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research article

Dynamic nuclear polarization at 40 kHz magic angle spinning

Chaudhari, Sachin R.
•
Berruyer, Pierrick
•
Gajan, David
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2016
Physical Chemistry Chemical Physics

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 inverted perpendicular and similar to 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 Si-29 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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Type
research article
DOI
10.1039/c6cp00839a
Web of Science ID

WOS:000374350600083

Author(s)
Chaudhari, Sachin R.
Berruyer, Pierrick
Gajan, David
Reiter, Christian
Engelke, Frank
Silverio, Daniel L.
Coperet, Christophe
Lelli, Moreno
Lesage, Anne
Emsley, Lyndon  
Date Issued

2016

Publisher

Royal Society of Chemistry

Published in
Physical Chemistry Chemical Physics
Volume

18

Issue

15

Start page

10616

End page

10622

Editorial or Peer reviewed

REVIEWED

Written at

OTHER

EPFL units
LRM  
Available on Infoscience
July 19, 2016
Use this identifier to reference this record
https://infoscience.epfl.ch/handle/20.500.14299/127848
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