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纳米晶二氧化锡的119Sn魔角旋转核磁共振

119Sn magic angle spinning NMR of nanocrystalline SnO2.

作者信息

Sabarinathan V, Vinod Chandran C, Ramasamy S, Ganapathy S

机构信息

Department of Nuclear Physics, University of Madras, Guindy Campus, Chennai 600025, India.

出版信息

J Nanosci Nanotechnol. 2008 Jan;8(1):321-8.

Abstract

Nanocrystalline SnO2 samples of different grain sizes, prepared by inert gas condensation technique (IGCT) and chemical precipitation method and conforming to the tetragonal phase, have been studied by variable speed (3-10 kHz) 119Sn MAS NMR at 11.74 Tesla field. 119Sn solid-state NMR results show that the IGCT prepared samples have good crystallinity and phase purity compared to the samples prepared by the chemical method. The determination of 119Sn chemical shielding parameters (delta iso, delta delta and eta) from slow MAS spectra shows that the 119Sn isotropic chemical shift (delta iso) is strongly influenced at smaller grain sizes, attributable to the change in the O2- local symmetry for the surface 119Sn ions at smaller grain sizes. The observed line widths in MAS spectra are significantly larger than the life-time broadening due to spin-lattice (T1) and spin-spin (T2) relaxation. The 119Sn MAS NMR spectra are thus inhomogeneously broadened by a distribution of isotropic chemical shifts, the line broadening increasing with decrease in grain size.

摘要

采用惰性气体冷凝技术(IGCT)和化学沉淀法制备了不同晶粒尺寸且符合四方相的纳米晶二氧化锡样品,并在11.74特斯拉磁场下通过变速(3 - 10千赫兹)119Sn 魔角旋转核磁共振(MAS NMR)对其进行了研究。119Sn 固态核磁共振结果表明,与化学方法制备的样品相比,IGCT 制备的样品具有良好的结晶度和相纯度。从慢速MAS 谱图确定119Sn 化学屏蔽参数(δiso、δδ 和 η)表明,在较小晶粒尺寸下,119Sn 各向同性化学位移(δiso)受到强烈影响,这归因于较小晶粒尺寸下表面119Sn 离子的O2- 局部对称性变化。MAS 谱图中观察到的线宽明显大于自旋 - 晶格(T1)和自旋 - 自旋(T2)弛豫导致的寿命展宽。因此,119Sn MAS NMR 谱图因各向同性化学位移的分布而不均匀展宽,线展宽随晶粒尺寸减小而增加。

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