu 2? ions in these samples. The influence of synthesis conditions such as solvent, precursor type, calcinations temperature and time on the detectability of CuO and the morphology and microstructure of the hybrid were also studied. The calcinations conditions had a significant effect on the appearance and intensity of CuO diffraction peaks.