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Formation and characterization of a SnO_2-Al_2O _3 system derived from a sol-gel process based on different tin precursors

机译:基于不同锡前体的溶胶-凝胶工艺衍生的SnO_2-Al_2O_3体系的形成与表征

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摘要

A series of SnO_2-Al_2O_3 samples with SnO_2 to Al_2O_3 molar ratio of 1:1, 0.5:1, 0.25:1 and 0.1:1, have been synthesized by the sol-gel technique using Al(C _3H_7O)_3 and tin (IV) dihydroxy 2,4-pentanedione acetate as precursors. Samples of the above series were characterized by thermal analysis, X-ray diffraction, Fourier transform infrared spectroscopy and nitrogen adsorption to establish their porous structure. The structures of the binary gel systems obtained were found to differ from those of the analogous series in which Sn(ac)_4 (acetic series) was used as precursor. The tin component introduced into the samples of both series was responsible for the narrowing of the range of diameters of the pores (contributing to the highest extent to the cumulative pore volume) relative to their range in pure aluminum gel. The range of the dominant pore diameters was at the same time shifted towards smaller values, but these changes were more pronounced for (ac) series. The use of β-diketonate complexes of tin instead of Sn(ac)_4, leads also to changes in the character of OH group on the surface of the binary gel samples. For this series (acac) of binary gels in the whole range of concentrations of the tin component only one type of hydroxyl groups appears, not present in the monocomponent aluminum gel and in the binary gels of (ac) series.
机译:利用Al(C _3H_7O)_3和锡(IV)通过溶胶-凝胶技术合成了一系列SnO_2-Al_2O_3样品,其中SnO_2与Al_2O_3的摩尔比为1:1、0.5:1、0.25:1和0.1:1 )乙酸二羟基2,4-戊二酮酯作为前体。通过热分析,X射线衍射,傅立叶变换红外光谱和氮吸附来表征上述系列的样品以建立其多孔结构。发现获得的二元凝胶体系的结构不同于其中使用Sn(ac)_4(乙酸系列)作为前体的类似系列的结构。相对于纯铝凝胶,引入到这两个系列的样品中的锡组分可导致孔直径范围的缩小(对累积孔体积的最大贡献)。同时,主要孔径的范围向较小的值移动,但是对于(ac)系列,这些变化更为明显。使用锡的β-二酮酸酯络合物代替Sn(ac)_4,还会导致二元凝胶样品表面OH基团的特性发生变化。对于该系列(acac)的二元凝胶,在锡组分的整个浓度范围内,仅出现一种类型的羟基,在单组分铝凝胶和(ac)系列的二元凝胶中不存在。

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