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Solvent-Free High-Field Dynamic Nuclear Polarization of Mesoporous Silica Functionalized with TEMPO

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Abstract

We report high-field magic-angle spinning dynamic nuclear polarization (MAS DNP) of mesoporous silica functionalized with nitroxide radicals. These results demonstrate that co-condensation can be employed to incorporate DNP polarizing agents into inorganic materials and that solvent-free DNP is feasible for porous materials. For the investigated material, the direct MAS DNP enhances the 29Si nuclear magnetic resonance (NMR) spectra, whereas the indirect MAS DNP via protons is inapplicable owing to the inefficiency of \({}^{1}\hbox{H}\rightarrow{}^{29}\hbox{Si}\) cross polarization transfer. Furthermore, the 29Si signals in direct experiments build up in a few seconds at 100 K. This fast polarization buildup improves the NMR sensitivity and will be useful for the investigation of direct DNP below 100 K.

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Acknowledgments

The authors are grateful for funding provided by Region Nord/Pas de Calais, Europe (FEDER), CNRS, French Minister of Science, FR-3050, USTL, ENSCL, Bruker BIOSPIN, and Contract No. ANR-2010-JCJC-0811-01.

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Authors and Affiliations

  1. Univ. Lille Nord de France, 59000, Lille, France

    Aany Sofia Lilly Thankamony, Olivier Lafon, Xingyu Lu, Julien Trébosc, Hervé Vezin & Jean-Paul Amoureux

  2. CNRS, UMR 8181, Unité de Catalyse et de Chimie du Solide, UCCS, Univ. Lille 1, Bât. C7, 59652, Villeneuve d’Ascq, France

    Aany Sofia Lilly Thankamony, Olivier Lafon, Xingyu Lu, Julien Trébosc & Jean-Paul Amoureux

  3. Bruker BioSpin SA, 34, rue de l’Industrie, 67166, Wissembourg Cedex, France

    Fabien Aussenac

  4. Bruker BioSpin Corporation, 15 Fortune Drive, Billerica, MA, 01821, USA

    Melanie Rosay

  5. CNRS, UMR 8516, Laboratoire de Spectrochimie Infrarouge et Raman, LASIR, Univ. Lille 1, Bât. C4, 59652, Villeneuve d’Ascq, France

    Hervé Vezin

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  1. Aany Sofia Lilly Thankamony
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Lilly Thankamony, A.S., Lafon, O., Lu, X. et al. Solvent-Free High-Field Dynamic Nuclear Polarization of Mesoporous Silica Functionalized with TEMPO. Appl Magn Reson 43, 237–250 (2012). https://doi.org/10.1007/s00723-012-0364-3

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