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Probing oxide-based glass structures by solid-state NMR: Opportunities and limitations
Journal of Magnetic Resonance Open Pub Date : 2023-03-28 , DOI: 10.1016/j.jmro.2023.100112
Mattias Edén

This Primer critically reviews the possibilities and limitations of probing the short-range structure of an oxide-based glass by routine magic-angle spinning (MAS) or triple-quantum MAS (3QMAS) nuclear magnetic resonance (NMR) experiments. We briefly outline the structural features of oxide-based glasses and the basics of solid-state NMR. Besides suggesting guidelines for selecting favorable experimental conditions and important considerations for recording high-quality MAS NMR spectra amenable for subsequent analysis, we review options for extracting NMR observables and their distributions from spins-1/2 as well as half-integer spin quadrupolar nuclei. Considering that the isotropic chemical shift remains the primary probe of local structure by MAS NMR, we thoroughly review its dependence on the short-range oxide-based glass parameters from the viewpoint of a very simple and intuitive but qualitative model. The utility of deconvolutions of notably 29Si and 31P MAS NMR spectra are discussed critically. We also suggest alternative yet qualitative analysis options that are available whenever MAS NMR spectral deconvolutions are not warranted without additional information, which incidentally applies to a majority of modern multicomponent glasses.



中文翻译:

通过固态 NMR 探测氧化物基玻璃结构:机遇与局限

本入门书批判性地回顾了通过常规魔角旋转 (MAS) 或三量子 MAS (3QMAS) 核磁共振 (NMR) 实验探测氧化物基玻璃的短程结构的可能性和局限性。我们简要概述了氧化物基玻璃的结构特征和固态 NMR 的基础知识。除了建议选择有利实验条件的指南和记录适合后续分析的高质量 MAS NMR 光谱的重要考虑因素外,我们还回顾了从自旋 1/2 和半整数自旋四极核中提取 NMR 可观测值及其分布的选项。考虑到各向同性化学位移仍然是 MAS NMR 局部结构的主要探针,我们从一个非常简单直观但定性的模型的角度彻底审查了它对短程氧化物基玻璃参数的依赖性。值得注意的是,反卷积的效用批判性地讨论了29 Si 和31 P MAS NMR 光谱。我们还建议在没有额外信息的情况下,只要 MAS NMR 光谱解卷积不被保证,就可以使用替代但定性的分析选项,这顺便适用于大多数现代多组分玻璃。

更新日期:2023-03-28
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