Pierre Florian

Conditions Extrêmes et Matériaux Haute Température et Irradiation

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Dominique Massiot

Conditions Extrêmes et Matériaux Haute Température et Irradiation

100

Franck Fayon

Centre National de la Recherche Scientifique

Valérie Montouillout

Conditions Extrêmes et Matériaux Haute Température et Irradiation

Daniel R. Neuville

Université Paris Cité

Mathieu Allix

Conditions Extrêmes et Matériaux Haute Température et Irradiation

Philip J. Grandinetti

The Ohio State University

Emmanuel Véron

Conditions Extrêmes et Matériaux Haute Température et Irradiation

Ana Isabel Becerro

Instituto de Ciencia de Materiales de Sevilla

Catherine Bessada

Conditions Extrêmes et Matériaux Haute Température et Irradiation

Cécile Genevois

Conditions Extrêmes et Matériaux Haute Température et Irradiation

Cooperative Institutions

Centre National de la Recherche Scientifique

340

Conditions Extrêmes et Matériaux Haute Température et Irradiation

Université d'Orléans

Sorbonne Université

Université Claude Bernard Lyon 1

ETH Zurich

Université Paris Cité

Institut de Chimie

Université de Bordeaux

Laboratoire de Chimie

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NMR of materials up to the nanometer scale

HAL (Le Centre pour la Communication Scientifique Directe) (2012)

Dominique Massiot Sylvian Cadars Michaël Deschamps Franck Fayon Valérie Montouillout

Nanometre

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13C, 25Mg, and 43Ca Solid-State NMR for the Purpose of Dolomitic Marbles Provenance Elucidation

Materials (2023)

Isabelle Pianet Anna Gutiérrez García-Moreno Marie-Claire Savin Nicolas Frèrebeau Julien Trébosc

The study of the provenance of dolomitic marble artefacts has become relevant since it was discovered that quarries of this marble other than that of Cape-Vathy located on the island of Thasos have been exploited since Antiquity. To improve our knowledge about the provenance of materials and the extent of their dispersion, multiple archaeometric studies were performed in the past including isotope analyses, petrography, cathodoluminescence, and elemental analyses. In the present work, solid-state nuclear magnetic resonance (NMR) spectroscopy has been added to this panel of techniques. NMR allows the characterization of the material at a molecular level by looking at different nuclei: carbon, magnesium, and calcium. Statistical analysis of the data collected on both quarry samples and archaeologic items was also implemented and clearly demonstrates the efficiency of a holistic approach for provenance elucidation. Finally, the first 25Mg NMR tests have shown the potential of this technique to discriminate between dolomitic marbles of different provenance. The results are discussed in terms of their historical meaning and illustrate the exploitation of sources of dolomitic marbles other than the Greek Thasos source.

Characterization

10.3390/ma16041468

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Structural Description of the Na₂B₄O₇−Na₃AlF₆−TiO₂ System. 2. A Multinuclear NMR Approach of Melts and Solids

The Journal of Physical Chemistry B (2007)

Pierre Florian Elena Maria Anghel Catherine Bessada

A quantitative structural investigation of pseudo-binary Na2B4O7−[Na3AlF6−TiO2]11 was carried out by NMR spectroscopy. We applied high-resolution solid-state NMR on quenched samples and in situ high-temperature NMR spectroscopy on molten compositions to obtain a more accurate description of the melts. Consistent with our previous findings, two compositional ranges can be evidenced. Below 50 mol % Na2B4O7, the TiIV → TiVI valence conversion prevails, leading to the formation of B(O,F)3 species at the expense of B(O,F)4 ones and a low average coordination number of aluminum; above 50 mol %, the system behaves mainly like the binary Na2B4O7−Na3AlF6 where Na3AlF6 is playing a network former role. The dominant oxyfluoro-species evidenced by double-resonance NMR in the quenched samples are BO2F2, BO3F, BO2F, BOF2, NaO7F, NaO6F2, and AlO4F with sodium in various coordination states, Na(O,F)8, Na(O,F)7, and Na(O,F)6. F−Ti bonds were found to be almost negligible whereas F−Al2, F−B, F−Na, and F−Al−Na bonds were clearly observed in the solid state.

10.1021/jp065201p

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Citations (10)

Structural and scintillation properties of new Ce3+-doped alumino-borate

Optical Materials (2001)

O. Aloui-Lebbou Christelle Goutaudier S. Kubota Christophe Dujardin M.Th. Cohen-Adad

10.1016/s0925-3467(00)00062-8

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High-Field ¹⁷O MAS NMR Investigation of Phosphonic Acid Monolayers on Titania

Chemistry of Materials (2008)

Florence Brodard-Séverac Gilles Guerrero Jocelyne Maquet Pierre Florian Christel Gervais

High-field 17O MAS NMR was used to investigate the binding of self-assembled monolayers of 17O-enriched phosphonic acids deposited on a titania anatase support. The spectra were recorded at two different magnetic fields (9.4 and 17.6 T), to improve the reliability of the simulations of the different resonances. The spectra recorded at 17.6 T offer an excellent resolution between the different oxygen sites, P═O, P−O−H, and P−O−Ti, thus greatly facilitating their quantification. The data reported here give direct evidence of the extensive formation of Ti−O−P bonds in the surface modification of titania by phosphonic acids. The presence of residual P═O and P−O−H sites indicates the presence of several different binding modes in phosphonic acid monolayers. The chemical shift of P−O−Ti sites is consistent with bridging (as opposed to chelating) modes.

Chemical shift

10.1021/cm8012683

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Visibility of Al Surface Sites of γ-Alumina: A Combined Computational and Experimental Point of View

The Journal of Physical Chemistry C (2014)

Raphaël Wischert Pierre Florian Christophe Copéret Dominique Massiot Philippe Sautet

The nature of γ-alumina (γ-Al2O3) surface sites leaves many open questions today, and solid-state NMR spectroscopy has been proposed and used as a tool for assessing their structure. Here, we calculated 27Al NMR parameters from first principles in periodic boundary conditions for a large number of Al sites with different coordination, potentially present on the alumina surface. The nature and accordingly the NMR parameters of these sites change with the level of hydroxylation and thereby the pretreatment temperature of γ-Al2O3. While the Al chemical shift is little affected by hydroxylation, the magnitude of the quadrupolar interaction at the Al nucleus is strongly correlated to hydroxylation, with high to very high quadrupolar coupling constant (CQ) values (20–34 MHz) on the weakly hydrated major (110) termination, which contains highly reactive Lewis acidic “defect sites”, and gradual lowering to bulklike CQ values of around 5 MHz on highly hydrated surfaces. In addition, we studied the effects of local symmetry on the EFG tensor of Al atoms and the effects of hydrating neighboring Al sites. These calculation were combined with {1H}27Al cross-polarization NMR experiments, carried out at high magnetic field (20 T) and high magic angle spinning (MAS) frequency (30 kHz) on γ-Al2O3 pretreated at different temperatures. We clearly show that this method is mainly sensitive to strongly hydrated surface sites besides the much more abundant bulk Al atoms, and that catalytically important high-CQ Al centers (Lewis acid sites) and even some types of hydroxylated Al sites are not visible in the spectrum. Therefore, even current high-field NMR experiments are not (yet) able to provide a complete picture of the structure of γ-Al2O3 and much caution should be exercised when interpreting 27Al NMR spectra.

Magic angle spinning

Hydroxylation

10.1021/jp503277m

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Citations (105)

Resolved-detrimental langasite-type surface crystallization in yttrium lanthanum gallium-rich heavy metal oxide glasses for infra-red optical fiber applications

Florian Calzavara Pierre Florian Vincent Sarou‐Kanian Franck Fayon Christine Labrugère‐Sarroste

Lanthanum

Gallium Oxide

Lanthanum oxide

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Apport de la RMN haute température in-situ sur la structure et la dynamique des aluminates et alumino-silicates liquides

HAL (Le Centre pour la Communication Scientifique Directe) (2010)

Pierre Florian Daniel R. Neuville Najim Sadiki Valérie Montouillout Dominique Massiot

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Verres et vitrocéramiques oxyazotés : Propriétés mécaniques et luminescentes

HAL (Le Centre pour la Communication Scientifique Directe) (2021)

Alexis Duval Alain Moréac Bernard Hehlen Farah Inoubli Pierre Florian

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Structure et propriété des verres et des liquides : le rôle de l’aluminium

Matériaux & Techniques (2010)

Daniel R. Neuville Pierre Florian Charles Le Losq Dominique Massiot

Le verre est un matériau naturel ou fabriqué de la main de l’homme qui présente une structure désordonnée à l’échelle atomique. Parmi les principaux éléments des verres d’oxyde on trouve les éléments Si, Al, Ca et Na. Si et Al vont former un réseau tridimensionnel de tétraèdres SiO4 et/ou AlO4– qui seront connectés entre eux, ou bien entourés de Na ou de Ca jouant différents rôles en fonction du rapport M/Al (avec M = Na/2 ou Ca). Cependant l’aluminium peut jouer un rôle plus complexe en étant aussi en coordinence 5.

10.1051/mattech/2011014

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Citations (4)