Dynamic nuclear polarization at 40 kHz magic angle spinning

Abstract : DNP-enhanced solid-state NMR spectroscopy under magic angle spinning (MAS) is rapidly developing into a powerful analytical tool to investigate the structure of a wide range of solid materials, because it provides unsurpassed sensitivity gains. Most developments and applications of DNP MAS NMR were so far reported at moderate spinning frequencies (up to 14 kHz using 3.2 mm rotors). Here, using a 1.3 mm MAS DNP probe operating at 18.8 T and ∼100 K, we show that signal amplification factors can be increased by up to a factor two when using smaller volume rotors as compared to 3.2 mm rotors, and report enhancements of around 60 over a range of sample spinning rates from 10 to 40 kHz. Spinning at 40 kHz is also shown to increase 29Si coherence lifetimes by a factor three as compared to 10 kHz, substantially increasing sensitivity in CPMG type experiments. The contribution of quenching effects to the overall sensitivity gain at very fast MAS is evaluated, and applications are reported on a functionalised mesostructured organic–inorganic material.
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Article dans une revue
Physical Chemistry Chemical Physics, Royal Society of Chemistry, 2016, 18 (15), pp.10616-10622. 〈10.1039/C6CP00839A 〉
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Contributeur : Agnès Bussy <>
Soumis le : mercredi 20 avril 2016 - 09:55:14
Dernière modification le : dimanche 9 décembre 2018 - 13:38:03

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Sachin R Chaudhari, Pierrick Berruyer, David Gajan, Christian Reiter, Frank Engelke, et al.. Dynamic nuclear polarization at 40 kHz magic angle spinning . Physical Chemistry Chemical Physics, Royal Society of Chemistry, 2016, 18 (15), pp.10616-10622. 〈10.1039/C6CP00839A 〉. 〈hal-01304650〉

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