RM2i : RMN et Matériaux Inorganiques

Responsable : Laurent Delevoye (CR CNRS)



 

 

 

 

 

 

 

Membres de l’équipe :

Amoureux Jean-Paul, Professeur

Delevoye Laurent, Chargé de Recherches CNRS

Lafon Olivier, Professeur

Mear François, Maître de Conférences.

Montagne Lionel, Professeur

Pourpoint Frédérique, Maître de Conférences.

Trebosc Julien, Ingénieur de Recherches CNRS (Fédération Chevreul).

 

Mots clefs :

- Nouvelles méthodes avancées de RMN à l'état solide, surtout appliquées aux noyaux quadripolaires.
- DNP-NMR : développements méthodologiques.
- Calculs DFT de paramètres RMN
- Applications aux matériaux inorganiques et hybrides: verres, catalyseurs, céramiques, nanomatériaux, MOF ...
- Structure et applications des verres
- Chimie des phosphates
- Domaines d’applications :

  • Énergie (Self-guérison verres d'étanchéité pour SOFC)
  • Développement durable (vitrification de déchet nucléaire)
  • Aéronautique (revêtements protecteurs pour les matériaux composites)

Thèmes de recherche de l’équipe :

Comme l'indique le nom de notre équipe, nous avons deux champs de recherche complémentaires:
Notre premier centre d’intérêt se situe dans la relation entre la structure atomique et les propriétés physiques des matériaux non cristallins (verres). L'approche est pluridisciplinaire, associant des compétences complémentaires en chimie des verres et en spectroscopie RMN à l'état solide.

Comme illustré sur la figure ci-dessous, ces deux compétences permettent de couvrir différents aspects de la science du verre, incluant la formulation et la synthèse des verres, leur caractérisation structurale de pointe et leurs applications.
Les activités de l’équipe dans le domaine de la RMN des solides impliquent le développement de nouvelles séquences permettant d'augmenter à la fois la résolution et la sensibilité des mesures. Nous développons des méthodes dans tous les domaines qui impliquent des hauts champs magnétiques (18.8T et 21T) et pour des vitesses de rotation élevées (jusqu'à 60 kHz), avec une expertise particulière des noyaux quadripolaires. Nous nous efforçons par exemple de concevoir de nouvelles expériences de corrélation afin d'améliorer la caractérisation structurale des réseaux vitreux.
Un accent est mis sur les verres de  phosphate, qui constituent une autre compétence forte de l’équipe. Ceux-ci peuvent être des verres de purs phosphates, mais aussi des verres d'aluminosilicate, de borosilicate et vanadate à réseau mixte (c'est-à-dire combinés avec des entités phosphates).

Nous développons ces verres pour des applications non conventionnelles dans les domaines des combustibles nucléaires (vitrification de déchets spéciaux), l'auto-guérison de verres d'étanchéité pour les piles à combustible haute température (SOFC) et les revêtements anti-oxydation de composants aéronautiques (freins d’avion et tuyère de réacteur).

 

 

Étudiants / enseignement :


Nous accueillons des étudiants au sein de notre équipe au niveau master (1 et 2), et aussi dans le cadre des échanges Erasmus. Nous formons à la recherche des doctorants, et accueillons des post-docs en soutien à des projets académiques ou industriels.

Nous sommes impliqués dans l'enseignement de RMN dans le master ERASMUS "Advanced Spectroscopy for Chemists" http://www.master-asc.org/index.php et de la valorisation des matériaux inorganiques dans le master «Chimie pour l'énergie et l'environnement».

Résultats scientifiques récents:

Nous sommes parmi les pionniers de la caractérisation des matériaux mésoporeux et des nanomatériaux par Polarisation Dynamique Nucléaire (DNP). En particulier, nous avons démontré que la DNP directe 29Si est complémentaire de la DNP indirecte 29Si via les protons. La DNP directe permet notamment d’observer les sites 29Si situés au voisinage des centres paramagnétiques. A l’inverse, la DNP indirecte permet d’observer sélectivement les premières couches sous la surface (à moins de 0,5 nm de la surface). Les différentes contributions au gain DNP ont été mesurées. La DNP a été utilisée pour sonder les proximités 27Al-27Al à la surface de l’alumine mésoporeuse. Nous cherchons actuellement à optimiser le transfert DNP, à combiner la DNP avec des méthodes RMN avancées et à étendre le domaine d’application de cette technique.

Fig 1: La DNP directe permet notamment d’observer les sites 29Si situés au voisinage des centres paramagnétiques. A l’inverse, la DNP indirecte permet d’observer sélectivement les premières couches sous la surface

Fig 2 Observation des connectivités dans les solides par RMN.

Nous avons introduit, des méthodes nouvelles pour l’observation des proximités homo-  et hétéro-nucléaires. Ces méthodes, qui ont l’avantage d’être utilisables à haut champ et pour des fréquences de rotation élevées, ont permis de repousser les limites en termes d’efficacité et de robustesse. Nous avons pu observer les proximités internucléaires, même en présence de fortes interactions telles que l’interaction quadripolaire, l’écrantage électronique ou les couplages dipolaires. Nous avons montré qu’il est possible d’observer des proximités entre noyaux de fréquences proches (13C-27Al). Ces techniques ont été utilisées pour sonder la structure de matériaux inorganiques cristallins (fluoroaluminates, aluminophosphate, polyoxométallates), verres, catalyseurs supportés, complexes organométallique.

Nous associons les développements méthodologiques en RMN des solides à la caractérisation structurale de systèmes réels en catalyse. En particulier, nous avons relevé le défi d’identifier des entités de surface en faible quantité, des hydrures d’aluminium (Al-H), greffées sur de l’alumine, en réalisant des expériences RMN de corrélations via le couplage scalaire et dipolaire entre Al et H. Ces nouvelles méthodes, particulièrement puissantes ont permis de mieux comprendre la structure locale des centres actifs, et de montrer que ces espèces étaient à l’origine de la réactivité exceptionnelle de ce catalyseur.

Fig 3: Les correlations 1H-27Al mettent en évidence les sites protons d’un catalyseur à base d’alumine

Fig 4 : Le calcul DFT des paramètres RMN permet de décomposer avec précision le spectre de l’oxygène-17 de Na5P3O10.

Nous avons contribué à mieux comprendre les relations qui lient les paramètres RMN à la structure de matériaux inorganiques cristallisés et amorphes. En particulier, nous nous sommes intéressés à l’oxygène-17, en combinant approches par RMN expérimentale et par calculs DFT de paramètres RMN pour démontrer que dans des verres de phosphates, l’information structurale locale est encodée par l’interaction quadripolaire alors que l’interaction d’écrantage électronique nous renseigne sur la structure vitreuse à longue distance. En y ajoutant la dynamique moléculaire, nous avons proposé pour la première fois une structure d’un verre modèle qui rend compte des distributions de paramètres RMN
Dans un article récemment publié dans le Journal of the American Chemical Society, nous avons montré, en collaboration avec des collègues du LC2P2 (M. Taoufik, CNRS-Université Lyon 1) de Villeurbanne et du LPCNO (L. Maron, CNRS-INSA) comment la Résonance Magnétique Nucléaire (RMN) de l’oxygène-17 permettait de dévoiler avec une précision non atteinte jusqu’alors comment se comporte la surface-même du support dans des catalyseurs hétérogènes. Par le biais de mesures directes (homonucléaires) et impliquant différents couples de noyaux (hétéronucléaires, hydrogène et oxygène), et en combinant des expériences RMN récemment développées, il a été possible non seulement d’extraire les proportions des différentes espèces présentes en surface mais surtout de déterminer les positions relatives de différents fragments. Des calculs théoriques, menés par nos collègues toulousains, sont venus guider et conforter les interprétations, une approche nécessaire pour un noyau aussi complexe que l’oygène-17. Ceci devrait permettre de mieux comprendre la structure des catalyseurs hétérogènes au niveau moléculaire et ainsi de guider leur synthèse vers l’obtention de matériaux aux performances améliorées.

Fig 5 : Différentes étapes de la caractérisation approfondie de la surface d’un catalyseur : en combinant un enrichissement sélectif de la surface du catalyseur en oxygène-17 à des études RMN à haut champ et à des calculs DFT, il est possible de révéler des caractéristiques structurelles insoupçonnées.

 

Fig 6: Spectre de corrélation 31P-51V montrant la connectivité phosphate-vanadate dans un réseau vitreux.

L’activité phare du groupe ‘Verre et RMN’ consiste en la caractérisation par RMN avancée de matériaux vitreux (historiquement à base phosphatée). Ces travaux, basés sur l’application de séquences récentes de RMN de corrélation homo- et hétéro-nucléaire, ont permis de déterminer pour la première fois la nature des motifs structuraux présents dans les verres à réseau mixte boro-, alumino- et vanado-phosphatés. Ces informations inédites ont permis de mieux comprendre comment la structure complexe de ces matériaux gouverne leurs intéressantes propriétés macroscopiques, notamment pour le stockage de déchets nucléaires spéciaux (iode, sulfates)

Nous avons développé en collaboration avec le CEA de Marcoule des verres d’aluminophosphate d’argent capables d’immobiliser jusqu’à 20% en masse d’iode radioactif sans volatilisation au cours du traitement thermique. Les études structurales montrent que l’iode s’insère dans le réseau vitreux sans modifier sa connectivité.

 

Fig 7: Modèle de l’incorporation d’iode dans un réseau vitreux aluminophosphate déduit des études structurales.

 

Fig 8 : Des particules de borure de vanadium dispersées dans la matrice vitreuse permettent de cicatriser une fissure à 800°C en moins d’une heure

 
Notre équipe est la première à avoir appliqué le concept de cicatrisation extrinsèque (par ajout de particules cicatrisantes) aux matériaux vitreux. Le MEB environnemental et la nano-tomographie montrent qu’une fissure se comble par formation in-situ d’un nouveau verre. Le concept a été validé à l’échelle semi-industrielle grâce à un projet de maturation OSEO-Région NPdC réalisé en collaboration avec le CEA. Nous abordons actuellement l’extension du concept aux verres en couches minces.

Nous menons depuis de nombreuses années des travaux sur l’antioxydation des matériaux composites carbonés dans le cadre de partenariats avec les sociétés HERAKLES-SNECMA et MESSIER-BUGATTI. Les applications visent la protection de freins d’avion ou le traitement cosmétique de tuyères de réacteurs.

 

 

 

Collaborations industrielles :

Messier (PhD): protection anticatalytique de freins d'avions
Snecma (PhD): revêtement anti-oxydation pour une application aéronautique.
Snecma (post-doc): Solution d’émaillage de réacteur d'avion (projet ARCOCE)
Arc International: formulation de verre
CEA: matrice de verre pour l'immobilisation de sulfate et d'iode.
DGA: auto-guérison de revêtements de verre à haute-température.

Bruker: Développement de méthodes de RMN avancés.

 

Collaborations scientifiques :

Verres: G.P. Kothiyal, Bhabha Atomic Research Centre, Bombai, Inde, J.J. Videau, ICMCB., L. Koudelka, Dpt of chem. eng., University of Pardubice (Tchéquie). Léo van Wullen, Institut fur Physikalische Chemie, University of Muenster (Allemagne), Philippe Thomas, LPCTS, Limoge, Francisco Munoz, ICV Madrid.

Méthodologie RMN: M. Pruski et T. Kobayashi, Ames-Iowa, USA, Zhehong Gan, Tallahassee, USA, Stefan Steuernagel, Karlsruhe, Allemagne, Subramanian Ganapathy, Pune, Inde , F. Taulelle et C. Martineau, université Versailles, J. Frye, Fort-Collins, USA, Jun Ashida, Tokyo, Japon, Eriks Kupce, UK. P.K. Madhu, Mumbai, Inde; D. Massiot, F. Fayon et M. Deschamps, Orléans, France; P. Lesot, université Paris-Sud, France ; Th. Charpentier, CEA Saclay, France ; S. Vega, Rehovot, Israel ; J. Rocha et L. Mafra, Aveiro, Portugal ; S. Antonijevic, Berkeley, USA.; F. Deng, Wuhan, China ; Maria Alba, ICSM-CSIC, Sevilla ; Mostafa Taoufik, LC2P2, Lyon ; Laurent Maron, LPCNO, Toulouse ; F. Aussenac, Bruker BioSpin, Wissembourg, France ; M. Rosay, Bruker BioSpin, Billerica, USA ; Y. Nishiyama, JEOL Resonance, Tokyo, Japan ; B. Hu, East China Normal University, Shanghai, China ; T. Polenova, Univ. Delaware, Newark, USA ; K. Takegoshi, Univ. Kyoto, Japan; Marek J. Potrzebowski Polish Academy of Sciences, Lodz, Poland.  

 

Principaux équipements utilises par l’équipe :

- Notre équipe est fortement impliquée dans le groupement scientifique RMN du Nord-Pas de Calais (GS-RMN). Nous disposons d’équipements de pointe dans le cadre du centre de RMN de Lille (7 spectromètres de 100 à 800 et 900 MHz ).

- La Plateforme RMN de Lille est un des 5 sites d’accueil de la Très Grande Infrastructure de Recherche (TGIR) en RMN à très haut-champ. http://www.tgir-rmn.org/

- Atelier de verre (élaboration de verre jusqu'à 1600 ° C, traitements thermiques sous atmosphère contrôlée)

- Analyses thermiques (DSC, TGA-DTA-MS, TMA)

- Microscopie de chauffage (1400 ° C)

- Viscosimètre à plaques parallèles (jusqu'à 1000 ° C)

- Diffraction des rayons X (mono-cristaux, poudres, haute-température, atm. contrôlée)

- Microsonde électronique, fluorescence X

- Analyses de surface (XPS)

- Equipement d'enrichissement isotopique (17O)

 

Animation scientifique :

  • International solid-state NMR workshop: Kyoto, Japon, Mai 2009 ; Wuhan, Chine, Novembre 2009 ; Puebla, Mexique, avril 2011 ; Pune, Inde, juillet 2011 ; Dalian, Chine, Mai 2013.
  • Organisation d’une école d’été sur la RMN des solides : Sevilla, Espagne, Sept. de 2008 à 2012
  • Formations de RMN liquide et solide, deux fois par an au centre de RMN de l'USTL ((http://www.univ-lille1.fr/rmn)

Etudiants en thèse et post-docs :

 

Creton E.

Thèse

Elaboration et caractérisation de protection anti-oxydation des composites SiC/SiC

CIFRE SNECMA

2006 2009

Vasconcelos F.

Thèse

Calculs DFT appliqués aux paramètres RMN de noyaux quadripolaires

A MRES

2006 2009

Coillot D.

Thèse

Composites autocicatrisants pour le scellement de SOFC

AM MRES

2007 2010

Forler N.

Thèse

Application of high-field 17O solid-state NMR to the study of phosphate glass hydration

A MRES

2008 2010

Hu B.

Thèse

Manipulation des interactions dipolaires en RMN à l'état solide.

COLLTERR NPdC

2006 2009

Wang Q.

Thèse

Observation par RMN des proximités homonucléaires entre noyaux de spin-1/2 ou quadripolaires

Affaires étrangères

2008 2010

Lu X.

Thèse

Méthodologie RMN pour les solides

Bruker Région NPdC

2010-2013

Lilly Thankamony A.S.

Thèse

Synergie RMN-RPE: développement de la DNP-RMN pour l’étude des matériaux

A MRES label président

2010 2013

Rajbhandari P.

Thèse

RMN haut-champ pour la caractérisation avancée de verres de phosphate dopés

BDI CNRS-Région

2010 2013

Castanie S.

Thèse

verres auto cicatrisants haute Température

DGA

2010 2013

Lemesle T.

Thèse

Etude et caractérisation structurale de verres pour le confinement de l'iode

CEA

2010 2013

Gatoux A.

Thèse

Protection Anti-Oxydation à haute température pour matériaux composites C/C

Contrat Messier Bugatti

2010 2013

Girard G.

Thèse

Structural Characterization of disorder by solid-state NMR and DFT calculations

Ministère Lille 1 Région

2012-2015

Shen M.

Thèse

Corrélation homonucléaire à haute vitesse et haut champ magnétique dans les matériaux innovants 

CSC-Chine

2012-2015

Li X.

Thèse

Distances et proximités entre spin-1/2-noyaux quadripolaires dans les matériaux hybrides et inorganiques

CSC-Chine

2012-2015

Duong N. T.

Thèse

Caractérisation des matériaux poreux nanostructurés par DNP-RMN

BDI CNRS-CEA

2012-2015

Perez S.

Post-doc

Mise au point d’un traitement cosmétique pour composites aéronautiques

SNECMA - ARCOCE

2009-2010

Pavon-Gonzales E.

Post-doc

RMN de matériaux silicates désordonnés.

Lille1

2011-2012

Pourpoint F.

ATER

Mesure de distances 13C-27Al dans les solides

ENSCL

Sept2011- août 2012

Grekov D

Thèse

Caractérisation par RMN avancée de systèmes catalytiques  

ANR

Sept. 2013-Août 2016

 

Publications

Dans la base de données : 187
  • 2017

  • Aluminosilicate glass thin films elaborated by pulsed laser deposition.
    Carlier Thibault, Saitzek Sébastien, Méar François O., Blach Jean-François, Ferri Anthony, Huvé Marielle, Montagne Lionel.
    Applied Surface Science, vol. 397, pg. 13-18 (2017) DOI
     
  • Well defined molybdenum oxo alkyl complex supported on silica by surface organometallic chemistry: A highly active olefin metathesis pre-catalyst.
    Merle Nicolas, Le Quéméner Frédéric, Bouhoute Yassine, Szeto Kai C., De Mallmann Aimery, Barman Samir, Samantaray Manoja K, Delevoye Laurent, Gauvin Régis M., Taoufik Mostafa, Basset Jean Marie.
    Journal of the American Chemical Society, vol. 139, pg. 2144-2147 (2017) DOI
     
  • 2016

  • Characterization and structural investigation of lead borophosphate glasses modified by tungsten oxide.
    Koudelka Ladislav, Rösslerová Ivana, Kalenda Petr, Mošner Petr, Montagne Lionel, Revel Bertrand.
    Journal of Alloys and Compounds, vol. 658, pg. 377-384 (2016) DOI
     
  • Silica/MAO/(n-BuCp)2ZrCl2catalyst: effect of support dehydroxylation temperature on the grafting of MAO and ethylene polymerization.
    Bashir Muhammad Ahsan, Vancompernolle Tom, Gauvin Régis M., Delevoye Laurent, Merle Nicolas, Monteil Vincent, Taoufik Mostafa, McKenna Timothy F. L., Boisson Christophe.
    Catal. Sci. Technol., vol. 6, pg. 2962-2974 (2016) DOI
     
  • Development of silica-supported frustrated Lewis pairs: highly active transition metal-free catalysts for the Z-selective reduction of alkynes.
    Szeto Kai C., Sahyoun Wissam, Merle Nicolas, Castelbou Jessica Llop, Popoff Nicolas, Lefebvre Frédéric, Raynaud Jean, Godard Cyril, Claver Carmen, Delevoye Laurent, Gauvin Régis M., Taoufik Mostafa.
    Catal. Sci. Technol., vol. 6, pg. 882-889 (2016) DOI
     
  • The design of a bipodal bis(pentafluorophenoxy)aluminate supported on silica as an activator for ethylene polymerization using surface organometallic chemistry.
    Sauter Dominique W., Popoff Nicolas, Bashir Muhammad Ahsan, Szeto Kai C., Gauvin Régis M., Delevoye Laurent, Taoufik Mostafa, Boisson Christophe.
    Chem. Commun., vol. 52, pg. 4776-4779 (2016) DOI
     
  • Self-Healing Glassy Thin Coating for High-Temperature Applications.
    Castanié Sandra, Carlier Thibault, Méar François O., Saitzek Sébastien, Blach Jean-François, Podor Renaud, Montagne Lionel.
    ACS Applied Materials < Interfaces, vol. 8, pg. 4208-4215 (2016) DOI
     
  • Structural investigation of BaOB2O3P2O5 glasses by NMR and Raman spectroscopy.
    Koudelka Ladislav, Kalenda Petr, Mošner Petr, Černošek Zdeněk, Montagne Lionel, Revel Bertrand.
    Journal of Molecular Structure, vol. 1119, pg. 212-219 (2016) DOI
     
  • Structure and thermochemical study of strontium sodium phosphate glasses.
    Cherbib Mohamed Atef, Krimi Saida, El Jazouli Abdelaziz, Khattech Ismail, Montagne Lionel, Revel Bertrand, Jemal Mohamed.
    Journal of Non-Crystalline Solids, vol. 447, pg. 59-65 (2016) DOI
     
  • Ligand exchange-mediated activation and stabilization of a Re-based olefin metathesis catalyst by chlorinated alumina.
    Gallo Alessandro, Fong Anthony, Szeto Kai Chung, Rieb Julia, Delevoye Laurent, Gauvin Régis M., Taoufik Mostafa, Peters Baron, Scott Susannah L.
    Journal of the American Chemical Society, (2016) DOI
     
  • Silica-Supported Tungsten Neosilyl Oxo Precatalysts: Impact of the Podality on Activity and Stability in Olefin Metathesis.
    Grekov D., Bouhoute Y., Szeto K. C., Merle N., De Mallmann A., Lefebvre F., Lucas C., Del Rosal I., Maron L., Gauvin R. M., Delevoye L., Taoufik M.
    Organometallics, vol. 35 (13), pg. 2188-2196 (2016) DOI
     
  • Statistics of silicate units in binary glasses.
    Gaddam Anuraag, Montagne Lionel, Ferreira José M. F.
    The Journal of Chemical Physics, vol. 145, pg. 124505 (2016) DOI
     
  • Stability of metal–organic frameworks under gamma irradiation.
    Volkringer C., Falaise C., Devaux P., Giovine R., Stevenson V., Pourpoint F., Lafon O., Osmond M., Jeanjacques C., Marcillaud B., Sabroux J. C., Loiseau T.
    Chem. Commun., vol. 52, pg. 12502-12505 (2016) DOI
     
  • Macromol. Rapid Commun. 22/2016.
    Larabi Cherif, Szeto Kai C., Bouhoute Yassine, Charlin Marc O., Merle Nicolas, Mallmann Aimery De, Gauvin Regis M., Delevoye Laurent, Taoufik Mostafa.
    Macromolecular Rapid Communications, vol. 37, pg. 1848-1848 (2016) DOI
     
  • 17O MAS NMR studies of oxo-based olefin metathesis catalysts: a critical assessment of signal enhancement methods.
    Grekov D., Bouhoute Y., Del Rosal I., Maron L., Taoufik M., Gauvin R. M., Delevoye L.
    Phys. Chem. Chem. Phys., vol. 18, pg. 28157-28163 (2016) DOI
     
  • Modification of silica-supported tungsten neosilyl oxo precatalysts: impact of substituted phenol on activity and stability in olefin metathesis.
    Bouhoute Y., Del Rosal I., Szeto K. C., Merle N., Grekov D., De Mallmann A., Le Roux E., Delevoye L., Gauvin R. M., Maron L., Taoufik M.
    Catal. Sci. Technol., vol. 6, pg. 8532-8539 (2016) DOI
     
  • 2015

  • Selective Secondary Face Modification of Cyclodextrins by Mechanosynthesis.
    Menuel Stéphane, Doumert Bertrand, Saitzek Sébastien, Ponchel Anne, Delevoye Laurent, Monflier Eric, Hapiot Frédéric.
    The Journal of Organic Chemistry, vol. 80, pg. 6259-6266 (2015) DOI
     
  • Effect of post treatment on the local structure of hierarchical Beta prepared by desilication and the catalytic performance in Friedel–Crafts alkylation.
    Wang Yi, Sun Yinyong, Lancelot Christine, Lamonier Carole, Morin Jean-Charles, Revel Bertrand, Delevoye Laurent, Rives Alain.
    Microporous and Mesoporous Materials, vol. 206, pg. 42-51 (2015) DOI
     
  • Investigation of zinc alkali pyrophosphate glasses. Part I: Development of low-Tg and high stability glasses.
    Rajbhandari P., Montagne L., Tricot G.
    Materials Chemistry and Physics, vol. 155, pg. 17-22 (2015) DOI
     
  • Investigation of zinc alkali pyrophosphate glasses. Part II: Local and medium range orders analysed by 1D/2D NMR.
    Rajbhandari P., Chen Y., Doumert B., Montagne L., Tricot G.
    Materials Chemistry and Physics, vol. 155, pg. 23-29 (2015) DOI
     
  • Matériaux vitreux auto-cicatrisants pour application à haute température, élaborés sous forme de couches minces.
    Carlier Thibault, Méar François O., Saitzek Sébastien, Blach Jean-François, Podor Renaud, Montagne Lionel.
    Matériaux < Techniques, vol. 103, pg. 406 (2015) DOI
     
  • Glass-forming ability, structure and physical properties of ZnO-In2O3-P2O5 glasses.
    Petr Mosner, Ladislav Koudelka, Antonin Racicky, Lionel Montagne, Bertrand Revel.
    Phys. Chem. Glasses: Eur. J. Glass Sci. Technol. B, vol. 56 (4), pg. 121-127 (2015) DOI
     
  • Accessing Realistic Models for the WO3–SiO2Industrial Catalyst through the Design of Organometallic Precursors.
    Bouhoute Y., Grekov D., Szeto K. C., Merle N., De Mallmann A., Lefebvre F., Raffa G., Del Rosal I., Maron L., Gauvin R. M., Delevoye L., Taoufik M.
    ACS Catalysis, pg. 1-18 (2015) DOI
     
  • Selective Grafting of Ga(i-Bu)3on the Silanols of Mesoporous H-ZSM-5 by Surface Organometallic Chemistry.
    Szeto Kai C., Gallo Alessandro, Hernández-Morejudo Selene, Olsbye Unni, De Mallmann Aimery, Lefebvre Frédéric, Gauvin Régis M., Delevoye Laurent, Scott Susannah L., Taoufik Mostafa.
    The Journal of Physical Chemistry C, vol. 119, pg. 26611-26619 (2015) DOI
     
  • 2D- and 3D Observation and Mechanism of Self-Healing in Glass-Boron Composites.
    Castanié Sandra, Méar Francois O., Podor Renaud, Suhonen Heikki, Montagne Lionel, Riemanis I.
    Journal of the American Ceramic Society, pg. 1-7 (2015) DOI
     
  • Bismuth-silver phosphate glasses as alternative matrices for the conditioning of radioactive iodine.
    Lemesle Thomas, Montagne Lionel, Méar * François O, Revel Bertrand, Campayo Lionel, Pinet Olivier.
    Eur. J. Glass Sci. Technol. B, vol. 56 (2), pg. 71-75 (2015)
     
  • Investigation of (100−x)[0.5PbO.0.2B2O3.0.3P2O5] .xMoO3 glasses.
    Rösslerová Ivana, Koudelka Ladislav, Holubová * Jana, Mošner Petr, Montagne Lionel, Revel Bertrand.
    Eur. J. Glass Sci. Technol. B, vol. 56 (1), pg. 1-7 (2015)
     
  • Insights into the Catalytic Activity of Nitridated Fibrous Silica (KCC-1) Nanocatalysts from15N and29Si NMR Spectroscopy Enhanced by Dynamic Nuclear Polarization.
    Lilly Thankamony Aany Sofia, Lion Cédric, Pourpoint Frédérique, Singh Baljeet, Perez Linde Angel J., Carnevale Diego, Bodenhausen Geoffrey, Vezin Hervé, Lafon Olivier, Polshettiwar Vivek.
    Angewandte Chemie International Edition, vol. 54, pg. 2190-2193 (2015) DOI
     
  • 2014

  • Immobilization of radioactive iodine in silver aluminophosphate glasses.
    Lemesle Thomas, Méar François O., Campayo Lionel, Pinet Olivier, Revel Bertrand, Montagne Lionel.
    Journal of Hazardous Materials, vol. 264, pg. 117-126 (2014) DOI
     
  • The structure and properties of zinc aluminophosphate glasses.
    Smith Charmayne E., Brow Richard K., Montagne Lionel, Revel Bertrand.
    Journal of Non-Crystalline Solids, vol. 386, pg. 105-114 (2014) DOI
     
  • Labile Degree of Disorder in Bismuth-Oxophosphate Compounds: Illustration through Three New Structural Types.
    Aliev A., Endara D., Huvé M., Colmont M., Roussel P., Delevoye L., Tran T.T., Halasyamani P.S., Mentré O.
    Inorganic Chemistry, vol. 53, pg. 861-871 (2014) DOI
     
  • Probing 27Al–13C proximities in metal–organic frameworks using dynamic nuclear polarization enhanced NMR spectroscopy.
    Pourpoint Frédérique, Thankamony Aany Sofia Lilly, Volkringer Christophe, Loiseau Thierry, Trébosc Julien, Aussenac Fabien, Carnevale Diego, Bodenhausen Geoffrey, Vezin Hervé, Lafon Olivier, Amoureux Jean-Paul.
    Chemical Communications, vol. 50, pg. 933 (2014) DOI
     
  • Structural, textural and acid–base properties of carbonate-containing hydroxyapatites.
    Silvester Lishil, Lamonier Jean-François, Vannier Rose-Noëlle, Lamonier Carole, Capron Mickaël, Mamede Anne-Sophie, Pourpoint Frédérique, Gervasini Antonella, Dumeignil Franck.
    Journal of Materials Chemistry A, vol. 2, pg. 11073-11090 (2014) DOI
     
  • The structural role of tellurium dioxide in lead borophosphate glasses.
    Koudelka Ladislav, Rösslerová Ivana, Černošek Zdeněk, Mošner Petr, Montagne Lionel, Revel Bertrand.
    Journal of Non-Crystalline Solids, vol. 401, pg. 124-128 (2014) DOI
     
  • Behavior of indium oxide in zinc phosphate and borophosphate glasses.
    Koudelka Ladislav, Račický Antonín, Mošner Petr, Rösslerová Ivana, Montagne Lionel, Revel Betrand.
    Journal of Materials Science, vol. 49, pg. 6967-6974 (2014) DOI
     
  • An Investigation of Chlorine Ligands in Transition-Metal Complexes via35Cl Solid-State NMR and Density Functional Theory Calculations.
    O’Keefe Christopher A., Johnston Karen E., Sutter Kiplangat, Autschbach Jochen, Gauvin Régis, Trébosc Julien, Delevoye Laurent, Popoff Nicolas, Taoufik Mostafa, Oudatchin Konstantin, Schurko Robert W.
    Inorganic Chemistry, vol. 53, pg. 9581-9597 (2014) DOI
     
  • Enforcing Z-selectivity in olefin metathesis through use of catalysts grafted on well-defined phenolic hybrid material.
    Popoff Nicolas, Szeto Kai C., Merle Nicolas, Espinas Jeff, Pelletier Jérémie, Lefebvre Frederic, Thivolle-Cazat Jean, Delevoye Laurent, De Mallmann Aimery, Gauvin Regis M., Taoufik Mostafa.
    Catalysis Today, vol. 235, pg. 41-48 (2014) DOI
     
  • Heteronuclear NMR Spectroscopy as a Surface-Selective Technique: A Unique Look at the Hydroxyl Groups of γ-Alumina..
    Taoufik Mostafa, Szeto Kai C., Merle Nicolas, Rosal Iker Del, Maron Laurent, Trébosc Julien, Tricot Grégory, Gauvin Régis M., Delevoye Laurent.
    Chemistry - A European Journal, vol. 20, pg. 4038-4046 (2014) DOI
     
  • Heteronuclear NMR Spectroscopy as Surface-Selective Technique: A Unique Look at the Hydroxyl Groups of γ-Alumina.
    Taoufik Mostafa, Szeto Kai C., Merle Nicolas, Rosal Iker Del, Maron Laurent, Trébosc Julien, Tricot Grégory, Gauvin Régis M., Delevoye Laurent.
    Chemistry - A European Journal, vol. 20, pg. 3856-3856 (2014) DOI
     
  • The D-HMQC MAS-NMR Technique.
    Tricot Gregory, Trébosc Julien, Pourpoint Frédérique, Gauvin Régis, Delevoye Laurent.
    annu. Rep. NMR, vol. 81, pg. 145-184 (2014) DOI
     
  • Correlation 2D-NMR experiments involving both13C and2H isotopes in oriented media: methodological developments and analytical applications.
    Lesot Philippe, Lafon Olivier, Berdagué Philippe.
    Magnetic Resonance in Chemistry, vol. 52, pg. 595-613 (2014) DOI
     
  • Improving the resolution in proton-detected through-space heteronuclear multiple quantum correlation NMR spectroscopy.
    Shen Ming, Trébosc J., Lafon O., Pourpoint F., Hu Bingwen, Chen Qun, Amoureux J.-P.
    Journal of Magnetic Resonance, vol. 245, pg. 38-49 (2014) DOI
     
  • Primostrato Solid-State NMR Enhanced by Dynamic Nuclear Polarization: Pentacoordinated Al3+Ions Are Only Located at the Surface of Hydrated γ-Alumina.
    Lee Daniel, Duong Nghia Tuan, Lafon Olivier, De Paëpe Gaël.
    The Journal of Physical Chemistry C, vol. 118, pg. 25065-25076 (2014) DOI
     
  • Criteria for sensitivity enhancement by compressed sensing: practical application to anisotropic NAD 2D-NMR spectroscopy.
    Kazimierczuk Krzysztof, Lafon Olivier, Lesot Philippe.
    The Analyst, vol. 139, pg. 2702 (2014) DOI
     
  • Quantitative Analysis of the Proximities of OH Ligands and Vanadium Sites in a Polyoxovanadate Cluster Using Frequency-Selective1H–51V Solid-State NMR Spectroscopy.
    Pourpoint Frédérique, Trébosc Julien, Bonhomme Christian, Durupthy Olivier, Steunou Nathalie, Lafon Olivier, Amoureux Jean-Paul.
    The Journal of Physical Chemistry C, vol. 118, pg. 18580-18588 (2014) DOI
     
  • Well-Defined Supported Mononuclear Tungsten Oxo Species as Olefin Metathesis Pre-Catalysts.
    Bouhoute Yassine, Garron Anthony, Grekov Denys, Merle Nicolas, Szeto Kai C., De Mallmann Aimery, Del Rosal Iker, Maron Laurent, Girard Guillaume, Gauvin Régis M., Delevoye Laurent, Taoufik Mostafa.
    ACS Catalysis, vol. 4, pg. 4232-4241 (2014) DOI
     
  • Host–Guest Interactions in Dealuminated HY Zeolite Probed by13C–27Al Solid-State NMR Spectroscopy.
    Li Shenhui, Pourpoint Frédérique, Trébosc Julien, Zhou Lei, Lafon Olivier, Shen Ming, Zheng Anmin, Wang Qiang, Amoureux Jean-Paul, Deng Feng.
    The Journal of Physical Chemistry Letters, vol. 5, pg. 3068-3072 (2014) DOI
     
  • Direct evidence of Lowenstein<#039;s rule violation in swelling high-charge micas.
    Pavón E., Osuna F. J., Alba M. D., Delevoye L.
    Chemical Communications, vol. 50, pg. 6984 (2014) DOI
     
  • Characterising local environments in high energy density Li-ion battery cathodes: a combined NMR and first principles study of LiFexCo1−xPO4.
    Strobridge Fiona C., Middlemiss Derek S., Pell Andrew J., Leskes Michal, Clément Raphaële J., Pourpoint Frédérique, Lu Zhouguang, Hanna John V., Pintacuda Guido, Emsley Lyndon, Samoson Ago, Grey Clare P.
    Journal of Materials Chemistry A, vol. 2, pg. 11948 (2014) DOI
     
  • 2013

  • Design and Application of a Hybrid Material Featuring Well-Defined, Tuneable Grafting Sites for Supported Catalysis..
    Popoff Nicolas, Espinas Jeff, Pelletier Jérémie, Szeto Kai C., Thivolle-Cazat Jean, Delevoye Laurent, Gauvin Régis M., Taoufik Mostafa.
    ChemCatChem, vol. 5 (7), pg. 1971-1977 (2013) DOI
     
  • Description of the Intermediate Length Scale Structural Motifs in Sodium Vanado-phosphate Glasses by Magnetic Resonance Spectroscopies.
    Tricot Gregory, Vezin Hervé.
    The Journal of Physical Chemistry C, vol. 117, pg. 1421-1427 (2013) DOI
     
  • Study of the thermal degradation of an aluminium phosphinate–aluminium trihydrate combination.
    Duquesne Sophie, Fontaine Gaëlle, Cérin-Delaval Oriane, Gardelle Bastien, Tricot Grégory, Bourbigot Serge.
    Thermochimica Acta, vol. 551, pg. 175-183 (2013) DOI
     
  • Structural characterization of an electrically insulating diffusion barrier on a plasma-sprayed ceramic for severe environment applications.
    Joly Alexandre, Brun Patrice, Lacombe Jacques, Tricot Grégory, Denoirjean Alain.
    Surface and Coatings Technology, vol. 220, pg. 204-208 (2013) DOI
     
  • Structure of Nb2O5–NaPO3 glasses by X-ray and neutron diffraction.
    Hoppe U., Delevoye L., Montagne L., Zimmermann M. v., Hannon A. C.
    Physical Chemistry Chemical Physics, vol. 15 (22), pg. 8520-8528 (2013) DOI
     
  • New insights into the structure of oxynitride NaPON phosphate glasses by 17-oxygen NMR.
    Muñoz F., Delevoye L., Montagne L., Charpentier T.
    Journal of Non-Crystalline Solids, vol. 363, pg. 134-139 (2013) DOI
     
  • Extended Czjzek model applied to NMR parameter distributions in sodium metaphosphate glass.
    Vasconcelos Filipe, Cristol Sylvain, Paul Jean-François, Delevoye Laurent, Mauri Francesco, Charpentier Thibault, Le Caër Gérard.
    Journal of Physics: Condensed Matter, vol. 25, pg. 255402 (2013) DOI
     
  • Probing proximities between different quadrupolar isotopes using multi-pulse cross-polarization.
    Lu Xingyu, Tankamony Aany Sofia Lilly, Trébosc Julien, Lafon Olivier, Amoureux Jean-Paul.
    Journal of Magnetic Resonance, vol. 228, pg. 148-158 (2013) DOI
     
  • Mesoporous Silica Nanoparticles Loaded with Surfactant: Low Temperature Magic Angle Spinning13C and29Si NMR Enhanced by Dynamic Nuclear Polarization.
    Lafon Olivier, Thankamony Aany S. Lilly, Kobayashi Takeshi, Carnevale Diego, Vitzthum Veronika, Slowing Igor I., Kandel Kapil, Vezin Hervé, Amoureux Jean-Paul, Bodenhausen Geoffrey, Pruski Marek.
    The Journal of Physical Chemistry C, vol. 117, pg. 1375-1382 (2013) DOI
     
  • Analysis of sensitivity enhancement by dynamic nuclear polarization in solid-state NMR: a case study of functionalized mesoporous materials.
    Kobayashi Takeshi, Lafon Olivier, Lilly Thankamony Aany S., Slowing Igor I., Kandel Kapil, Carnevale Diego, Vitzthum Veronika, Vezin Hervé, Amoureux Jean-Paul, Bodenhausen Geoffrey, Pruski Marek.
    Physical Chemistry Chemical Physics, vol. 15, pg. 5553 (2013) DOI
     
  • Indirect and direct 29Si dynamic nuclear polarization of dispersed nanoparticles.
    Lafon Olivier, Thankamony Aany Sofia Lilly, Rosay Melanie, Aussenac Fabien, Lu Xingyu, Trébosc Julien, Bout-Roumazeilles Viviane, Vezin Hervé, Amoureux Jean-Paul.
    Chemical Communications, vol. 49, pg. 2864-2866 (2013) DOI
     
  • Comparison of various sampling schemes and accumulation profiles in covariance spectroscopy with exponentially decaying 2D signals.
    Li Yixuan, Hu Bingwen, Chen Qun, Wang Qiang, Zhang Zhengfeng, Yang Jun, Noda Isao, Trébosc Julien, Lafon Oliver, Amoureux Jean-Paul, Deng Feng.
    The Analyst, vol. 138, pg. 2411 (2013) DOI
     
  • Understanding the High Photocatalytic Activity of (B, Ag)-Codoped TiO2under Solar-Light Irradiation with XPS, Solid-State NMR, and DFT Calculations.
    Feng Ningdong, Wang Qiang, Zheng Anmin, Zhang Zhengfeng, Fan Jie, Liu Shang-Bin, Amoureux Jean-Paul, Deng Feng.
    Journal of the American Chemical Society, vol. 135, pg. 1607-1616 (2013) DOI
     
  • An NMR-Driven Crystallography Strategy to Overcome the Computability Limit of Powder Structure Determination: A Layered Aluminophosphate Case.
    Bouchevreau Boris, Martineau Charlotte, Mellot-Draznieks Caroline, Tuel Alain, Suchomel Matthew R., Trébosc Julien, Lafon Olivier, Amoureux Jean-Paul, Taulelle Francis.
    Chemistry - A European Journal, vol. 19, pg. 5009-5013 (2013) DOI
     
  • High-Resolution Structural Characterization of Two Layered Aluminophosphates by Synchrotron Powder Diffraction and NMR Crystallographies.
    Bouchevreau Boris, Martineau Charlotte, Mellot-Draznieks Caroline, Tuel Alain, Suchomel Matthew R., Trébosc Julien, Lafon Olivier, Amoureux Jean-Paul, Taulelle Francis.
    Chemistry of Materials, vol. 25, pg. 2227-2242 (2013) DOI
     
  • Broadband homonuclear correlation spectroscopy driven by combined sequences under fast magic angle spinning for NMR structural analysis of organic and biological solids.
    Hou Guangjin, Yan Si, Trébosc Julien, Amoureux Jean-Paul, Polenova Tatyana.
    Journal of Magnetic Resonance, vol. 232, pg. 18-30 (2013) DOI
     
  • Simple and accurate determination of X–H distances under ultra-fast MAS NMR.
    Paluch Piotr, Pawlak Tomasz, Amoureux Jean-Paul, Potrzebowski Marek J.
    Journal of Magnetic Resonance, vol. 233, pg. 56-63 (2013) DOI
     
  • Signal enhancement of J-HMQC experiments in solid-state NMR involving half-integer quadrupolar nuclei.
    Wang Qiang, Trébosc Julien, Li Yixuan, Xu Jun, Hu Bingwen, Feng Ningdong, Chen Qun, Lafon Olivier, Amoureux Jean-Paul, Deng Feng.
    Chemical Communications, vol. 49, pg. 6653-6655 (2013) DOI
     
  • A study of transition-metal organometallic complexes combining 35Cl solid-state NMR, 35Cl NQR and first-principles DFT calculations.
    Johnston K E, O’Keefe C A, Gauvin R M, Trébosc J, Delevoye L, Amoureux J -P, Popoff N, Taoufik M, Oudatchin K, Schurko R W.
    Chemistry - A European Journal, (2013) DOI
     
  • Influence of Au addition on magnetic properties of iron oxide in a silica–phosphate glass matrix.
    Sharma K., Prajapat C.L., Meena Sher Singh, Singh M.R., Yusuf S.M., Montagne L., Kothiyal G.P.
    Journal of Magnetism and Magnetic Materials, vol. 345, pg. 24-28 (2013) DOI
     
  • Measurement of the shortest hetero-nuclear distances in multiple-spin systems using constant-time correlation NMR methods.
    Amoureux Jean-Paul, Lu Xingyu, Trébosc Julien, Lafon Olivier.
    CrystEngComm, (2013) DOI
     
  • 95Mo Solid-State Nuclear Magnetic Resonance Spectroscopy and Quantum Simulations: Synergetic Tools for the Study of Molybdenum Cluster Materials.
    Cuny Jérôme, Cordier Stéphane, Perrin Christiane, Pickard Chris J., Delevoye Laurent, Trébosc Julien, Gan Zhehong, Pollès Laurent Le, Gautier Régis.
    Inorganic Chemistry, vol. 52, pg. 617-627 (2013) DOI
     
  • 71Ga NMR in chalcogenide and chalco-halide glasses.
    Ledemi Yannick, Bureau Bruno, Le Caër Gérard, Calvez Laurent, Roiland Claire, Tricot Grégory, Florian Pierre, Nazabal Virginie, Massiot Dominique.
    Journal of Non-Crystalline Solids, (2013) DOI
     
  • Broadband excitation in solid-state NMR using interleaved DANTE pulse trains with N pulses per rotor period.
    Lu Xingyu, Trébosc Julien, Lafon Olivier, Carnevale Diego, Ulzega Simone, Bodenhausen Geoffrey, Amoureux Jean-Paul.
    Journal of Magnetic Resonance, vol. 236, pg. 105-116 (2013) DOI
     
  • Synergic effect of V2O5 and P2O5 on the sealing properties of barium–strontium–alumino-silicate glass/glass–ceramics.
    Sharma K., Kothiyal G.P., Montagne L., Méar F.O., Revel B.
    International Journal of Hydrogen Energy, vol. 38, pg. 15542-15552 (2013) DOI
     
  • Advances in Structural Studies on Alkylaluminum Species in the Solid State via Challenging27Al–13C NMR Spectroscopy and X-ray Diffraction.
    Pourpoint Frédérique, Morin Yohann, Gauvin Régis M., Trébosc Julien, Capet Frédéric, Lafon Olivier, Amoureux Jean-Paul.
    The Journal of Physical Chemistry C, vol. 117, pg. 18091-18099 (2013) DOI
     
  • On the Track to Silica-Supported Tungsten Oxo Metathesis Catalysts: Input from17O Solid-State NMR.
    Merle Nicolas, Girard Guillaume, Popoff Nicolas, De Mallmann Aimery, Bouhoute Yassine, Trébosc Julien, Berrier Elise, Paul Jean-François, Nicholas Christopher P., Del Rosal Iker, Maron Laurent, Gauvin Régis M., Delevoye Laurent, Taoufik Mostafa.
    Inorganic Chemistry, vol. 52, pg. 10119-10130 (2013) DOI
     
  • Vanadium Oxo Organometallic Species Supported on Silica for the Selective Non-oxidative Dehydrogenation of Propane.
    Szeto Kai C., Loges Björn, Merle Nicolas, Popoff Nicolas, Quadrelli Alessandra, Jia Hongpeng, Berrier Elise, De Mallmann Aimery, Delevoye Laurent, Gauvin Régis M., Taoufik Mostafa.
    Organometallics, vol. 32, pg. 6452-6460 (2013) DOI
     
  • 2012

  • The mixed glass former effect in twin-roller quenched lithium borophosphate glasses.
    Raguenet B., Tricot G., Silly G., Ribes M., Pradel A.
    Solid State Ionics, vol. 208, pg. 25-30 (2012) DOI
     
  • Detailed analysis of the S-RESPDOR solid-state NMR method for inter-nuclear distance measurement between spin-1/2 and quadrupolar nuclei.
    Lu Xingyu, Lafon Olivier, Trébosc Julien, Amoureux Jean-Paul.
    Journal of Magnetic Resonance, vol. 215, pg. 34-49 (2012) DOI
     
  • Novel Tailormade Bi4MO4(PO4)2Structural Type (M = Mg, Zn).
    Endara Diana, Colmont Marie, Huvé Marielle, Tricot Grégory, Carpentier Laurent, Mentré Olivier.
    Inorganic Chemistry, vol. 51, pg. 4438-4447 (2012) DOI
     
  • High-resolution through-space correlations between spin-1/2 and half-integer quadrupolar nuclei using the MQ-D-R-INEPT NMR experiment.
    Martineau Charlotte, Bouchevreau Boris, Taulelle Francis, Trébosc Julien, Lafon Olivier, Paul Amoureux Jean.
    Physical Chemistry Chemical Physics, vol. 14, pg. 7112 (2012) DOI
     
  • Practical choice of 1H–1H decoupling schemes in through-bond 1H–{X} HMQC experiments at ultra-fast MAS.
    Nishiyama Yusuke, Lu Xingyu, Trébosc Julien, Lafon Olivier, Gan Zhehong, Madhu P.K., Amoureux Jean-Paul.
    Journal of Magnetic Resonance, vol. 214, pg. 151-158 (2012) DOI
     
  • Quantitative cross-polarization at magic-angle spinning frequency of about 20kHz.
    Takeda Kazuyuki, Noda Yasuto, Takegoshi K., Lafon Olivier, Trébosc Julien, Amoureux Jean-Paul.
    Journal of Magnetic Resonance, vol. 214, pg. 340-345 (2012) DOI
     
  • Inhibition of the catalytic oxidation of carbon/carbon composite materials by an aluminophosphate coating.
    Tricot Grégory, Nicolaus Nathalie, Diss Pascal, Montagne Lionel.
    Carbon, vol. 50, pg. 3440-3445 (2012) DOI
     
  • A new formulation of barium–strontium silicate glasses and glass-ceramics for high-temperature sealant.
    Sharma K., Kothiyal G.P., Montagne L., Méar F.O., Revel B.
    International Journal of Hydrogen Energy, (2012) DOI
     
  • Development and characterization of glass-ceramic sealants in the (CaO–Al2O3–SiO2–B2O3) system for Solid Oxide Electrolyzer Cells.
    Khedim Hichem, Nonnet Hélène, Méar François O.
    Journal of Power Sources, vol. 216, pg. 227-236 (2012) DOI
     
  • New viscous sealing glasses for electrochemical cells.
    Coillot Daniel, Méar François O., Nonnet Hélène, Montagne Lionel.
    International Journal of Hydrogen Energy, vol. 37, pg. 9351-9358 (2012) DOI
     
  • Development and characterisation of glass and glass ceramic sealants for solid oxide electrolyser cells.
    Nonnet Hélène, Khedim Hichem, Méar François O.
    Ionics, vol. 18, pg. 441-447 (2012) DOI
     
  • Solvent-Free High-Field Dynamic Nuclear Polarization of Mesoporous Silica Functionalized with TEMPO.
    Lilly Thankamony Aany Sofia, Lafon Olivier, Lu Xingyu, Aussenac Fabien, Rosay Melanie, Trébosc Julien, Vezin Hervé, Amoureux Jean-Paul.
    Applied Magnetic Resonance, vol. 43, pg. 237-250 (2012) DOI
     
  • 17O NMR Gives Unprecedented Insights into the Structure of Supported Catalysts and Their Interaction with the Silica Carrier.
    Merle Nicolas, Trébosc Julien, Baudouin Anne, Rosal Iker Del, Maron Laurent, Szeto Kai, Genelot Marie, Mortreux André, Taoufik Mostafa, Delevoye Laurent, Gauvin Régis M.
    Journal of the American Chemical Society, vol. 134, pg. 9263-9275 (2012) DOI
     
  • Observation of proximities between spin-1∕2 and quadrupolar nuclei: Which heteronuclear dipolar recoupling method is preferable?.
    Lu X., Lafon O., Trébosc J., Tricot G., Delevoye L., Méar F., Montagne L., Amoureux J. P.
    The Journal of Chemical Physics, vol. 137, pg. 144201 (2012) DOI
     
  • Some recent studies on glass/glass-ceramics for use as sealants with special emphasis for high temperature applications.
    Kothiyal G. P., Goswami Madhumita, Tiwari Babita, Sharma Kuldeep, Ananthanarayanan A., Montagne Lionel.
    Journal of Advanced Ceramics, vol. 1, pg. 110-129 (2012) DOI
     
  • Structural studies of boron and tellurium coordination in zinc borophosphate glasses by 11B MAS NMR and Raman spectroscopy.
    Vosejpková Kateřina, Koudelka Ladislav, Černošek Zdeněk, Mošner Petr, Montagne Lionel, Revel Bertrand.
    Journal of Physics and Chemistry of Solids, vol. 73, pg. 324-329 (2012) DOI
     
  • Structure and properties of lead tungstate phosphate glasses.
    Koudelka Ladislav, Šubčík Jiří, Mošner Petr, Gregora Ivan, Montagne Lionel, Delevoye Laurent.
    Phys. Chem. Glasses: Eur. J. Glass Sci. Technol. B, vol. 53 (3), pg. 86–92 (2012)
     
  • Glass-forming ability and structure of glasses in the ZnO–WO3–P2O5 system.
    Koudelka Ladislav, Šubčík Jiří, Mošner Petr, Gregora Ivan, Montagne Lionel, Delevoye Laurent.
    Phys. Chem. Glasses: Eur. J. Glass Sci. Technol. B, vol. 53 (3), pg. 79–85 (2012)
     
  • Fine Hierarchy of the V–O Bonds by Advanced Solid State NMR: Novel Pb4(VO2)(PO4)3Structure as a Textbook Case.
    Tricot Grégory, Mentré Olivier, Cristol Sylvain, Delevoye Laurent.
    Inorganic Chemistry, vol. 51, pg. 13108-13113 (2012) DOI
     
  • Triclinic–Cubic Phase Transition and Negative Expansion in the Actinide IV (Th, U, Np, Pu) Diphosphates.
    Wallez Gilles, Raison Philippe E., Dacheux Nicolas, Clavier Nicolas, Bykov Denis, Delevoye Laurent, Popa Karin, Bregiroux Damien, Fitch Andrew N., Konings Rudy J. M.
    Inorganic Chemistry, vol. 51, pg. 4314-4322 (2012) DOI
     
  • A facile route for preparing a mesoporous palladium coordination polymer as a recyclable heterogeneous catalyst.
    Zhang Siyong, Liu Qinghua, Shen Ming, Hu Bingwen, Chen Qun, Li Hexing, Amoureux Jean-Paul.
    Dalton Transactions, vol. 41, pg. 4692 (2012) DOI
     
  • Detailed analysis of the TIMES and TIMES0 high-resolution MAS methods for high-resolution proton NMR.
    Lu Xingyu, Lafon Olivier, Trébosc Julien, Thankamony Aany Sofia Lilly, Nishiyama Yusuke, Gan Zhehong, Madhu P.K., Amoureux Jean-Paul.
    Journal of Magnetic Resonance, vol. 223, pg. 219-227 (2012) DOI
     
  • Very-Long-Distance Correlations in Proteins Revealed by Solid-State NMR Spectroscopy.
    Hu Bingwen, Trébosc Julien, Lafon Oliver, Chen Qun, Masuda Yuichi, Takegoshi K., Amoureux Jean-Paul.
    ChemPhysChem, vol. 13, pg. 3585-3588 (2012) DOI
     
  • Uniform broadband excitation of crystallites in rotating solids using interleaved sequences of delays alternating with nutation.
    Vitzthum Veronika, Caporini Marc A., Ulzega Simone, Trébosc Julien, Lafon Olivier, Amoureux Jean-Paul, Bodenhausen Geoffrey.
    Journal of Magnetic Resonance, vol. 223, pg. 228-236 (2012) DOI
     
  • Broadband excitation in solid-state NMR of paramagnetic samples using Delays Alternating with Nutation for Tailored Excitation (‘Para-DANTE’).
    Carnevale Diego, Vitzthum Veronika, Lafon Olivier, Trébosc Julien, Amoureux Jean-Paul, Bodenhausen Geoffrey.
    Chemical Physics Letters, vol. 553, pg. 68-76 (2012) DOI
     
  • Measurement of Aluminum-Carbon Distances Using S-RESPDOR NMR Experiments.
    Pourpoint Frédérique, Trébosc Julien, Gauvin Régis M., Wang Qiang, Lafon Olivier, Deng Feng, Amoureux Jean-Paul.
    ChemPhysChem, vol. 13, pg. 3605-3615 (2012) DOI
     
  • Structure and properties of lead boro-phosphate glasses doped with molybdenum oxide.
    Koudelka L, Rosslerova I, Cernosek Z, Mosner P, Montagne L, Revel B, Tricot G.
    Phys. Chem. Glasses: Eur. J. Glass Sci. Technol. B, vol. 53, pg. 6 (2012)
     
  • Enhanced 2D solid-state NMR correlation spectroscopy of quadrupolar nuclei using dynamic nuclear polarization.
    Lee D, Takahashi H, Thankamony A S Lilly, Dacquin J -Ph, Bardet M, Lafon O, Paëpe G De.
    Journal of the American Chemical Society, vol. 134, pg. 18491 (2012) DOI
     
  • Broadband finite-pulse radio-frequency-driven recoupling (fp-RFDR) with (XY8)41 super-cycling for homo-nuclear correlations in very high magnetic fields at fast and ultra-fast MAS frequencies.
    Shen Ming, Hu Bingwen, Lafon Oliver, Trébosc Julien, Chen Qun, Amoureux Jean-Paul.
    Journal of Magnetic Resonance, vol. 223, pg. 107-119 (2012) DOI
     
  • 2011

  • The effect of P2O5 on the structure, sintering and sealing properties of barium calcium aluminum boro-silicate (BCABS) glasses.
    Ananthanarayanan A., Kothiyal G.P., Montagne L., Tricot G., Revel B.
    Materials Chemistry and Physics, vol. 130, pg. 880-889 (2011) DOI
     
  • Densified low-hygroscopic form of P2O5 glass.
    Brazhkin V. V., Akola J., Katayama Y., Kohara S., Kondrin M. V., Lyapin A. G., Lyapin S. G., Tricot G., Yagafarov O. F.
    Journal of Materials Chemistry, vol. 21, pg. 10442 (2011) DOI
     
  • Influence of the Active Particles on the Self-Healing Efficiency in Glassy Matrix.
    Coillot Daniel, Méar François O., Podor Renaud, Montagne Lionel.
    Advanced Engineering Materials, vol. 13, pg. 426-435 (2011) DOI
     
  • A tunable homonuclear dipolar decoupling scheme for high-resolution proton NMR of solids from slow to fast magic-angle spinning.
    Gan Zhehong, Madhu P.K., Amoureux Jean-Paul, Trébosc Julien, Lafon Olivier.
    Chemical Physics Letters, vol. 503, pg. 167-170 (2011) DOI
     
  • Broad-band homo-nuclear correlations assisted by 1H irradiation for bio-molecules in very high magnetic field at fast and ultra-fast MAS frequencies.
    Hu Bingwen, Lafon Oliver, Trébosc Julien, Chen Qun, Amoureux Jean-Paul.
    Journal of Magnetic Resonance, vol. 212, pg. 320-329 (2011) DOI
     
  • Structural study of PbO–MoO3–P2O5 glasses by Raman and NMR spectroscopy.
    Koudelka Ladislav, Rösslerová Ivana, Holubová Jana, Mošner Petr, Montagne Lionel, Revel Bertrand.
    Journal of Non-Crystalline Solids, vol. 357, pg. 2816-2821 (2011) DOI
     
  • Fast and High-Resolution Stereochemical Analysis by Nonuniform Sampling and Covariance Processing of Anisotropic Natural Abundance 2D 2H NMR Datasets.
    Lafon Olivier, Hu Bingwen, Amoureux Jean-Paul, Lesot Philippe.
    Chemistry - A European Journal, vol. 17, pg. 6716-6724 (2011) DOI
     
  • Beyond the Silica Surface by Direct Silicon-29 Dynamic Nuclear Polarization.
    Lafon Olivier, Rosay Melanie, Aussenac Fabien, Lu Xingyu, Trébosc Julien, Cristini Odile, Kinowski Christophe, Touati Nadia, Vezin Hervé, Amoureux Jean-Paul.
    Angewandte Chemie International Edition, vol. 50, pg. 8367-8370 (2011) DOI
     
  • Observing 13C–13C connectivities at high magnetic fields and very high spinning frequencies.
    Lafon Olivier, Trébosc Julien, Hu Bingwen, Paëpe Gaël De, Amoureux Jean-Paul.
    Chemical Communications, vol. 47, pg. 6930 (2011) DOI
     
  • Rotor-synchronized dipolar-filter sequence at fast MAS in solid-state NMR.
    Liu Qing-Hua, Ma Chao, Hu Bing-Wen, Chen Qun, Trebosc Julien, Lafon Olivier, Amoureux Jean-Paul.
    Journal of Magnetic Resonance, vol. 212, pg. 455-459 (2011) DOI
     
  • Structure and properties of glasses in ZnO–P2O5–TeO2 system.
    Mošner Petr, Vosejpková Kateřina, Koudelka Ladislav, Montagne Lionel, Revel Bertrand.
    Journal of Non-Crystalline Solids, vol. 357, pg. 2648-2652 (2011) DOI
     
  • NMR investigation of the crystallization mechanism of LaF3 and NaLaF4 phases in aluminosilicate glasses.
    Muñoz Francisco, de Pablos-Martín Araceli, Hémono Nicolas, Pascual María Jesús, Durán Alicia, Delevoye Laurent, Montagne Lionel.
    Journal of Non-Crystalline Solids, vol. 357, pg. 1463-1468 (2011) DOI
     
  • Revisiting the ‘mixed glass former effect’ in ultra-fast quenched borophosphate glasses by advanced 1D/2D solid state NMR.
    Raguenet B., Tricot G., Silly G., Ribes M., Pradel A.
    Journal of Materials Chemistry, vol. 21, pg. 17693 (2011) DOI
     
  • A Well-Defined Silica-Supported Lanthanum Bis(phosphinimino)methanide.
    Revel Bertrand, Delevoye Laurent, Tricot Grégory, Rastätter Marcus, Kuzdrowska Magdalena, Roesky Peter W., Gauvin Régis M.
    European Journal of Inorganic Chemistry, vol. 2011, pg. 1366-1369 (2011) DOI
     
  • Structural characterisation of phosphate materials: new insights into the spatial proximities between phosphorus and quadrupolar nuclei using the D-HMQC MAS NMR technique.
    Tricot G., Lafon O., Trébosc J., Delevoye L., Méar F., Montagne L., Amoureux J-P.
    Physical Chemistry Chemical Physics, vol. 13, pg. 16786 (2011) DOI
     
  • Thermal stability of a low Tg phosphate glass investigated by DSC, XRD and solid state NMR.
    Tricot Grégory, Revel Bertrand, Wegner Sebastian.
    Journal of Non-Crystalline Solids, vol. 357, pg. 2708-2712 (2011) DOI
     
  • Measurement of 13C–1H dipolar couplings in solids by using ultra-fast magic-angle spinning NMR spectroscopy with symmetry-based sequences.
    Wang Qiang, Lu Xingyu, Lafon Olivier, Trébosc Julien, Deng Feng, Hu Bingwen, Chen Qun, Amoureux Jean-Paul.
    Physical Chemistry Chemical Physics, vol. 13, pg. 5967 (2011) DOI
     
  • Efficiency at high spinning frequencies of heteronuclear decoupling methods designed to quench rotary resonance.
    Weingarth Markus, Trébosc Julien, Amoureux Jean-Paul, Bodenhausen Geoffrey, Tekely Piotr.
    Solid State Nuclear Magnetic Resonance, vol. 40, pg. 21-26 (2011) DOI
     
  • A Comparative Overview of Glass-Ceramic Characterization by MAS-NMR and XRD.
    Ananthanarayanan Arvind, Tricot Gregory, Kothiyal Govind Prasad, Montagne Lionel.
    Critical Reviews in Solid State and Materials Sciences, vol. 36, pg. 229-241 (2011) DOI
     
  • Boron isotopes as pH proxy: A new look at boron speciation in deep-sea corals using 11B MAS NMR and EELS.
    Rollion-Bard Claire, Blamart Dominique, Trebosc Julien, Tricot Grégory, Mussi Alexandre, Cuif Jean-Pierre.
    Geochimica et Cosmochimica Acta, vol. 75, pg. 1003-1012 (2011) DOI
     
  • Aluminum Incorporation in TiO2Rutile at High Pressure: An XRD and High-Resolution27Al NMR Study.
    Escudero Alberto, Delevoye Laurent, Langenhorst Falko.
    The Journal of Physical Chemistry C, vol. 115, pg. 12196-12201 (2011) DOI
     
  • Synthesis, Crystal and Electronic Structures, and Magnetic Properties of LiLn9Mo16O35 (Ln=La, Ce, Pr, and Nd) Compounds Containing the Original Cluster Mo16O36.
    Gougeon Patrick, Gall Philippe, Cuny Jérôme, Gautier Régis, Le Pollès Laurent, Delevoye Laurent, Trébosc Julien.
    Chemistry - A European Journal, vol. 17, pg. 13806-13813 (2011) DOI
     
  • Characterization of lead, barium and strontium leachability from foam glasses elaborated using waste cathode ray-tube glasses.
    Yot Pascal G., Méar François O.
    Journal of Hazardous Materials, vol. 185, pg. 236-241 (2011) DOI
     
  • Determination of coordination modes and estimation of the 31P–31P distances in heterogeneous catalyst by solid state double quantum filtered 31P NMR spectroscopy.
    Zhang Si-Yong, Wang Mei-Tao, Liu Qing-Hua, Hu Bing-Wen, Chen Qun, Li He-Xing, Amoureux Jean-Paul.
    Physical Chemistry Chemical Physics, vol. 13, pg. 5617 (2011) DOI
     
  • Modification of Molybdenum Structural Environment in Borosilicate Glasses with Increasing Content of Boron and Calcium Oxide by 95Mo MAS NMR.
    Magnin Magali, Schuller Sophie, Mercier Cyrille, Trébosc Julien, Caurant Daniel, Majérus Odile, Angéli Frédéric, Charpentier Thibault, Jantzen C.
    Journal of the American Ceramic Society, vol. 94, pg. 4274-4282 (2011) DOI
     
  • Local relaxation in lanthanum silicate oxyapatites by Raman scattering and MAS-NMR.
    Guillot Stéphanie, Beaudet-Savignat Sophie, Lambert Sébastien, Roussel Pascal, Tricot Gregory, Vannier Rose-Noelle, Rubbens Annick.
    Journal of Raman Spectroscopy, vol. 42, pg. 1455-1461 (2011) DOI
     
  • A well-defined silica-supported aluminium alkyl through an unprecedented, consecutive two-step protonolysis–alkyl transfer mechanism.
    Pelletier Jérémie, Espinas Jeff, Vu Nghiem, Norsic Sébastien, Baudouin Anne, Delevoye Laurent, Trébosc Julien, Le Roux Erwan, Santini Catherine, Basset Jean-Marie, Gauvin Régis M., Taoufik Mostafa.
    Chemical Communications, vol. 47, pg. 2979 (2011) DOI
     
  • Matériaux vitreux autocicatrisants pour application à haute température.
    Coillot D., Méar F.O., Podor R., Montagne L.
    Matériaux < Techniques, vol. 98, pg. 403-407 (2011) DOI
     
  • 2010

  • MAS-NMR studies of lithium aluminum silicate (LAS) glasses and glass–ceramics having different Li2O/Al2O3 ratio.
    Ananthanarayanan A., Kothiyal G.P., Montagne L., Revel B.
    Journal of Solid State Chemistry, vol. 183, pg. 120-127 (2010) DOI
     
  • MAS-NMR investigations of the crystallization behaviour of lithium aluminum silicate (LAS) glasses containing P2O5 and TiO2 nucleants.
    Ananthanarayanan A., Kothiyal G.P., Montagne L., Revel B.
    Journal of Solid State Chemistry, vol. 183, pg. 1416-1422 (2010) DOI
     
  • Characterization of self-healing glassy composites by high-temperature environmental scanning electron microscopy (HT-ESEM).
    Coillot D., Podor R., Mear F. O., Montagne L.
    Journal of Electron Microscopy, vol. 59, pg. 359-366 (2010) DOI
     
  • New insights into oxygen environments generated during phosphate glass alteration: a combined 17O MAS and MQMAS NMR and first principles calculations study.
    Forler Nina, Vasconcelos Filipe, Cristol Sylvain, Paul Jean-François, Montagne Lionel, Charpentier Thibault, Mauri Francesco, Delevoye Laurent.
    Physical Chemistry Chemical Physics, vol. 12, pg. 9053 (2010) DOI
     
  • Structure and properties of ZnO–B2O3–P2O5–TeO2 glasses.
    Mošner Petr, Vosejpková Kateřina, Koudelka Ladislav, Montagne Lionel, Revel Bertrand.
    Materials Chemistry and Physics, vol. 124, pg. 732-737 (2010) DOI
     
  • Distance measurement between a spin-1/2 and a half-integer quadrupolar nuclei by solid-state NMR using exact analytical expressions.
    Chen Lei, Lu Xingyu, Wang Qiang, Lafon Olivier, Trébosc Julien, Deng Feng, Amoureux Jean-Paul.
    Journal of Magnetic Resonance, vol. 206, pg. 269-273 (2010) DOI
     
  • Measurement of hetero-nuclear distances using a symmetry-based pulse sequence in solid-state NMR.
    Chen Lei, Wang Qiang, Hu Bingwen, Lafon Olivier, Trébosc Julien, Deng Feng, Amoureux Jean-Paul.
    Physical Chemistry Chemical Physics, vol. 12, pg. 9395 (2010) DOI
     
  • Indirect high-resolution detection for quadrupolar spin-3/2 nuclei in dipolar HMQC solid-state NMR experiments.
    Trébosc Julien, Lafon Olivier, Hu Bingwen, Amoureux Jean-Paul.
    Chemical Physics Letters, vol. 496, pg. 201-207 (2010) DOI
     
  • Homonuclear dipolar recoupling under ultra-fast magic-angle spinning: Probing 19F−19F proximities by solid-state NMR.
    Wang Qiang, Hu Bingwen, Lafon Olivier, Trébosc Julien, Deng Feng, Amoureux Jean-Paul.
    Journal of Magnetic Resonance, vol. 203, pg. 113-128 (2010) DOI
     
  • The structure of phosphate and borosilicate glasses and their structural evolution at high temperatures as studied with solid state NMR spectroscopy: Phase separation, crystallisation and dynamic species exchange.
    Wegner Sebastian, van Wüllen Leo, Tricot Gregory.
    Solid State Sciences, vol. 12, pg. 428-439 (2010) DOI
     
  • Design of a well-defined, silica-supported chiral Zn scaffold for enantioselective catalysis.
    Ternel Jérémy, Delevoye Laurent, Agbossou-Niedercorn Francine, Roisnel Thierry, Gauvin Régis M., Thomas Christophe M.
    Dalton Transactions, vol. 39, pg. 3802 (2010) DOI
     
  • Autonomic Self-Repairing Glassy Materials.
    Coillot Daniel, Méar François O., Podor Renaud, Montagne Lionel.
    Advanced Functional Materials, vol. 20, pg. 4371-4374 (2010) DOI
     
  • Glass-forming ability and structure of ZnO–MoO3–P2O5 glasses.
    .
    Journal of Non-Crystalline Solids, vol. 356, pg. 2509-2516 (2010) DOI
     
  • First-principles calculations of NMR parameters for phosphate materials.
    Vasconcelos Filipe, Cristol Sylvain, Paul Jean-François, Montagne Lionel, Mauri Francesco, Delevoye Laurent.
    Magnetic Resonance in Chemistry, vol. 48, pg. S142-S150 (2010) DOI
     
  • Characterization and Performance of Glass-Ceramic Sealants for SOECs.
    Khedim Hichem, Connelly Andrew J., Nonnet Hélène, Coillot Daniel, Mear François, Montagne Lionel.
    Advances in Science and Technology, vol. 64, pg. 76-82 (2010) DOI
     
  • Development of the first well-defined tungsten oxo alkyl derivatives supported on silica by SOMC: towards a model of WO3/SiO2 olefin metathesis catalyst.
    Mazoyer Etienne, Merle Nicolas, Mallmann Aimery de, Basset Jean-Marie, Berrier Elise, Delevoye Laurent, Paul Jean-François, Nicholas Christopher P., Gauvin Régis M., Taoufik Mostafa.
    Chemical Communications, vol. 46, pg. 8944 (2010) DOI
     
  • Polymerization of racemic β-butyrolactone using supported catalysts: a simple access to isotactic polymers.
    Ajellal Noureddine, Durieux Guillaume, Delevoye Laurent, Tricot Grégory, Dujardin Christophe, Thomas Christophe M., Gauvin Régis M.
    Chemical Communications, vol. 46, pg. 1032 (2010) DOI
     
  • Heteronuclear NMR Correlations To Probe the Local Structure of Catalytically Active Surface Aluminum Hydride Species on γ-Alumina.
    Mazoyer Etienne, Trébosc Julien, Baudouin Anne, Boyron Olivier, Pelletier Jérémie, Basset Jean-Marie, Vitorino Marta J., Nicholas Christopher P., Gauvin Régis M., Taoufik Mostafa, Delevoye Laurent.
    Angewandte Chemie International Edition, vol. 49, pg. 9854-9858 (2010) DOI
     
  • Anion-Vacancy-Induced Magneto−Crystalline Anisotropy in Fluorine-Doped Hexagonal Cobaltites.
    Mentré Olivier, Kabbour Houria, Ehora Ghislaine, Tricot Grégory, Daviero-Minaud Sylvie, Whangbo Myung-Hwan.
    Journal of the American Chemical Society, vol. 132, pg. 4865-4875 (2010) DOI
     
  • Insights into the Dealumination of Zeolite HY Revealed by Sensitivity-Enhanced 27Al DQ-MAS NMR Spectroscopy at High Field.
    Yu Zhiwu, Zheng Anmin, Wang Qiang, Chen Lei, Xu Jun, Amoureux Jean-Paul, Deng Feng.
    Angewandte Chemie International Edition, vol. 49, pg. 8657-8661 (2010) DOI
     
  • 2009

  • Structure and properties of MoO3-containing zinc borophosphate glasses.
    Jiří Šubčík, Koudelka Ladislav, Mošner Petr, Montagne Lionel, Revel Bertrand, Gregora Ivan.
    Journal of Non-Crystalline Solids, vol. 355, pg. 970-975 (2009) DOI
     
  • Composition and structure dependence of the properties of lithium borophosphate glasses showing boron anomaly.
    Muñoz Francisco, Montagne Lionel, Pascual Luis, Durán Alicia.
    Journal of Non-Crystalline Solids, vol. 355, pg. 2571-2577 (2009) DOI
     
  • Network Dynamics and Species Exchange Processes in Aluminophosphate Glasses: An in situ High Temperature Magic Angle Spinning NMR View.
    Wegner Sebastian, van Wüllen Leo, Tricot Gregory.
    The Journal of Physical Chemistry B, vol. 113, pg. 416-425 (2009) DOI
     
  • Double-quantum 19F–19F dipolar recoupling at ultra-fast magic angle spinning NMR: application to the assignment of 19F NMR spectra of inorganic fluorides.
    Wang Qiang, Hu Bingwen, Fayon Franck, Trébosc Julien, Legein Christophe, Lafon Olivier, Deng Feng, Amoureux Jean-Paul.
    Physical Chemistry Chemical Physics, vol. 11, pg. 10391 (2009) DOI
     
  • Double-quantum homonuclear NMR correlation spectroscopy of quadrupolar nuclei subjected to magic-angle spinning and high magnetic field.
    Wang Q., Hu B., Lafon O., Trébosc J., Deng F., Amoureux J.P.
    Journal of Magnetic Resonance, vol. 200, pg. 251-260 (2009) DOI
     
  • Double-quantum NMR spectroscopy of 31P species submitted to very large CSAs.
    Hu B., Delevoye L., Lafon O., Trébosc J., Amoureux J.P.
    Journal of Magnetic Resonance, vol. 200, pg. 178-188 (2009) DOI
     
  • Indirect Detection via Spin-1/2 Nuclei in Solid State NMR Spectroscopy: Application to the Observation of Proximities between Protons and Quadrupolar Nuclei.
    Lafon Olivier, Wang Qiang, Hu Bingwen, Vasconcelos Filipe, Trébosc Julien, Cristol Sylvain, Deng Feng, Amoureux Jean-Paul.
    The Journal of Physical Chemistry A, vol. 113, pg. 12864-12878 (2009) DOI
     
  • Proton-proton homonuclear dipolar decoupling in solid-state NMR using rotor-synchronized z-rotation pulse sequences.
    Lafon Olivier, Wang Qiang, Hu Bingwen, Trébosc Julien, Deng Feng, Amoureux Jean-Paul.
    The Journal of Chemical Physics, vol. 130, pg. 014504 (2009) DOI
     
  • Correlation NMR spectroscopy involving quadrupolar nuclei.
    Amoureux J.P., Trébosc J., Delevoye L., Lafon O., Hu B., Wang Q.
    Solid State Nuclear Magnetic Resonance, vol. 35, pg. 12-18 (2009) DOI
     
  • Robust and efficient spin-locked symmetry-based double-quantum homonuclear dipolar recoupling for probing 1H–1H proximity in the solid-state.
    Hu B., Wang Q., Lafon O., Trébosc J., Deng F., Amoureux J.P.
    Journal of Magnetic Resonance, vol. 198, pg. 41-48 (2009) DOI
     
  • Homonuclear dipolar decoupling schemes for fast MAS.
    Amoureux Jean-Paul, Hu Bingwen, Trébosc Julien, Wang Qiang, Lafon Olivier, Deng Feng.
    Solid State Nuclear Magnetic Resonance, vol. 35, pg. 19-24 (2009) DOI
     
  • Q-shear transformation for MQMAS and STMAS NMR spectra.
    Hung Ivan, Trébosc Julien, Hoatson Gina L., Vold Robert L., Amoureux Jean-Paul, Gan Zhehong.
    Journal of Magnetic Resonance, vol. 201, pg. 81-86 (2009) DOI
     
  • Enantiodiscrimination of Flexible Cyclic Solutes Using NMR Spectroscopy in Polypeptide Chiral Mesophases: Investigation ofcis-Decalin and THF.
    Aroulanda Christie, Lafon Olivier, Lesot Philippe.
    The Journal of Physical Chemistry B, vol. 113, pg. 10628-10640 (2009) DOI
     
  • 1H–1H double-quantum CRAMPS NMR at very-fast MAS (νR=35kHz): A resolution enhancement method to probe 1H–1H proximities in solids.
    Mafra Luís, Gomes José R.B., Trébosc Julien, Rocha João, Amoureux Jean-Paul.
    Journal of Magnetic Resonance, vol. 196, pg. 88-91 (2009) DOI
     
  • Evidence of crystalline/glassy intermediates in bismuth phosphates.
    Colmont Marie, Delevoye Laurent, Mentré Olivier.
    New Journal of Chemistry, vol. 33, pg. 19-22 (2009) DOI
     
  • Well-Defined Silica-Supported Calcium Reagents: Control of Schlenk Equilibrium by Grafting.
    Gauvin Régis M., Buch Frank, Delevoye Laurent, Harder Sjoerd.
    Chemistry - A European Journal, vol. 15, pg. 4382-4393 (2009) DOI
     
  • WO3-doped zinc borophosphate glasses .
    Montagne Lionel, Jiří Šubčík, Ladislav Koudelka, Petr Mošner, Ivan Gregora, Bertrand Revel.
    European Journal of Glass Science and Technology Part B, vol. 50, pg. 243-248 (2009)
     
  • 2008

  • Influence of phosphorus speciation on the phase separation of Na2O-B2O3-SiO2 glasses.
    Munoz F, Montagne L, Delevoye L.
    Physics and Chemistry of Glasses-European Journal of Glass Science and Technology Part B, vol. 49 (6), pg. 339-345 (2008)
     
  • 17O Solid-State NMR and First-Principles Calculations of Sodium Trimetaphosphate (Na3P3O9), Tripolyphosphate (Na5P3O10), and Pyrophosphate (Na4P2O7).
    Vasconcelos Filipe, Cristol Sylvain, Paul Jean-Francois, Tricot Grégory, Amoureux Jean-Paul, Montagne Lionel, Mauri Francesco, Delevoye Laurent.
    Inorganic Chemistry, vol. 47, pg. 7327-7337 (2008) DOI
     
  • New insights into the thermal evolution of aluminophosphate solutions: A complementary XRD and solid state NMR study.
    Tricot G., Coillot D., Creton E., Montagne L.
    Journal of the European Ceramic Society, vol. 28, pg. 1135-1141 (2008) DOI
     
  • Structure and properties of potassium niobato-borophosphate glasses.
    Koudelka Ladislav, Pospíšil Jaroslav, Mošner Petr, Montagne Lionel, Delevoye Laurent.
    Journal of Non-Crystalline Solids, vol. 354, pg. 129-133 (2008) DOI
     
  • Increased electrical conductivity of LiPON glasses produced by ammonolysis.
    MUNOZ F, DURAN A, PASCUAL L, MONTAGNE L, REVEL B, RODRIGUES A.
    Solid State Ionics, vol. 179, pg. 574-579 (2008) DOI
     
  • Solid-state NMR covariance of homonuclear correlation spectra.
    Hu Bingwen, Amoureux Jean-Paul, Trebosc Julien, Deschamps Michael, Tricot Gregory.
    The Journal of Chemical Physics, vol. 128, pg. 134502 (2008) DOI
     
  • Through-space MP-CPMAS experiments between spin-1/2 and half-integer quadrupolar nuclei in solid-state NMR.
    Hu B., Amoureux J.P., Trébosc J., Hafner S.
    Journal of Magnetic Resonance, vol. 192, pg. 8-16 (2008) DOI
     
  • Comparison of several hetero-nuclear dipolar recoupling NMR methods to be used in MAS HMQC/HSQC.
    Hu B., Trébosc J., Amoureux J.P.
    Journal of Magnetic Resonance, vol. 192, pg. 112-122 (2008) DOI
     
  • Enhanced resolution in proton solid-state NMR with very-fast MAS experiments.
    Amoureux Jean-Paul, Hu Bingwen, Trébosc Julien.
    Journal of Magnetic Resonance, vol. 193, pg. 305-307 (2008) DOI
     
  • 3D 1H–13C–14N correlation solid-state NMR spectrum.
    Siegel Renée, Trébosc Julien, Amoureux Jean-Paul, Gan Zhehong.
    Journal of Magnetic Resonance, vol. 193, pg. 321-325 (2008) DOI
     
  • Heteronuclear dipolar decoupling effects on multiple-quantum and satellite-transition magic-angle spinning NMR spectra.
    Ganapathy S., Delevoye L., Amoureux J. P., Madhu P. K.
    Magnetic Resonance in Chemistry, vol. 46, pg. 948-954 (2008) DOI
     
  • High-resolution 14N-edited 1H–13C correlation NMR experiment to study biological solids.
    Amoureux Jean-Paul, Trébosc Julien, Hu Bingwen, Halpern-Manners Nicholas, Antonijevic Sasa.
    Journal of Magnetic Resonance, vol. 194, pg. 317-320 (2008) DOI
     
  • Rapid analysis of isotopically unmodified amino acids by high-resolution 14N-edited 1H–13C correlation NMR spectroscopy.
    Amoureux Jean-Paul, Wang Qiang, Hu Bingwen, Lafon Olivier, Trébosc Julien, Deng Feng.
    Chemical Communications, pg. 6525 (2008) DOI
     
  • MAS-NMR study of lithium zinc silicate glasses and glass-ceramics with various ZnO content.
    Goswami Madhumita, Kothiyal Govind P., Montagne Lionel, Delevoye Laurent.
    Journal of Solid State Chemistry, vol. 181, pg. 269-275 (2008) DOI
     
  • Microstructural evolution of amorphous silica following alkali–silica reaction.
    Hamoudi A., Khouchaf L., Depecker C., Revel B., Montagne L., Cordier P.
    Journal of Non-Crystalline Solids, vol. 354, pg. 5074-5078 (2008) DOI
     
  • Structure and nonlinear optical properties of sodium–niobium phosphate glasses.
    Flambard A., Videau J.J., Delevoye L., Cardinal T., Labrugère C., Rivero C.A., Couzi M., Montagne L.
    Journal of Non-Crystalline Solids, vol. 354, pg. 3540-3547 (2008) DOI
     

 


Glasses and NMR Methodology

(Will become “NMR and Inorganic Materials” on Jan.1st 2015)

Head : Lionel Montagne (2006-2014), Laurent Delevoye (2015-2019)



 

 

 

 

 

 

 

Group members

Amoureux Jean-Paul, Professor

Delevoye Laurent, Researcher

Lafon Olivier, Professor

Mear François, Ass. Prof.

Montagne Lionel, Professor

Pourpoint Frédérique, Ass. Prof.

Trebosc Julien, Engineer Researcher

 

Key words:

New advanced solid-state NMR methods, especially applied to quadrupolar nuclei.  

DNP-NMR

DFT calculation of NMR parameters

Applications to inorganic and hybrid materials: glasses, catalysts, ceramics, nanomaterials, MOF…

Structure and applications of glasses

Phosphate chemistry

Applications fields:

- Energy (Self-healing sealing glasses for SOFC)

- Sustainable development (Special nuclear waste vitrification)

- Aeronautic (protective coatings for composite materials)

 

Research aims of the group : 

As indicated by our group’s name, we have two complementary field of research:

Our first interest is to understand the relationship between the atomic structure and the physical properties of non-crystalline materials (e.g. glasses). The approach is multidisciplinary, combining complementary skills in chemistry of glasses and solid-state NMR spectroscopy. As illustrated in the figure below, these two skills allow covering different aspects of glass science, including the formulation and synthesis of glasses, their advanced structural characterization, and their applications.

The activities of the group in the field of solid-state NMR involve the development of new sequences to increase both resolution and sensitivity of spectra. We develop methods in all fields that involve high magnetic fields (18.8T and 21T) and high spinning speed (up to 60 kHz) with a historical expertise for half integer quadrupolar nuclei. We focus especially on the design of novel correlation experiments in order to improve the structural characterization of glasses at atomic level. More recently, we have developed skills in the combination of DFT approach to NMR parameters as a complement to structural characterisation by experimental NMR, with a focus on systems featuring disorder, such as glasses and materials for catalytic applications.

A major current focus is on phosphate-containing glasses. These can be phosphate-network glasses as well as aluminosilicate, borosilicate and vanadate glasses mixed network with phosphate. We are developing these glasses for non-conventional applications in the domains of Nuclear fuels vitrification (for special wastes), self-healing sealing glasses for Solid-Oxides Fuel Cells, and antioxidation coatings for aeronautic components.

 

 

 

Students / Teaching:

We welcome students in the group in the frame of masters (1 and 2), Erasmus exchanges, PhD, post-docs. Our subjects deal with applied or academic research. Please consult the lab’s web page for subjects, or one of us for information.

We are involved in NMR teaching in the “Advanced Spectroscopy for Chemists” master http://www.master-asc.org/index.php and “Chemistry for Energy and Environment” master.

 

NMR facilities of the group :

Our group is strongly involved in the NMR scientific group of Nord-Pas de Calais region (GS-RMN) allowing projects for new cutting-edge equipments (800 and 900 MHz NMR spectrometers) to become reality. As a result, NMR site of Lille is now a fully-fledge partner in the french national CNRS Very Large Facility (Très Grande Infrastructure de Recherche  : TGIR ).

 

Recent scientific results:

 

We are among the pioneers of the characterization of mesoporous materials and nanomaterials by Nuclear Dynamics (DNP) Polarization. In particular, we demonstrated that the direct 29Si DNP is complementary to the indirect 29Si DNP via protons. Direct DNP allows the detection of the 29Si sites in the vicinity of the paramagnetic centers. In contrast, the indirect DNP permits the selective observation of the first layers below the surface (less than 0.5 nm from the surface). DNP has been used to probe the nearby 27Al-27Al on the surface of mesoporous alumina. We are currently seeking to optimize the DNP transfer, combining DNP with advanced NMR methods and to extend the field of application of this technique.

Fig 1: Direct DNP allows the detection of the 29Si sites in the vicinity of the paramagnetic centers. In contrast, the indirect DNP permits the selective observation of the first layers below the surface.

We have introduced new methods for observing nearby homo-and hetero-nuclei. These methods, which are applicable at high magnetic field and high MAS frequencies, have pushed the boundaries in terms of efficiency and robustness. We observed the internuclear proximities, even in the presence of strong interactions such as the quadrupole interaction, electronic shielding or dipolar couplings. We have shown that it is possible to measure distances between nuclei with close frequencies (13C-27Al). These techniques have been used to probe the structure of inorganic crystalline materials (fluoroaluminate, aluminophosphate polyoxometalates), glasses, supported organometallic complex catalysts.

We combine methodological developments in solid-state NMR for the structural characterization of real catalytic systems. In particular, we could identify surface features of a small quantity of aluminum hydride (Al-H), grafted on alumina, by conducting NMR correlation experiments using the scalar and dipolar coupling between Al and H. These new methods have provided strong understanding of the local structure of the active centers, and shown that these species were responsible for the exceptional reactivity of the catalyst.

Fig 3: 1H-27Al correlation spectrum enables to highlight the protonated aluminum sites.

 

Fig 4 : DFT calculation of NMR parameters enables to decompose the complex 17O spectrum of c-NaPO3.

We aim to better understand the relationships that bind the NMR parameters to the structure of crystalline and amorphous inorganic materials. In particular, we are interested in oxygen-17, combining experimental approaches by NMR and DFT calculations of NMR parameters to demonstrate that in phosphate glasses, the local structural information is encoded by the quadrupole interaction while the interaction of electronic screening provides information on the glass structure at long distance. With the help of molecular dynamics, we have proposed for the first time a structure of a glass model that accounts the distributions of NMR parameters.

In a recent article published in the Journal of the American Chemical Society, we have demonstrated, in collaboration with our colleagues from LC2P2 (M. Taoufik, CNRS Université de Lyon 1) and from LPCNO (L. Maron, CNRS-INSA, Toulouse), how 17-oxygène NMR can be a unique probe for the characterisation of the very surface of heterogeneous catalysts. Through direct homonuclear and heteronuclear correlations involving different pairs of nuclei (hydrogen and oxygen) and combining recently developed NMR experiments, it was possible not only to extract the proportions of the different species at the surface of silica carrier but especially to determine the relative positions of the various fragments. Theoretical calculations, carried out by our colleagues in Toulouse, strengthen interpretations, a necessary approach for such complex nucleus as oxygen-17. This should allow a better understanding of the structure of heterogeneous catalysts at the molecular level and thus guide the synthesis to obtain materials with improved performance.

Fig 5 : Different stages of 17-oxygen NMR characterization of the surface of a catalyst: by combining selective enrichment of the surface of the catalyst, 17-oxygen NMR studies at high magnetic field and DFT calculations, it is possible to reveal unexpected structural features.

 

Fig 6: 31P-51V correlation spectrum showing phosphate-vanadate connectivity in a glass.

 

The flagship of the 'Glass and NMR” group activity is the characterization by advanced NMR of glass materials (historically phosphate based). This work, based on the application of recent homo-and hetero-nuclear correlation NMR sequences, have identified for the first time the nature of the structural units present in the glasses with mixed network: borosilicate, aluminosilicate and vanado-phosphate. This new information has led to a better understanding of how the complex structure of these materials governs their macroscopic properties, like for instance the storage of special nuclear waste (iodine, sulfates).

Silver aluminophosphate glasses have been developed to immobilize up to 20 wt% of radioactive iodine without volatilization during the vitrification process. Structural studies show that iodine is inserted into the glass network without changing its connectivity or aggregate form.

 

Fig 7: The model for iodine incorporation into a phosphate glass network, as deduced from NMR analyses.

 

 

Fig 8 : Vanadium boride particles dispersed within the glass matrix enable to heal a crack at 800°C within less than 1 hour.

 
Our team is the first to have applied the concept of extrinsic healing (by adding healing particles) in glassy materials. Environmental SEM and nano-tomography showed a crack filled by in-situ formation of a new glass. The concept was validated in semi-industrial scale with a maturation project funded by Region NPdC and OSEO in collaboration with the CEA. We now extend the concept to thin layer glasses deposited by pulsed laser ablation.

Investigation of the anti-oxidation property of a phosphate coating for C/C composites and formulation of anti-oxidation coatings for SiC/SiC composites (Aeronautical applications, industrial contracts with SNECMA and MESSIER-BUGATTI companies).

 

Fig.9: Thermal evolution of aluminium phosphate solutions monitored by 31P NMR analyses. Oxidation tests performed on protected (left side) and unprotected (middle and right side)C/C materials, showing the efficiency of the anti-oxidation coating.

 

 

Industrial collaborations :

Messier (PhD): Anticatalytic protection of aircraft brakes

Snecma (PhD): Antioxidation coating for aeronautic application.

Snecma (post-doc): Enameling solution for aircraft reactor (ARCOCE project)

Arc international: glass formulation

Isover Saint-Gobain (PhD): Biosoluble glass fibers

Bruker: Development of advanced NMR methods.

CEA: new glass matrix for the immobilization of sulfate and iodide nuclear wastes.

DGA: Self-healing HT glass coatings

 

Scientific collaborations :

Glass science: G.P. Kothiyal, Bhabha Atomic Research Centre, Bombai, Inde, J.J. Videau, ICMCB., L. Koudelka, Dpt of chem. eng., University of Pardubice (Tchéquie). Léo van Wullen, Institut fur Physikalische Chemie, University of Muenster (Allemagne), Philippe Thomas, LPCTS, Limoge, Francisco Munoz, ICV Madrid.

NMR Methodology: M. Pruski et T. Kobayashi, Ames-Iowa, USA, Zhehong Gan, Tallahassee, USA, Stefan Steuernagel, Karlsruhe, Allemagne, Subramanian Ganapathy, Pune, Inde , F. Taulelle et C. Martineau, université Versailles, J. Frye, Fort-Collins, USA, Jun Ashida, Tokyo, Japon, Eriks Kupce, UK. P.K. Madhu, Mumbai, Inde; D. Massiot, F. Fayon et M. Deschamps, Orléans, France; P. Lesot, université Paris-Sud, France ; Th. Charpentier, CEA Saclay, France ; S. Vega, Rehovot, Israel ; J. Rocha et L. Mafra, Aveiro, Portugal ; S. Antonijevic, Berkeley, USA.; F. Deng, Wuhan, China ; Maria Alba, ICSM-CSIC, Sevilla ; Mostafa Taoufik, LC2P2, Lyon ; Laurent Maron, LPCNO, Toulouse ; F. Aussenac, Bruker BioSpin, Wissembourg, France ; M. Rosay, Bruker BioSpin, Billerica, USA ; Y. Nishiyama, JEOL Resonance, Tokyo, Japan ; B. Hu, East China Normal University, Shanghai, China ; T. Polenova, Univ. Delaware, Newark, USA ; K. Takegoshi, Univ. Kyoto, Japan; Marek J. Potrzebowski Polish Academy of Sciences, Lodz, Poland.  

 

Main equipments used by the group

-         solid-state NMR at the NMR center of the USTL (http://www.univ-lille1.fr/rmn): 100 WB (solids), 300 NB (liquids), 400 NB (liquids), two 400 WB (solids), 800 and 900 NB (mixed liquids-solids) http://www.rmn800.univ-lille1.fr/

-         Glass shop (glass elaboration up to 1600°C, thermal treatments under controlled atmospheres)

-         Thermal analyses (DSC, TGA-DTA, TMA)

-         Heating microscope (1400°C)

-         Parallel plates viscosimeter (up to 1000°C)

-         X-Ray diffraction (single-crystals, powders)

-         Electron microprobe, X-ray fluorescence

-         Surface analyses (XPS)

-         Isotopic enrichment facilities (17O)

 

Scientific animation :

International solid-state NMR workshop: Kyoto, Japon, Mai 2009 ; Wuhan, Chine, Novembre 2009 ; Puebla, Mexique, avril 2011 ; Pune, Inde, juillet 2011 ; Dalian, Chine, Mai 2013.

 

Organisation summer school in solid-state NMR : Sevilla, Spain, Sept. from 2008 to 2012

 

-                       Liquid and solid NMR trainings, held twice a year at the NMR centre of the USTL ((http://www.univ-lille1.fr/rmn)

 

 

 

PhD students and post-docs:

 

Creton E.

Thèse

Elaboration et caractérisation de protection anti-oxydation des composites SiC/SiC

CIFRE SNECMA

2006 2009

Vasconcelos F.

Thèse

Calculs DFT appliqués aux paramètres RMN de noyaux quadripolaires

A MRES

2006 2009

Coillot D.

Thèse

Composites autocicatrisants pour le scellement de SOFC

AM MRES

2007 2010

Forler N.

Thèse

Application of high-field 17O solid-state NMR to the study of phosphate glass hydration

A MRES

2008 2010

Hu B.

Thèse

Manipulation des interactions dipolaires en RMN à l'état solide.

COLLTERR NPdC

2006 2009

Wang Q.

Thèse

Observation par RMN des proximités homonucléaires entre noyaux de spin-1/2 ou quadripolaires

Affaires étrangères

2008 2010

Lu X.

Thèse

Méthodologie RMN pour les solides

Bruker Région NPdC

2010-2013

Lilly Thankamony A.S.

Thèse

Synergie RMN-RPE: développement de la DNP-RMN pour l’étude des matériaux

A MRES label président

2010 2013

Rajbhandari P.

Thèse

RMN haut-champ pour la caractérisation avancée de verres de phosphate dopés

BDI CNRS-Région

2010 2013

Castanie S.

Thèse

verres auto cicatrisants haute Température

DGA

2010 2013

Lemesle T.

Thèse

Etude et caractérisation structurale de verres pour le confinement de l'iode

CEA

2010 2013

Gatoux A.

Thèse

Protection Anti-Oxydation à haute température pour matériaux composites C/C

Contrat Messier Bugatti

2010 2013

Girard G.

Thèse

Structural Characterization of disorder by solid-state NMR and DFT calculations

Ministère Lille 1 Région

2012-2015

Shen M.

Thèse

Corrélation homonucléaire à haute vitesse et haut champ magnétique dans les matériaux innovants 

CSC-Chine

2012-2015

Li X.

Thèse

Distances et proximités entre spin-1/2-noyaux quadripolaires dans les matériaux hybrides et inorganiques

CSC-Chine

2012-2015

Duong N. T.

Thèse

Caractérisation des matériaux poreux nanostructurés par DNP-RMN

BDI CNRS-CEA

2012-2015

Perez S.

Post-doc

Mise au point d’un traitement cosmétique pour composites aéronautiques

SNECMA - ARCOCE

2009-2010

Pavon-Gonzales E.

Post-doc

 

Lille1

2011-2012

Pourpoint F.

ATER

Mesure de distances 13C-27Al dans les solides

ENSCL

Sept2011- aout 2012

Grekov D

Thèse

Caractérisation par RMN avancée de systèmes catalytiques 

ANR

Sept. 2013-Août 2016