Network connectivity in cesium borosilicate glasses: 17O multiple-quantum MAS and double-resonance NMR

Aguiar, Pedro M.; Michaelis, Vladimir K.; McKinley, Christine M.; Kroeker, Scott

doi:10.1016/j.jnoncrysol.2012.12.010

Cited by 31 publications

(25 citation statements)

References 57 publications

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“…Unfortunately, the NMR sensitive isotope 17 O does not present favorable NMR characteristics: its low natural abundance (0.037%) thus requires 17 O enrichment, and its 5/2 spin requires special NMR sequences to provide spectra with sufficient resolution. While 17 O has been widely used to analyze the structure of borosilicate-based glasses [65][66][67][68][69][70], there is, to our knowledge, only one paper about 17 O NMR on enriched borophosphate glasses [26]. However, this paper from 2005 clearly showed the possibility of separating bridging P-O-P and P-O-B oxygens by using MQ-MAS NMR experiments [49] and there is no doubt that conducting such a study with the high field NMR machines and the correlation NMR sequences now available would provide a very interesting set of data that would shed new light onto the borophosphate network organization.…”

Section: Discussionmentioning

confidence: 99%

Solid State NMR: A Powerful Tool for the Characterization of Borophosphate Glasses

2020

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This review will show how solid state nuclear magnetic resonance (NMR) has contributed to a better understanding of the borophosphate glass structure. Over the last fifteen years, 1D and 2D magic angle spinning (MAS)-NMR has been used to produce key information about both local and medium range organization in this type of glass. After a brief presentation on borophosphate glasses, the paper will focus on the description of the local order of phosphate and borate species obtained by 1D 31P-and 11B-MAS-NMR experiments, with a special emphasis on the improvements obtained at high magnetic fields on the borate speciation description. The last part of this review will show how correlation NMR provided new insights into the intermediate length scale order. Special attention will be paid to the quantitative data retrieved from 11B/31P REDOR-based NMR sequences and to the qualitative connectivity schemes observed on the 2D 11B/31P maps edited with the heteronuclear multiple quantum coherence (HMQC) NMR techniques.

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Section: Discussionmentioning

confidence: 99%

Solid State NMR: A Powerful Tool for the Characterization of Borophosphate Glasses

2020

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“…5 In order to increase the sensitivity of the experiments and address these problems, samples have been isotopically enriched, 6–8 population transfer techniques optimized, 9,10 and experiments performed at high magnetic fields (≥18.8 T), which improves the Boltzmann polarizaton. 11–16 In addition, dynamic nuclear polarization (DNP) has recently provided enhancements in 17 O signal intensities of up to 115, offering an additional boost in sensitivity important for studies of challenging systems. 17–21 Finally, higher Zeeman fields also narrow the second-order powder patterns, increasing sensitivity and improving the spectral resolution.…”

Section: Introductionmentioning

confidence: 99%

¹⁷O NMR Investigation of Water Structure and Dynamics

2016

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The structure and dynamics of the bound water in barium chlorate monohydrate were studied with 17O nuclear magnetic resonance (NMR) spectroscopy in samples that are stationary and spinning at the magic-angle in magnetic fields ranging from 14.1 to 21.1 T. 17O NMR parameters of the water were determined, and the effects of torsional oscillations of the water molecule on the 17O quadrupolar coupling constant (CQ) were delineated with variable temperature MAS NMR. With decreasing temperature and reduction of the librational motion, we observe an increase in the experimentally measured CQ explaining the discrepancy between experiments and predictions from density functional theory. In addition, at low temperatures and in the absence of 1H decoupling, we observe a well-resolved 1H–17O dipole splitting in the spectra, which provides information on the structure of the H2O molecule. The splitting arises because of the homogeneous nature of the coupling between the two 1H–17O dipoles and the 1H–1H dipole.

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“…The signal is narrowed by motional averaging at high temperature. The doped ions can stay temporarily at unstable sites in the glass network [37,38] and such ions are stabilized by ion migration. Therefore, we also assume line narrowing as ensemble average by annealing at high temperature.…”

Section: Resultsmentioning

confidence: 99%

Hyperpolarized cesium ions doped in a glass material

Ishikawa

2014

Journal of Magnetic Resonance

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Network connectivity in cesium borosilicate glasses: 17O multiple-quantum MAS and double-resonance NMR

Cited by 31 publications

References 57 publications

Solid State NMR: A Powerful Tool for the Characterization of Borophosphate Glasses

Solid State NMR: A Powerful Tool for the Characterization of Borophosphate Glasses

¹⁷O NMR Investigation of Water Structure and Dynamics

Hyperpolarized cesium ions doped in a glass material

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Network connectivity in cesium borosilicate glasses: 17O multiple-quantum MAS and double-resonance NMR

Cited by 31 publications

References 57 publications

Solid State NMR: A Powerful Tool for the Characterization of Borophosphate Glasses

Solid State NMR: A Powerful Tool for the Characterization of Borophosphate Glasses

17O NMR Investigation of Water Structure and Dynamics

Hyperpolarized cesium ions doped in a glass material

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Product

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¹⁷O NMR Investigation of Water Structure and Dynamics