NMR and EPR Characterization of Functionalized ...
Document type :
Article dans une revue scientifique
DOI :
Permalink :
Title :
NMR and EPR Characterization of Functionalized Nanodiamonds
Author(s) :
Presti, Charlène [Auteur]
Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier [ICGM ICMMM]
Thankamony, Aany Sofia Lilly [Auteur]
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Alauzun, Johan G. [Auteur]
Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier [ICGM ICMMM]
Mutin, P. Hubert [Auteur]
Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier [ICGM ICMMM]
Carnevale, Diego [Auteur]
GGRC-ISIC-EPFL
Lion, Cedric [Auteur]
Unité de Glycobiologie Structurale et Fonctionnelle (UGSF) - UMR 8576
Unité de Glycobiologie Structurale et Fonctionnelle - UMR 8576 [UGSF]
Vezin, Herve [Auteur]
Laboratoire Avancé de Spectroscopie pour les Intéractions la Réactivité et l'Environnement - UMR 8516 [LASIRE]
Laurencin, Danielle [Auteur]
Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier [ICGM ICMMM]
Lafon, Olivier [Auteur]
Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier [ICGM ICMMM]
Thankamony, Aany Sofia Lilly [Auteur]
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Alauzun, Johan G. [Auteur]
Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier [ICGM ICMMM]
Mutin, P. Hubert [Auteur]
Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier [ICGM ICMMM]
Carnevale, Diego [Auteur]
GGRC-ISIC-EPFL
Lion, Cedric [Auteur]

Unité de Glycobiologie Structurale et Fonctionnelle (UGSF) - UMR 8576
Unité de Glycobiologie Structurale et Fonctionnelle - UMR 8576 [UGSF]
Vezin, Herve [Auteur]

Laboratoire Avancé de Spectroscopie pour les Intéractions la Réactivité et l'Environnement - UMR 8516 [LASIRE]
Laurencin, Danielle [Auteur]
Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier [ICGM ICMMM]
Lafon, Olivier [Auteur]

Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Journal title :
The Journal of Physical Chemistry C
Abbreviated title :
J. Phys. Chem. C
Volume number :
119
Pages :
12408-12422
Publication date :
2015
ISSN :
12408–12422
English keyword(s) :
Functionalization
Carbon nanomaterials
Nuclear magnetic resonance spectroscopy
Polarization
Nanocrystals
Carbon nanomaterials
Nuclear magnetic resonance spectroscopy
Polarization
Nanocrystals
HAL domain(s) :
Chimie/Chimie inorganique
English abstract : [en]
We investigated the potential of solid-state NMR using magic angle spinning (MAS) with and without dynamic nuclear polarization (DNP) and electron paramagnetic resonance (EPR) for the characterization of functionalized ...
Show more >We investigated the potential of solid-state NMR using magic angle spinning (MAS) with and without dynamic nuclear polarization (DNP) and electron paramagnetic resonance (EPR) for the characterization of functionalized nanodiamonds (NDs). We showed that conventional 1H, 31P, and 13C solid-state NMR spectra allow differentiating in a straightforward way NDs from commercial sources and custom-made NDs bearing aromatic or aliphatic phosphonate moieties at their surface. Besides, the short nuclear relaxation times prove the close proximity between the endogenous paramagnetic centers of NDs and the grafted organic moieties. EPR spectra confirmed the presence of these paramagnetic centers in functionalized NDs, which are centered on dangling bonds as well as a few N0 defects, corresponding to the substitution of carbon atoms by nitrogen ones. Hyperfine sublevel correlation spectroscopy indicates that the N0 paramagnetic centers are mostly located in the disordered shell of NDs. Preliminary DNP-enhanced NMR experiments at 9.4 T and 100 K under MAS have shown a lack of significant DNP enhancement, which can be attributed to the short relaxation times of the unpaired electrons and the nuclei in NDs. When using exogenous polarizing agents, the endogenous unpaired electrons contribute to a leakage of polarization. Furthermore, low temperatures lead to a broadening of NMR signals. It therefore appears that conventional direct excitation remains the NMR method of choice for the characterization of functionalized NDs.Show less >
Show more >We investigated the potential of solid-state NMR using magic angle spinning (MAS) with and without dynamic nuclear polarization (DNP) and electron paramagnetic resonance (EPR) for the characterization of functionalized nanodiamonds (NDs). We showed that conventional 1H, 31P, and 13C solid-state NMR spectra allow differentiating in a straightforward way NDs from commercial sources and custom-made NDs bearing aromatic or aliphatic phosphonate moieties at their surface. Besides, the short nuclear relaxation times prove the close proximity between the endogenous paramagnetic centers of NDs and the grafted organic moieties. EPR spectra confirmed the presence of these paramagnetic centers in functionalized NDs, which are centered on dangling bonds as well as a few N0 defects, corresponding to the substitution of carbon atoms by nitrogen ones. Hyperfine sublevel correlation spectroscopy indicates that the N0 paramagnetic centers are mostly located in the disordered shell of NDs. Preliminary DNP-enhanced NMR experiments at 9.4 T and 100 K under MAS have shown a lack of significant DNP enhancement, which can be attributed to the short relaxation times of the unpaired electrons and the nuclei in NDs. When using exogenous polarizing agents, the endogenous unpaired electrons contribute to a leakage of polarization. Furthermore, low temperatures lead to a broadening of NMR signals. It therefore appears that conventional direct excitation remains the NMR method of choice for the characterization of functionalized NDs.Show less >
Language :
Anglais
Audience :
Internationale
Popular science :
Non
Administrative institution(s) :
ENSCL
CNRS
Centrale Lille
Univ. Artois
Université de Lille
CNRS
Centrale Lille
Univ. Artois
Université de Lille
Collections :
Research team(s) :
RMN et matériaux inorganiques (RM2I)
Submission date :
2019-09-25T14:06:13Z
2021-02-25T09:12:51Z
2021-02-25T09:12:51Z