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Félix Galindo-Hernández,Gloria del Ángel,Carlos Guzmán,Ricardo Gómez 한양대학교 세라믹연구소 2008 Journal of Ceramic Processing Research Vol.9 No.6
Sol-gel TiO2-CeO2 semiconductors were synthesized at pH 3 and 9 using titanium alkoxide as the initial reactant; and either nitric acid or ammonium hydroxide as hydrolysis agents. The gels annealed at 473, 673 and 873 K were characterized by nitrogen adsorption,X-ray diffraction and Raman spectroscopy. The surface fractal dimension, crystallite size, titanium deficiency and electron density were calculated by the Frenkel-Halsey-Hill method, Rietveld refinement, and Fourier electron density map, respectively. Mesoporous materials showing high specific surface areas (250-99m2/g for pH 3 and 267-88 m2/g for pH 9) were obtained in both preparations. Anatase and anatase-cerianite crystalline phases were observed by X-ray diffraction in the samples prepared at pH 3 and pH 9 respectively. Nanocrystalline structures (from 7.1 to 43.6 nm) and an important titanium deficiency, depending on the synthesis conditions are reported. The Fourier electron density maps showed that for the semiconductors prepared at pH 3 the electron density was contracted in comparison with the samples synthesized at pH 9 where enlarged electron density maps were observed. A good agreement between the electron density maps and the surface fractal dimensions was obtained. Sol-gel TiO2-CeO2 semiconductors were synthesized at pH 3 and 9 using titanium alkoxide as the initial reactant; and either nitric acid or ammonium hydroxide as hydrolysis agents. The gels annealed at 473, 673 and 873 K were characterized by nitrogen adsorption,X-ray diffraction and Raman spectroscopy. The surface fractal dimension, crystallite size, titanium deficiency and electron density were calculated by the Frenkel-Halsey-Hill method, Rietveld refinement, and Fourier electron density map, respectively. Mesoporous materials showing high specific surface areas (250-99m2/g for pH 3 and 267-88 m2/g for pH 9) were obtained in both preparations. Anatase and anatase-cerianite crystalline phases were observed by X-ray diffraction in the samples prepared at pH 3 and pH 9 respectively. Nanocrystalline structures (from 7.1 to 43.6 nm) and an important titanium deficiency, depending on the synthesis conditions are reported. The Fourier electron density maps showed that for the semiconductors prepared at pH 3 the electron density was contracted in comparison with the samples synthesized at pH 9 where enlarged electron density maps were observed. A good agreement between the electron density maps and the surface fractal dimensions was obtained.