沸石的光电子和离子散射光谱研究。第四部分钒改性沸石的XPS研究

M. Wark, M. Koch, A. Brückner, W. Grünert
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引用次数: 29

摘要

将钒以不同的添加量(0.36 ~ 3.3 wt.%)和化学状态引入沸石中,并通过XPS、UV-VIS和EPR光谱对其进行了研究。所研究的钒沸石是钒硅沸石、钒离子(VO2+)交换的ZSM-5、MOR、Y、X和氧化钒聚集体,通过化学气相沉积VOCl3并随后水解和煅烧沉积在ZSM-5上。通过仔细处理x射线卫星减影,所有样品都获得了可靠的XPS分析。通过V 2p结合能的不同,可以区分出四种类型的钒(框架内V、VO2+离子、沸石内VV氧化物团簇和沸石外V2O5聚集体)。紫外可见光谱和EPR光谱证据支持了它们信号的分配。结果表明,XPS与UV-VIS和EPR相结合是分析含钒沸石的一种有效方法。
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Investigation of zeolites by photoelectron and ion scattering spectroscopy Part IV XPS studies of vanadium-modified zeolites
Vanadium was introduced into zeolites in different amounts (0.36–3.3 wt.%) and chemical states and was investigated by XPS, UV–VIS and EPR spectroscopies. The vanadium zeolites studied were vanadium silicalites, vanadyl ion (VO2+)-exchanged ZSM-5, MOR, Y, X and vanadium oxide aggregates deposited in/on ZSM-5 via chemical vapour deposition of VOCl3 with subsequent hydrolysis and calcination. By careful treatment of the X-ray satellite subtraction, reliable XPS analyses were obtained for all samples. Four types of vanadium species (intra-framework V, VO2+ ions, intra-zeolite VV oxide clusters and extra-zeolite V2O5 aggregates) could be discerned by their differing V 2p binding energies. The assignment of their signals was supported by UV–VIS and EPR spectroscopical evidence. It was thus shown that combination of XPS with UV–VIS and EPR provides a useful method for the analysis of vanadium-containing zeolites.
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