Pure ZnO and Ce-doped (5 at.%) ZnO aerogels were prepared by dissociation of dihydrate zinc acetate and cerium nitrate in methanol, followed by drying in supercritical conditions of the solvent. The concentration of zinc acetate solution and the atomic ratio Ce/Zn were fixed at 0.2 mol/L and 0.05 mol/L, respectively. XRD results showed a hexagonal wurtzite structure of ZnO aerogel crystallites and a formation of a separate second phase of ceria cubic phase with fluorite structure and 7.4 nm in size. The introduction of cerium in the solution had a negative effect on the aerogel crystalline quality. The crystallites size was found to be 16 nm in pure ZnO and 27 nm in Ce-doped ZnO aerogels. The grains of Ce-doped ZnO aerogel had torus shaped morphology with hollow centers, but those of pure ZnO were flattened semispheres. The calculated values of different structural parameters showed that cerium ions introduced into the ZnO lattice occupied interstitial sites and Zn ions substituted Ce ones in ceria lattice during the formation process. FT-IR and UV-Vis absorption spectra have not revealed any particularities due to the presence of cerium atoms in ZnO, indicating that Ce (5 at.%) doping of ZnO crystallites synthesized in supercritical methanol did not strongly affect the optical gap of the semiconductor. Micro-Raman studies confirmed the formation of cubic fluorite structure ceria in ZnO aerogel and showed that Raman active modes of ZnO are amplified with the presence of ceria.

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Zinc oxide nanoscale powder has been synthesized by a hydrothermal route using zinc sulfate and sodium hydroxide. The as-prepared powder was annealed at 600 °C for 2 h and then characterized by X-ray diffraction (XRD), scanning electron microscopy and infra-red Fourier transformed spectroscopy. XRD measurements have shown a ZnO hexagonal wurtzite polycrystalline structure with good crystallinity and the formation of a new sodium pyrosulfate phase in the as-prepared powder. The annealing improves the crystalline quality of the powder and transforms the sodium pyrosulfate phase to a sodium sulfate one. The thermal treatment does not affect the lattice parameters and the Zn–O bond length but improves the random orientation of the ZnO crystallites growth. ZnO crystallites have an interconnected-nano-needles morphology forming irregular shaped aggregates. The size of the crystallites is about 20 nm. EDX analysis has shown the presence of C and S in addition to Zn and O. FTIR spectra confirm the formation of ZnO and sodium sulfate. The synthesized ZnO powder has a very high crystalline quality and the used method is a very advantageous one for the fabrication of nanosized metal oxides from inorganic reactants for photo-catalysis applications.