Author: "Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)" - Searchworks@Jio Institute Digital Library Search Results

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Start Over Author "Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)"

108 results on '"Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)"'

1. Effect of isothermal annealing and continuous heating on the crystallization and the mechanical properties of a Fe based metallic glass

Author: Avettand-Fènoël, Marie-Noëlle, Sauvage, François-Xavier, Marinova, Maya, Addad, Ahmed, Taillard, Roland, Unité Matériaux et Transformations - UMR 8207 (UMET), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Laboratoire Avancé de Spectroscopie pour les Intéractions la Réactivité et l'Environnement - UMR 8516 (LASIRE), Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), and Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)
Subjects: [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], [CHIM.MATE]Chemical Sciences/Material chemistry
Abstract: International audience
Published: 2023

2. Nonequilibrium spherulitic magnetite in the Ryugu samples

Author: Elena Dobrică, Hope A. Ishii, John P. Bradley, Kenta Ohtaki, Adrian J. Brearley, Takaaki Noguchi, Toru Matsumoto, Akira Miyake, Yohei Igami, Mitsutaka Haruta, Hikaru Saito, Satoshi Hata, Yusuke Seto, Masaaki Miyahara, Naotaka Tomioka, Hugues Leroux, Corentin Le Guillou, Damien Jacob, Francisco de la Peña, Sylvain Laforet, Maya Marinova, Falko Langenhorst, Dennis Harries, Pierre Beck, Thi H.V. Phan, Rolando Rebois, Neyda M. Abreu, Jennifer Gray, Thomas Zega, Pierre-M. Zanetta, Michelle S. Thompson, Rhonda Stroud, Kate Burgess, Brittany A. Cymes, John C. Bridges, Leon Hicks, Martin R. Lee, Luke Daly, Phil A. Bland, Michael E. Zolensky, David R. Frank, James Martinez, Akira Tsuchiyama, Masahiro Yasutake, Junya Matsuno, Shota Okumura, Itaru Mitsukawa, Kentaro Uesugi, Masayuki Uesugi, Akihisa Takeuchi, Mingqi Sun, Satomi Enju, Aki Takigawa, Tatsuhiro Michikami, Tomoki Nakamura, Megumi Matsumoto, Yusuke Nakauchi, Hisayoshi Yurimoto, Ryuji Okazaki, Hikaru Yabuta, Hiroshi Naraoka, Kanako Sakamoto, Shogo Tachibana, Toru Yada, Masahiro Nishimura, Aiko Nakato, Akiko Miyazaki, Kasumi Yogata, Masanao Abe, Tatsuaki Okada, Tomohiro Usui, Makoto Yoshikawa, Takanao Saiki, Satoshi Tanaka, Fuyuto Terui, Satoru Nakazawa, Sei-ichiro Watanabe, Yuichi Tsuda, The University of New Mexico [Albuquerque], Kyoto University, Unité Matériaux et Transformations - UMR 8207 (UMET), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut Michel Eugène Chevreul - FR 2638 (IMEC), and Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)
Subjects: Magnetite, [SDU.ASTR]Sciences of the Universe [physics]/Astrophysics [astro-ph], Geochemistry and Petrology, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], [SDU.STU]Sciences of the Universe [physics]/Earth Sciences, Ryugu, Return samples, [PHYS.PHYS.PHYS-GEO-PH]Physics [physics]/Physics [physics]/Geophysics [physics.geo-ph], Nonequilibrium, Aqueous alteration, [CHIM.MATE]Chemical Sciences/Material chemistry, [PHYS.ASTR]Physics [physics]/Astrophysics [astro-ph]
Abstract: International audience; We have investigated several particles collected during each of two touchdowns of the Hayabusa2 spacecraft at the surface of the C-type asteroid 162173 Ryugu using various electron microscope techniques. Our detailed transmission electron microscopy study shows the presence of magnetite with various morphologies coexisting in close proximity. This is characteristic of CI chondrite-like materials and consistent with the mineral assemblages and compositions in the Ryugu parent body. We describe the microstructural characteristics of magnetite with different morphologies, which could have resulted from the chemical conditions (growth vs. diffusion rate) during their formation. Furthermore, we describe the presence of magnetites with a spherulitic structure composed of individual radiating fibers that are characterized by pervasive, homogeneously distributed euhedral to subhedral pores that have not been described in previous chondrite studies. This particular spherulitic structure is consistent with crystallization under nonequilibrium conditions. Additionally, the presence of a high density of defects within the magnetite fibers, the high surface/volume ratio of this morphology, and the presence of amorphous materials in several pores and at the edges of the acicular fibers further support their formation under nonequilibrium conditions. We suggest that the growth processes that lead to this structure result from the solution reaching a supersaturated state, resulting in an adjustment to a lower free energy condition via nucleation and rapid growth.
Published: 2023

3. Assessment of structures in phosphocaseinate dispersions by A4F, NMR and SAXS: The impact of demineralization and heat treatment on viscosity

Author: Márcio H. Nogueira, Luisa A. Scudeler, Lucile Humblot, Bertrand Doumert, Marie Hennetier, Frédéric Violleau, Celine Lesur, Guillaume Delaplace, Paulo.P.S. Peixoto, Unité Matériaux et Transformations - UMR 8207 (UMET), Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), Chimie Agro-Industrielle (CAI), Ecole nationale supérieure des ingénieurs en arts chimiques et technologiques (ENSIACET), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), INGREDIA SA, F-62000 Arras, France, Partenaires INRAE, This study started with the phD Thesis of Marcio Nogueira (These Cifre financed by ANRT) within the frame of the project 'Proteinolab', a partnership between the Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE) and Ingredia Dairy Experts . Hence, this work has allowed some funds from French National Research Agency (ANR) allocated to the project 'Proteinolab' but also from the ANR-financed 'ProteinoPeps' project, which enable us to strenghten scientific discussion and to consolidate the results through acceding to other experimental facilitie, and ANR-17-LCV2-0005,Proteinolab,Laboratoire commun de caractérisation des structures-fonctions d'isolats protéiques différenciés(2017)
Subjects: Dense dispersions, Viscosity, General Chemical Engineering, [SDV]Life Sciences [q-bio], Ultra-high-temperature, General Chemistry, Demineralization, Casein micelles, Food Science
Abstract: International audience; The present work aims to better understand the relation between heat treatment (Ultra High Temperature - UHT), partial demineralization of casein micelles (CMs) dispersions and their corresponded rheological properties. A multiscale analysis (SAXS, solid state NMR and Asymmetrical Flow Field Flow Fractionation (A4F)), has been used. Different samples with different levels of calcium/phosphorous demineralization (up to −30% of calcium content) have been studied before and after UHT treatment. The present data show that CM dispersions, displaying a mild demineralization, display an important decrease in viscosity after UHT. NMR shows that, during UHT, mild demineralized samples display stronger calcium/phosphorus intake than both, the non-demineralized and the strong demineralized ones. SAXS and A4F show that UHT-dependent calcium intake, in mild demineralization dispersions, seems to be responsible for a transformation of large casein aggregates into small and denser ones. This decrease of the large aggregates is probably the main reason of the UHT-dependent decrease in viscosity. These data show that a sample with a rather small amount of demineralization can have a quite important susceptibility to UHT in terms of viscosity.
Published: 2023

4. Photocatalytic Partial Oxidation of Methane to Carbon Monoxide and Hydrogen over CIGS Solar Cell

Author: Chunyang Dong, Di Hu, Karima Ben Tayeb, Pardis Simon, Ahmed Addad, Martine Trentesaux, Danilo Oliveira de Souza, Sergei Chernyak, Deizi V. Peron, Amelle Rebai, Jean-Francois Guillemoles, Xavier Wallart, Bruno Grandidier, Andrei Y. Khodakov, Negar Naghavi, Vitaly V. Ordomsky, Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Elettra Sincrotrone Trieste, Institut Photovoltaïque d’Ile-de-France (UMR) (IPVF), École polytechnique (X)-Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-TOTAL FINA ELF-EDF (EDF)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Photovoltaïque d’Ile-de-France (ITE) (IPVF)-Air Liquide [Siège Social], Institut Photovoltaïque d’Ile-de-France (ITE) (IPVF), Institut d’Électronique, de Microélectronique et de Nanotechnologie - UMR 8520 (IEMN), Centrale Lille-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Université Polytechnique Hauts-de-France (UPHF)-JUNIA (JUNIA), Université catholique de Lille (UCL)-Université catholique de Lille (UCL), EPItaxie et PHYsique des hétérostructures - IEMN (EPIPHY - IEMN), Université catholique de Lille (UCL)-Université catholique de Lille (UCL)-Centrale Lille-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Université Polytechnique Hauts-de-France (UPHF)-JUNIA (JUNIA), Physique - IEMN (PHYSIQUE - IEMN), Eco-Efficient Products & Processes Laboratory (E2P2L), RHODIA-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), The authors gratefully acknowledge the support of the French National Research Agency (SolarMethaCell project). We are grateful to the Elettra and Soleil synchrotrons for the use of beamtime., Renatech Network, and ANR-22-CE05-0019,SolarMethaCell,Conversion du méthane en molécules de plate-forme dans des conditions ambiantes à l'aide de cellules solaires(2022)
Subjects: [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Process Chemistry and Technology, Photocatalysis, Oxidation, CIGS, [CHIM.CATA]Chemical Sciences/Catalysis, [CHIM.MATE]Chemical Sciences/Material chemistry, [CHIM.INOR]Chemical Sciences/Inorganic chemistry, Syngas, Methane, Catalysis, General Environmental Science
Abstract: International audience; Methane valorization is one of the main challenges in the modern chemical industry. However, existing processes require high reaction temperatures. The alternative photocatalytic routes for methane valorization at ambient conditions would be highly attractive. Today, photovoltaic (PV) generation of electricity is one of the main sources of renewable energy. PV absorbers could be excellent candidates for photochemical applications. Herein, we report selective methane photocatalytic oxidation at ambient conditions into CO and H2 by conventional Cu(In,Ga)Se2 (CIGS) absorbers used in solar cells. A thin film of CIGS coated over Mo exhibits exceptional performance in methane partial oxidation to CO and H2 with a stable CO productivity of 2.4 mmol per g of CIGS and a selectivity to CO of over 80 %. The reaction proceeds via the facile dissociation of methane into disordered carbon and hydrogen over CIGS surface with subsequent regeneration of the surface by partial oxidation of carbon into CO.
Published: 2023

5. 13C, 25Mg, and 43Ca Solid-State NMR for the Purpose of Dolomitic Marbles Provenance Elucidation

Author: Isabelle Pianet, Anna Gutiérrez Garcia-Moreno, Marie-Claire Savin, Nicolas Frerebeau, Julien Trebosc, Pierre Florian, M. Pilar Lapuente Mercadal, Archéosciences Bordeaux, Université de Bordeaux (UB)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS), INSTITUT CATALÀ D'ARQUEOLOGIA CLÀSSICA (ICAC), Universitat Rovira i Virgili, Universitat Autònoma de Barcelona (UAB), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Conditions Extrêmes et Matériaux : Haute Température et Irradiation (CEMHTI), Université d'Orléans (UO)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Departamento de Ciencias de la Tierra, University of Zaragoza - Universidad de Zaragoza [Zaragoza], and ANR-10-LABX-0052,LaScArBx,Using the world in ancient societies : processes and forms of appropriation of space in Long Time(2010)
Subjects: Elemental analysis, [SHS.ARCHEO]Humanities and Social Sciences/Archaeology and Prehistory, principal component analysis, Principal component analysis, provenance, [CHIM.MATE]Chemical Sciences/Material chemistry, Dolomite, Stable isotope, NMR, Marble, dolomite, Provenance studies, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Provenance, General Materials Science
Abstract: Altres ajuts: This research was funded by LaScArBx program funded by the Agence Nationale de la Recherche (ANR-10-LABX-52, ROMAE2, 2019 Edition), the Cross-border Spanish-French Cooperation between the Autonomous Community of Aragon and the Région Nouvelle Aquitaine (2019 Edition, Marmol project, 2019), the French Centre National de la Recherche Scientifique (de Marmoribus, SMI-INSHS 2020), the region Nouvelle Aquitaine (Aquitania, Ornata, 2021-2024). Quarries, workshops, craftmen, and customers of artistic productions in stone from Hispania Tarraconensis" and IR INFRANALYTICS FR2054 for conducting NMR experiments. 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 25 Mg 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.
Published: 2023

6. Advances in the characterization of inorganic solids using NMR correlation experiments

Author: Andrew G.M. Rankin, Frédérique Pourpoint, Nghia Tuan Duong, Laurent Delevoye, Jean-Paul Amoureux, Olivier Lafon, Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie Radicalaire (ICR), and Aix Marseille Université (AMU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)
Subjects: [PHYS]Physics [physics], homonuclear, microporous materials, through-space, solid-state NMR correlation homonuclear heteronuclear through-bond through-space INADEQUATE HETCOR HMQC INEPT microporous materials catalysts minerals biomaterials, minerals, INADEQUATE, INEPT, catalysts, heteronuclear, through-bond, HMQC, correlation, solid-state NMR, [CHIM]Chemical Sciences, HETCOR, biomaterials
Abstract: International audience; As a local characterization technique endowed with atomic resolution, solid-state NMR spectroscopy provides unique insights on the atomic-level structure and dynamics of inorganic and hybrid materials. In particular, two-dimensional through-bond and through-space correlation experiments allow the observation of covalent bonds and proximities between identical or distinct isotopes, thus providing detailed information on the arrangement of atoms in the materials. Compared to biological and organic samples, inorganic and hybrid materials contain additional NMR-active nuclei, and notably quadrupolar isotopes with nuclear spin I ≥ 1, such as 11 B, 27 Al and 71 Ga, which are often subject to large quadrupolar interaction. Therefore, specific NMR correlation experiments have been developed to probe the local environment of these quadrupolar isotopes. We provide here an in-depth overview of correlation experiments, which have been employed for the characterization of inorganic and hybrid materials. We present first the through-space and through-bond correlation experiments to probe connectivities and proximities between identical nuclei, and then their counterparts for distinct isotopes. In both cases, we describe the experiments employed for spin-1/2 and quadrupolar isotopes. We indicate the state-of-the-art technique and the isotopes, for which they have been applied. Finally we present how these correlation NMR experiments have provided essential information on the atomic-level structure of different classes of inorganic hybrid materials, including (i) microporous materials (aluminophosphates, zeolites, metal-organic frameworks (MOFs)), (ii) metal oxide catalysts, such as amorphous silica alumina as well as supported metal complexes on alumina or silica, (iii) minerals and biomaterials and (iv) glasses.
Published: 2023

7. Extrusion-Spheronization of UiO-66 and UiO-66_NH2 into Robust-Shaped Solids and Their Use for Gaseous Molecular Iodine, Xenon, and Krypton Adsorption

Author: Alla Abramova, Nelly Couzon, Maëva Leloire, Philippe Nerisson, Laurent Cantrel, Sébastien Royer, Thierry Loiseau, Christophe Volkringer, Jérémy Dhainaut, Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Service d'Etude et de Recherche EXpérimentale (IRSN/PSN-RES/SEREX), Institut de Radioprotection et de Sûreté Nucléaire (IRSN), Laboratoire d'Expérimentation Environnement et Chimie (IRSN/PSN-RES/SEREX/L2EC), Institut de Radioprotection et de Sûreté Nucléaire (IRSN)-Institut de Radioprotection et de Sûreté Nucléaire (IRSN), ANR-19-ASTR-0015,TEXMOF,Textiles fonctionnalisés par des solides poreux de type MOF pour la capture et/ou la dégradation d'agents toxiques(2019), Université de Lille, CNRS, Centrale Lille, ENSCL, Univ. Artois, Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS], Unité de Catalyse et de Chimie du Solide (UCCS) - UMR 8181, Institut de Radioprotection et de Sûreté Nucléaire [IRSN], and Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181
Subjects: extrusion-spheronization, metal−organic frameworks, shaping, iodine capture, Xe/Kr separation, General Materials Science, [CHIM.CATA]Chemical Sciences/Catalysis, [CHIM.INOR]Chemical Sciences/Inorganic chemistry
Abstract: International audience; The use of an extrusion-spheronization process was investigated to prepare robust and highly porous extrudates and granules starting from UiO-66 and UiO-66_NH2 metal–organic framework powders. As-produced materials were applied to the capture of gaseous iodine and the adsorption of xenon and krypton. In this study, biosourced chitosan and hydroxyethyl cellulose (HEC) are used as binders, added in low amounts (less than 5 wt % of the dried solids), as well as a colloidal silica as a co-binder when required. Characterizations of the final shaped materials reveal that most physicochemical properties are retained, except the textural properties, which are impacted by the process and the proportion of binders (BET surface area reduction from 5 to 33%). On the other hand, the mechanical resistance of the shaped materials toward compression is greatly improved by the presence of binders and their respective contents, from 0.5 N for binderless UiO-66 granules to 17 N for UiO-66@HEC granules. UiO-66_NH2-based granules demonstrated consequent iodine capture after 48 h, up to 527 mg/g, in line with the pristine UiO-66_NH2 powder (565 mg/g) and proportionally to the retaining BET surface area (−5% after shaping). Analogously, the shaped materials presented xenon and krypton sorption isotherms correlated to their BET surface area and high predicted xenon/krypton selectivity, from 7.1 to 9.0. Therefore, binder-aided extrusion-spheronization is an adapted method to produce shaped solids with adequate mechanical resistance and retained functional properties.
Published: 2022

8. 1H, 13C and 15N chemical shift backbone resonance NMR assignment of tobacco calmodulin 2

Author: Emmanuelle Boll, Francois-Xavier Cantrelle, Olivier Lamotte, Sébastien Aimé, David Wendehenne, Xavier Trivelli, Biologie Structurale Intégrative (ERL 9002 - BSI ), Institut Pasteur de Lille, Réseau International des Instituts Pasteur (RIIP)-Réseau International des Instituts Pasteur (RIIP)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Facteurs de Risque et Déterminants Moléculaires des Maladies liées au Vieillissement - U 1167 (RID-AGE), Réseau International des Instituts Pasteur (RIIP)-Réseau International des Instituts Pasteur (RIIP)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Université de Lille-Centre Hospitalier Régional Universitaire [Lille] (CHRU Lille), Agroécologie [Dijon], Université de Bourgogne (UB)-Université Bourgogne Franche-Comté [COMUE] (UBFC)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Institut Agro Dijon, Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), The authors thank the Chevreul Institute (FR 2638) for its help in the development of this work. Chevreul Institute is supported by the « Ministère de l’Enseignement Supérieur et de la Recherche et de l’Innovation», the « CNRS » the « Région Hauts-de-France », the « Métropole Européenne de Lille » and the « Fonds Européen de Développement des Régions ». The Investissements d’Avenir program, project ISITE-BFC (contract ANR-15-IDEX-0003, grant NOISELESS - RA18041.AEC.IS) is alsoacknowledge for its support, ANR-15-IDEX-0003,BFC,ISITE ' BFC(2015), Université de Bourgogne (UB)-AgroSup Dijon - Institut National Supérieur des Sciences Agronomiques, de l'Alimentation et de l'Environnement-Université Bourgogne Franche-Comté [COMUE] (UBFC)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), and MILLOT, Dominique
Subjects: [SDV] Life Sciences [q-bio], calmodulin, calcium, CaM, Structural Biology, [SDV]Life Sciences [q-bio], NMR resonance assignment, tobacco, Biochemistry
Abstract: International audience; Calcium is a ubiquitous second messenger regulating numbers of cellular processes in living organisms. It encodes and transmits information perceived by cells to downstream sensors, including calmodulin (CaM), that initiate cellular responses. In plants, CaM has been involved in the regulation of plant responses to biotic and abiotic environmental cues. Plant CaMs possess a cysteine residue in their first calcium-binding motif EF-hand, which is not conserved in other eucaryotic organisms. In this work, we report the near-complete backbone chemical shift assignment of tobacco CaM2 with calcium. These results will be useful to study the impact of this particular EF-hand domain regarding CaM interaction with partners involved in stress responses.
Published: 2022

9. Chemical exchange of labile protons by deuterium enables selective detection of pharmaceuticals in solid formulations

Author: Claire Welton, Parth Raval, Julien Trébosc, G. N. Manjunatha Reddy, Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), and European Project: 795091,H2020,H2020-MSCA-IF-2017,ZEOCATALYST(2019)
Subjects: Dopamine, Metals and Alloys, [CHIM.THER]Chemical Sciences/Medicinal Chemistry, General Chemistry, [SDV.SP]Life Sciences [q-bio]/Pharmaceutical sciences, Deuterium, Catalysis, Surfaces, Coatings and Films, Electronic, Optical and Magnetic Materials, Pharmaceutical Preparations, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Materials Chemistry, Ceramics and Composites, Amino Acids, Protons
Abstract: International audience; Chemically assisted swapping of labile protons by deuterons is presented for amino acids, polysaccharides, pharmaceutical compounds, and their solid formulations. Solid-state packing interactions in these compounds are elucidated by 1H–2H isotope correlation NMR spectroscopy (iCOSY). A minuscule concentration of dopamine, 5 wt% or ∼100 μg, in a solid formulation can be detected by 2H NMR at 28.2 T (1H, 1200 MHz) in under a minute.
Published: 2022

10. Enhancing ammonia catalytic production over spatially confined cobalt molybdenum nitride nanoparticles in SBA-15

Author: Amanda Sfeir, Camila A. Teles, Carmen Ciotonea, G.N. Manjunatha Reddy, Maya Marinova, Jérémy Dhainaut, Axel Löfberg, Jean-Philippe Dacquin, Sébastien Royer, Said Laassiri, Université de Lille, CNRS, Centrale Lille, ENSCL, Univ. Artois, Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181, 3209|||Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS], Unité de Chimie Environnementale et Interactions sur le Vivant [UCEIV], Institut Chevreul - FR2638, Université Mohammed VI Polytechnique [Ben Guerir] [UM6P], Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Unité de Chimie Environnementale et Interactions sur le Vivant (UCEIV), Université du Littoral Côte d'Opale (ULCO), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), and Université Mohammed VI Polytechnique [Ben Guerir] (UM6P)
Subjects: History, nitrides, SBA-15, Polymers and Plastics, Ammonia synthesis, Process Chemistry and Technology, confined nanoparticles, [CHIM.CATA]Chemical Sciences/Catalysis, Business and International Management, Catalysis, Industrial and Manufacturing Engineering, General Environmental Science
Abstract: International audience; Ternary Co3Mo3N nitrides are reported to exhibit high catalytic activity in ammonia synthesis. However, synthesis of ternary nitrides requires thermal treatments at elevated temperatures and reactive atmospheres that lead to unavoidable surface reduction (~ 10 m2 g-1). In this work, we have developed a novel approach to improve the catalytic activity of Co3Mo3N through its dispersion into a high surface area silica-based support (SBA-15). During ammonolysis and ammonia synthesis conditions reaction, SBA-15 demonstrated good thermal and chemical stability maintaining an ordered porous structure and high surface area (> 500 m2 g-1). For application in ammonia synthesis, SBA-15 supported cobalt molybdenum catalysts with different metal loading (10, 20 and 30 wt.%) were prepared by a modified impregnation-infiltration protocol and their catalytic activity studied. The dispersion of CoMo nitride nanoparticles into SBA-15 structures resulted in the improvement of their structural and textural properties of nitrides as evidenced by XRD analysis, STEM-EDS, and N2- physisorption (e.g. 10-CoMo-N/SBA-15: 348 m2 g-1). Nevertheless, the surface composition of CoMo-N/SBA-15 catalysts was found to be similar to the non-supported Co3Mo3N. Furthermore, supported CoMo-N/SBA-15 displayed enhanced catalytic activity in ammonia synthesis (1714, 1429 and 810 μmol gactive phase-1 h-1 corresponding to the CoMo oxide loadings of 10, 20, 30 wt.% respectively) that outperform the classical Co3Mo3N catalyst (298 μmol gcatalyst-1 h-1). The results reported in this work highlights a novel approach for the design of nitride-based catalysts with superior catalytic properties in ammonia synthesis.; Les nitrures ternaires de Co3Mo3N présentent une activité catalytique élevée dans la synthèse d'ammoniac. Cependant, la synthèse de nitrures ternaires nécessite des traitements thermiques à des températures élevées et des atmosphères réactives qui conduisent à une réduction de surface inévitable (~ 10 m2 g-1). Dans ce travail, nous avons développé une nouvelle approche pour améliorer l'activité catalytique du Co3Mo3N grâce à sa dispersion dans un support à base de silice à surface élevée (SBA-15). Au cours de la réaction dans les conditions d'ammonolyse et de synthèse d'ammoniac, le SBA-15 a démontré une bonne stabilité thermique et chimique en maintenant une structure poreuse ordonnée et une surface spécifique élevée (> 500 m2 g-1). Pour une application dans la synthèse d'ammoniac, des catalyseurs au cobalt-molybdène sur support SBA-15 avec différentes charges métalliques (10, 20 et 30 % en poids) ont été préparés par un protocole d'imprégnation-infiltration modifié et leur activité catalytique étudiée. La dispersion des nanoparticules de nitrure de CoMo dans les structures SBA-15 a entraîné l'amélioration de leurs propriétés structurelles et texturales des nitrures, comme en témoignent l'analyse XRD, le STEM-EDS et la physisorption N2 (par exemple 10-CoMo-N/SBA-15 : 348 m2 g-1). Néanmoins, la composition de surface des catalyseurs CoMo-N/SBA-15 s'est avérée similaire à celle du Co3Mo3N non supporté. De plus, le CoMo-N/SBA-15 supporté a affiché une activité catalytique améliorée dans la synthèse d'ammoniac (1714, 1429 et 810 μmol gactive phase-1 h-1 correspondant aux charges d'oxyde CoMo de 10, 20, 30 % en poids respectivement) qui surpassent le catalyseur classique Co3Mo3N (298 μmol gcatalyst-1 h-1). Les résultats rapportés dans ce travail mettent en évidence une nouvelle approche pour la conception de catalyseurs à base de nitrure avec des propriétés catalytiques supérieures dans la synthèse d'ammoniac.
Published: 2022

11. Mechanochemical synthesis and study of the local structure of NaGaS2 glass and glass-ceramics

Author: Louisiane Verger, Julien Trébosc, Benoît Baptiste, Eric Furet, Killian Dénoue, Jiajie Zhang, François Cheviré, David Le Coq, Laurent Calvez, Olivier Lafon, Olivier Hernandez, Institut des Sciences Chimiques de Rennes (ISCR), Université de Rennes (UR)-Institut National des Sciences Appliquées - Rennes (INSA Rennes), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Ecole Nationale Supérieure de Chimie de Rennes (ENSCR)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut de minéralogie, de physique des matériaux et de cosmochimie (IMPMC), Muséum national d'Histoire naturelle (MNHN)-Institut de recherche pour le développement [IRD] : UR206-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS), Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut des Matériaux Jean Rouxel (IMN), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Nantes université - UFR des Sciences et des Techniques (Nantes univ - UFR ST), Nantes Université - pôle Sciences et technologie, Nantes Université (Nantes Univ)-Nantes Université (Nantes Univ)-Nantes Université - pôle Sciences et technologie, Nantes Université (Nantes Univ)-Nantes Université (Nantes Univ)-Nantes Université - Ecole Polytechnique de l'Université de Nantes (Nantes Univ - EPUN), Nantes Université (Nantes Univ)-Nantes Université (Nantes Univ), This publication is (partially) supported by the European Union through the European Regional Development Fund (ERDF), the Ministry of Higher Education and Research, the French Region of Brittany and Rennes Métropole. Financial support from the IR INFRANALYTICS FR2054 for conducting the research is gratefully acknowledged. O.L. and J.L. are grateful for funding provided by the Region Hauts-de-France (France), Europe (FEDER), CNRS, Ministère de l’Enseignement Supérieur et de la Recherche, CPER and Chevreul Institute (FR 2638)., Université de Lille, CNRS, Centrale Lille, ENSCL, Univ. Artois, Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181, and UCCS Équipe RMN et matériaux inorganiques
Subjects: Inorganic Chemistry, Amorphous materials, Granular materials, Annealing (metallurgy), [CHIM]Chemical Sciences, Nuclear magnetic resonance spectroscopy, Diffraction, [CHIM.MATE]Chemical Sciences/Material chemistry, Physical and Theoretical Chemistry
Abstract: International audience; NaGaS2 is a newly discovered compound that has already shown great promise for a variety of applications because of its layered structure and ion exchange properties. In this work, crystalline NaGaS2 has been synthesized by an alternative method to what has been previously published, namely, by mechanochemistry, either by a direct one-step process or by a two-step process. In the one-step process, crystalline NaGaS2 is directly formed by milling sodium sulfide Na2S and gallium(III) sulfide Ga2S3. However, an amorphous material is present in majority together with the crystalline phase. In the two-step process, amorphous NaGaS2 is first obtained by mechanical milling and then heated above its glass transition temperature to obtain a glass–ceramic mainly composed of crystalline NaGaS2. For the two-step process, changes of the local atomic-level structure in amorphous NaGaS2 and after crystallization were analyzed by high-field solid-state nuclear magnetic resonance (NMR) spectroscopy as well as by X-ray total scattering and pair distribution function (PDF) analysis. Based on quantitative analysis on the 23Na NMR spectra, modifying the annealing treatment can promote the formation of the crystalline phase up to a molar fraction of 83.8%.
Published: 2022

12. Multiscale characterization of a Fe based metallic glass: from its crystallization mechanism to its mechanical properties

Author: Avettand-Fènoël, Marie-Noëlle, Sauvage, Xavier, Marinova, Maya, Addad, Ahmed, Taillard, Roland, Unité Matériaux et Transformations - UMR 8207 (UMET), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), and Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)
Subjects: [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], [CHIM.MATE]Chemical Sciences/Material chemistry
Abstract: International audience
Published: 2022

13. Evolution of Ni-Fe nanoparticles upon oxidation-reduction and catalytic reaction: an advanced characterization study

Author: Marceau, Eric, Shi, D., Sadier, Achraf, Wojcieszak, Robert, Paul, Sébastien, Girardon, Jean-Sébastien, Mamede, Anne-Sophie, Marinova, Maya, Stievano, L., Sougrati, M. T., La Fontaine, C., Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), and Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)
Subjects: [CHIM]Chemical Sciences
Abstract: International audience
Published: 2022

14. Zinc effect during aluminum-copper and aluminum-brass dissimilar friction stir welding

Author: Avettand-Fènoël, Marie-Noëlle, Nagaoka, Toru, Marinova, Maya, Taillard, Roland, Unité Matériaux et Transformations - UMR 8207 (UMET), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), and Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)
Subjects: [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], [CHIM.MATE]Chemical Sciences/Material chemistry
Abstract: International audience
Published: 2022

15. Experimental characterization of the chemical composition and structure of molecular soot precursors and soot particles in a laminar diffusion flame by coupling ToF-SIMS and Raman spectroscopy

Author: Elias, Jessy, Faccinetto, Alessandro, Irimiea, Cornelia, Nuns, Nicolas, Pirim, Claire, Focsa, Cristian, Mercier, Xavier, Physicochimie des Processus de Combustion et de l’Atmosphère - UMR 8522 (PC2A), Université de Lille-Centre National de la Recherche Scientifique (CNRS), DMPE, ONERA, Université Paris Saclay [Palaiseau], ONERA-Université Paris-Saclay, Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), and Laboratoire de Physique des Lasers, Atomes et Molécules - UMR 8523 (PhLAM)
Subjects: [CHIM]Chemical Sciences
Abstract: International audience; The transformation process in sooting flames leading to the formation of nanoparticles in the condensed phase from molecular precursors in the gas phase (soot nucleation) is not yet fully understood [1]. Information on the physical chemical properties of the nascent particles is difficult to accessexperimentally but also essential for the validation of the hypotheses on soot nucleation currently being examined by the scientific community. In this work, we characterize the molecular precursors and the soot particles formed in a laminar diffusion methane flame by combining several in situ and ex situ diagnostics (fluorescence, incandescence, secondary ion mass spectrometry and Raman spectroscopy) with the goal of inferring the chemical composition and the structure of the nascent particles. The presented work highlights that several of the investigated physical chemical properties suddenly change within a narrow flame region that acquires the character of a discontinuity point correlated to the soot nucleation process. Notably, the obtained data shows evidences of the transition from flat to curved molecular structures, and the progressive apparition of finite size, sandwiched graphene like layers. Furthermore, the fraction of atomic hydrogen features a local maximum immediately upstream the detection of nascent soot particles consistent with the increasing in flame rate of C-C covalent bonds formation postulated by the major hypotheses explaining the nucleation of soot particles.References[1] J.W. Martin, M. Salamanca, M. Kraft, Soot inception: Carbonaceous nanoparticle formation in flames, Progress in Energy and Combustion Science. 88 (2022) 100956.https://doi.org/10.1016/j.pecs.2021.100956.
Published: 2022

16. Alternative strategy to grow large surface hBN on Ge films by molecular beam epitaxy

Author: Batista Pessoa, Walter, Franck, Max, Dabrowski, Jaroslaw, Wallart, X., Nuns, Nicolas, Lukosius, Mindaugas, Vignaud, Dominique, Institut d’Électronique, de Microélectronique et de Nanotechnologie - UMR 8520 (IEMN), Centrale Lille-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Université Polytechnique Hauts-de-France (UPHF)-JUNIA (JUNIA), Université catholique de Lille (UCL)-Université catholique de Lille (UCL), EPItaxie et PHYsique des hétérostructures - IEMN (EPIPHY - IEMN), Université catholique de Lille (UCL)-Université catholique de Lille (UCL)-Centrale Lille-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Université Polytechnique Hauts-de-France (UPHF)-JUNIA (JUNIA), IHP - Leibniz-Institut für innovative Mikroelektronik, Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), and Renatech Network
Subjects: [SPI]Engineering Sciences [physics]
Abstract: International audience; Hexagonal Boron Nitride is a two-dimensional insulator with a wide bandgap (~6 eV), chemically and thermally stable. Its 2D nature makes it exceptionally interesting as an ultrathin barrier, tunneling or passivation layer for integrated electronics and photonics, noticeably for the encapsulation of graphene or other 2D materials for next generation electronics [1]. In the case of germanium, Ge oxides are unstable and might induce thermal pits, limiting its applications [2]. Hence, hBN could be a good candidate not only for Ge passivation but also for ultra-capacitors (e.g., metal/hBN/Ge) and for graphene devices onGe (e.g. graphene/hBN heterostructures )[1,3]. In this work, we study the growth of large surface atomically thin hBN on Ge (001) films bymolecular beam epitaxy using boron effusion cell and a remote nitrogen plasma cell. Firstly, we discuss how the B/N precursor ratio influences the BN composition from B-rich to stoichiometric films (figure 1). Then, we consider the challenges related to the limitation of growth temperature due to Ge thermal pits formation. A BN buffer layer strategy was developed which significantly allows to increase the growth temperature without thermal pits formation, so that better quality BN can be grown.
Published: 2022

17. Relations entre la structure et les propriétés de composites piézoélectriques de BTO/P(VDF-co-TrFE)

Author: Girardot, Melanie, Addad, Ahmed, Tahon, Jean-Francois, Fadel, Alexandre, Marin, Adeline, Bouad, Vincent, Lyskawa, Joel, Barrau, Sophie, Unité Matériaux et Transformations - UMR 8207 (UMET), Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut Michel Eugène Chevreul - FR 2638 (IMEC), and Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)
Subjects: [CHIM.MATE]Chemical Sciences/Material chemistry
Abstract: National audience
Published: 2022

18. Lactide-Lactone Chain Shuttling Copolymerization Mediated by Aluminum-based complexes : access to new multiblock copolymers

Author: Meimoun, Julie, Stoclet, Grégory, Roussel, Pascal, Bria, Marc, Huret, Audrey, Bonnet, Fanny, Zinck, Philippe, Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Unité Matériaux et Transformations - UMR 8207 (UMET), Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), université de Bordeaux, Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), and ANR-21-CE06-0024,PLANAVETTE,Copolymérisation statistique par navette d'esters cycliques, une voie d'accès à de nouveaux copolymères multiblocs à base de PLA(2021)
Subjects: [CHIM.POLY]Chemical Sciences/Polymers, [CHIM.MATE]Chemical Sciences/Material chemistry, ComputingMilieux_MISCELLANEOUS
Abstract: International audience
Published: 2022

19. Unprecedented Lactide-Lactone Chain Shuttling Copolymerization Mediated by Aluminum-based complexes

Author: Meimoun, Julie, Huret, Audrey, Bria, Marc, Roussel, Pascal, Stoclet, Grégory, Bonnet, Fanny, Zinck, Philippe, Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Unité Matériaux et Transformations - UMR 8207 (UMET), and Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)
Subjects: [CHIM.POLY]Chemical Sciences/Polymers, [CHIM.MATE]Chemical Sciences/Material chemistry, ComputingMilieux_MISCELLANEOUS
Abstract: National audience
Published: 2022

20. Upon the effect of Zn during friction stir welding of aluminum-copper and aluminum-brass systems

Author: Maya Marinova, Roland Taillard, Toru Nagaoka, Marie-NoËlle Avettand-Fènoël, Unité Matériaux et Transformations - UMR 8207 (UMET), Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Osaka Research Institute of Industrial Science and Technology, Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), and Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL)
Subjects: brass, 0209 industrial biotechnology, Materials science, Friction stir welding, Strategy and Management, Flatness (systems theory), Mechanical properties, 02 engineering and technology, Welding, Management Science and Operations Research, Industrial and Manufacturing Engineering, law.invention, Brass, 020901 industrial engineering & automation, law, copper and zinc interlayer, Phase transformations, Composite material, Microstructure, Material flow, Filler metal, [CHIM.MATE]Chemical Sciences/Material chemistry, Interface, 021001 nanoscience & nanotechnology, Shear (sheet metal), Lap joint, visual_art, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], visual_art.visual_art_medium, 0210 nano-technology, Aluminum
Abstract: International audience; The present study deals with the effect of Zn on the linear friction stir lap welding of Al to Cu or to brass with a pinless tool. Zn was considered either as a filler metal or as an element in solid solution in α-brass. The lap joint configuration with a groove machined at the top of the bottom plate was chosen in order to test for the first time the influence of liquid Zn at the interface in case of melting by avoiding its ejection. Besides, the use of a pin free tool to join three millimeters thick plates is challenging. The paper presents and discusses the macrostructure and microstructure of the various joints together with their mechanical properties. A strong emphasis is given to the lubricating action of a liquid phase on the material flow as well as on the mechanisms of phase transformations at the various interfaces. The present work reports an early investigation of the material flow in linear friction stir lap welding with a pinless tool. The lap shear tensile fracture behavior of the welds is related to their interface morphology and microstructure. In particular, the fairly good shear resistance of the brass-Zn-Al joint arises from the composite nature of its interface despite its flatness and high thickness.
Published: 2020

21. The Impact of Diethyl Furan-2,5-dicarboxylate as an Aromatic Biobased Monomer toward Lipase-Catalyzed Synthesis of Semiaromatic Copolyesters

Author: Kifah Nasr, Audrey Favrelle-Huret, Rosica Mincheva, Gregory Stoclet, Marc Bria, Jean-Marie Raquez, Philippe Zinck, Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Université de Mons (UMons), Centre d'Innovation et de Recherche en Matériaux Polymères (CIRMAP), Unité Matériaux et Transformations - UMR 8207 (UMET), Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), and European Project: ALPO
Subjects: aromatic copolyesters, Polymers and Plastics, Process Chemistry and Technology, furan, Organic Chemistry, lipase, enzymatic polymerization, [CHIM.CATA]Chemical Sciences/Catalysis, time course profile, polycondensation
Abstract: International audience; Furan-2,5-dicarboxylic acid has been introduced in recent years as a green aromatic monomer toward the design of aromatic (co)polyesters with enhanced properties, i.e., polyethylene furanoate (PEF) that can definitely compete with its petroleum-based counterpart, i.e., polyethylene terephthalate (PET). In an attempt to produce biobased semiaromatic copolyesters in an efficient eco-friendly approach, we report herein the polycondensation of diethyl furan-2,5-dicarboxylate (DEFDC) with different aliphatic diols and diesters of variable chain length catalyzed by an immobilized lipase from Candida antarctica using a two-step polymerization reaction carried out in diphenyl ether. The influence of diol and diester chain length, the molar concentration of DEFDC, and the effect of enzyme loading were assessed via nuclear magnetic resonance (NMR), gel permeation chromatography (GPC), differential scanning calorimetry (DSC), and wide-angle X-ray scattering (WAXS). With high quantities of DEFDC, significant differences in terms of M̅n buildup were noticed. Only longer diols starting from octane-1,8-diol successfully reacted with up to 90% DEFDC as opposed to only 25% DEFDC reacting with short diols such as butane-1,4-diol. While varying the chain length of the diester, it was evident that shorter diols such as hexane-1,6-diol have better reactivity toward longer diesters, while dodecane-1,12-diol was reactive toward all tested diesters. The incorporation of long chain fatty dimer diols such as Pripol 2033 led to polyesters with higher M̅n and was successfully used to overcome the limitations of poor reactivity observed in the case of short diols in the presence of high furan content. The DSC results showed a pseudoeutectic behavior as a function of increasing the mol % of DEFDC, and a change in the crystalline phase was confirmed via WAXS analysis. Finally, this work showed the successful enzyme-catalyzed synthesis of several DEFDC biobased semiaromatic copolyesters with variable interesting properties that can be further optimized for possible applications in food packaging as well as other possibilities.; L'acide furane-2,5-dicarboxylique a été introduit ces dernières années en tant que monomère aromatique vert pour la conception de (co)polyesters aromatiques aux propriétés améliorées, comme le polyéthylène furanoate (PEF) qui peut définitivement concurrencer son homologue issu du pétrole, le polyéthylène téréphtalate (PET). Dans le but de produire des copolyesters semi-aromatiques d'origine biologique par une approche efficace et respectueuse de l'environnement, nous rapportons ici la polycondensation du furan-2,5-dicarboxylate de diéthyle (DEFDC) avec différents diols et diesters aliphatiques de longueur de chaîne variable, catalysée par une lipase immobilisée de Candida antarctica, en utilisant une réaction de polymérisation en deux étapes réalisée dans de l'éther diphénylique. L'influence de la longueur de chaîne des diols et des diesters, la concentration molaire de DEFDC, ainsi que l'effet de la charge enzymatique ont été évalués par Résonance Magnétique Nucléaire (RMN), chromatographie par perméation de gel (CPG), calorimétrie différentielle à balayage (DSC) et diffusion des rayons X à angle large (WAXS). Sans DEFDC, ou à faible teneur, l'augmentation de la longueur du diol n'a pas eu d'effet négatif sur la masse moléculaire moyenne en nombre (Mn) des copolyesters aliphatiques préparés. En revanche, lorsque des quantités élevées de DEFDC (plus de 40 % molaire) ont été ajoutées dans le milieu réactionnel, des différences significatives en termes d'accumulation de Mn ont été remarquées. Seuls les diols plus longs à partir de l'octane-1,8-diol ont été mis en réaction avec succès avec jusqu'à 90% de DEFDC, par opposition à seulement 25% de DEFDC avec des diols courts tels que le butane-1,4-diol. Le Mn obtenu a montré une tendance à diminuer en fonction de l'augmentation du % d'alimentation en DEFDC, surtout avec les diols courts où la diminution du Mn était plus prononcée. En faisant varier la longueur de la chaîne du diester, il était évident que les diols plus courts tels que l'hexane-1,6-diol ont une meilleure réactivité vis-à-vis des diesters plus longs, tandis que le dodécane-1,12-diol était réactif vis-à-vis de tous les diesters testés. L'incorporation de diols dimères gras à longue chaîne tels que le Pripol 2033 dans le milieu réactionnel a conduit à des polyesters avec un Mn plus élevé et a été utilisé avec succès pour surmonter les limitations de la faible réactivité observée dans le cas des diols courts en présence d'une teneur élevée en furanes. Les résultats de la calorimétrie différentielle à balayage (DSC) ont montré un comportement pseudo-eutectique caractérisé par une diminution du point de fusion (Tm) en fonction de l'augmentation du % molaire de DEFDC, suivie d'une augmentation à un % molaire plus élevé deࣙࣙ DEFDC (≥ 50%) et un changement de la phase cristalline confirmé par une analyse de diffusion des rayons X à grand angle (WAXS). Enfin, ce travail a montré la synthèse réussie par catalyse enzymatique de plusieurs copolyesters semi-aromatiques biosourcés avec des propriétés intéressantes variables, à base de DEFDC.
Published: 2022

22. Cyclodextrins Initiated Ring-Opening Polymerization of Lactide Using 4-Dimethylaminopyridine (DMAP) as Catalyst: Study of DMAP/β-CD Inclusion Complex and Access to New Structures

Author: Julie Meimoun, Yupin Phuphuak, Remi Miyamachi, Yong Miao, Marc Bria, Cyril Rousseau, Guilherme Nogueira, Andreia Valente, Audrey Favrelle-Huret, Philippe Zinck, Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Department of Chemistry [Faculty of Science, Naresuan University], Naresuan University, Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), UCCS Équipe Catalyse Supramoléculaire, Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Centro de Química Estrutural, Faculdade de Ciências da Universidade de Lisboa, Faculdade de Ciencias da Universidade de Lisboa, Université de Lille, CNRS, Centrale Lille, ENSCL, Univ. Artois, and Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS]
Subjects: [CHIM.ORGA]Chemical Sciences/Organic chemistry, ring-opening polymerization, rac-lactide, Pharmaceutical Science, Organic chemistry, [CHIM.CATA]Chemical Sciences/Catalysis, Analytical Chemistry, QD241-441, cyclodextrin, DMAP, Chemistry (miscellaneous), polylactide, Drug Discovery, organocatalysis, inclusion complex, polylactide carbohydrate conjugate, Molecular Medicine, [CHIM]Chemical Sciences, Physical and Theoretical Chemistry
Abstract: Les cyclodextrines (CD) sont des oligosaccharides cycliques utilisées dans de nombreux domaines. Le greffage de polymères sur les CD permet d'obtenir de nouvelles structures et applications. Le polylactide (PLA) est un polyester aliphatique biosourcé et biocompatible qui peut être greffé sur des CD par polymérisation par ouverture de cycle initiée par -OH. En utilisant la 4-diméthylaminopyridine (DMAP) comme organocatalyseur, une fonctionnalisation quantitative est atteinte sur les α-, β-, γ- et 2,3-diméthyl- β-cyclodextrines natives. Des distributions étroites de poids moléculaire sont obtenues avec les CD natifs (dispersité < 1.1). La combinaison DMAP/β-CD est utilisée comme étude de cas, et la formation d'un complexe d'inclusion (1/1) est montrée pour la première fois dans la littérature, qui est entièrement caractérisé par RMN. L'inclusion du DMAP dans la cavité se produit via le bord secondaire du β-CD et la constante d'association (Ka) est estimée à 88,2 M-1. Son utilisation comme initiateur de polymérisation par ouverture de cycle conduit à une efficacité de fonctionnalisation partielle, et donc à un conjugué β-CD-PLA plus hydrophile que celui obtenu à partir de β-CD natif. Les résultats de la polymérisation incluant également l'utilisation du complexe d'inclusion adamantane/β-CD comme initiateur suggèrent que l'inclusion du catalyseur DMAP dans le CD ne peut pas se produire pendant les réactions de polymérisation. Le rac-lactide ne forme pas de complexe d'inclusion avec le β-CD. Cyclodextrins (CDs) are cyclic oligosaccharides used in many fields. Grafting polymers onto CDs enables new structures and applications to be obtained. Polylactide (PLA) is a biobased, biocompatible aliphatic polyester that can be grafted onto CDs by -OH-initiated ring-opening polymerization. Using 4-dimethylaminopyridine (DMAP) as an organocatalyst, a quantitative functionalization is reached on native α-, β-, γ- and 2,3-dimethyl- β-cyclodextrins. Narrow molecular weight distributions are obtained with the native CDs (dispersity < 1.1). The DMAP/β-CD combination is used as a case study, and the formation of an inclusion complex (1/1) is shown for the first time in the literature, which is fully characterized by NMR. The inclusion of DMAP into the cavity occurs via the secondary rim of the β-CD and the association constant (Ka) is estimated to be 88.2 M−1. Its use as an initiator for ring-opening polymerization leads to a partial functionalization efficiency, and thus a more hydrophilic β-CD-PLA conjugate than that obtained starting from native β-CD. Polymerization results including also the use of the adamantane/β-CD inclusion complex as an initiator suggest that inclusion of the DMAP catalyst into the CD may not occur during polymerization reactions. Rac-lactide does not form an inclusion complex with β-CD. 27;3
Published: 2022

23. Versatility of Supported Gold Nanoparticles on Hydrotalcites used for Oxidation and Reduction Reactions

Author: Drault, Fabien, Snoussi, Youssef, Ferraz, Camila, Thuriot-Roukos, Joelle, Heyte, Svetlana, Junior, Ivaldo, Marinova, Maya, Paul, Sébastien, Wojcieszak, Robert, Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Universidade Federal do Rio de Janeiro (UFRJ), Institut Michel Eugène Chevreul - FR 2638 (IMEC), and Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)
Subjects: catalysis, oxidation, CO 2, Gold nanoparticles, reduction, furfural, [CHIM.CATA]Chemical Sciences/Catalysis
Abstract: Regardless of their size, supported gold nanoparticles are largely used for liquid-phase oxidation reactions. Small gold nanoparticles exhibit good performance during the reduction of organic compounds. The direct reduction of carboxylic acid to aldehyde is a famous and familiar reaction in the field of organic chemistry and is considered as one of the fundamental chemical transformations. Herein, we present Au/hydrotalcite, Au/MgO, and Au/Al2O3 systems as heterogeneous versatile catalysts to realize the oxidation of furfural (FF) to furoic acid (FA) and realize the reduction of FA to FF. Experiments showed that in standard aqueous conditions under air, FF can be easily oxidized to FA. When DMSO was used as a solvent to conduct the experiments under an atmosphere of CO2, FA was reduced to FF. The Au/HT series of catalysts was found to be active in both transformations, pointing out the versatility of the gold-based catalysts. The activity significantly depends on the acid-base properties of the catalyst.
Published: 2022

24. Combining heteronuclear correlation NMR with spin-diffusion to detect relayed Cl-H-H and N-H-H proximities in molecular solids

Author: Parth Raval, Julien Trébosc, Tomasz Pawlak, Yusuke Nishiyama, Steven P. Brown, G.N. Manjunatha Reddy, UCCS Équipe RMN et matériaux inorganiques, Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), UCCS Équipe Catalyse Supramoléculaire, Department of Bioorganic Chemistry Centre of Molecular and Macromolecular Studies Polish Academy of Sciences, Polish Academy of Sciences (PAN), RIKEN Center for Life Science Technologies (RIKEN CLST), RIKEN - Institute of Physical and Chemical Research [Japon] (RIKEN), Department of Physics [Coventry], University of Warwick [Coventry], European Project: 795091,H2020,H2020-MSCA-IF-2017,ZEOCATALYST(2019), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Centre of Molecular and Macromolecular Studies, Polska Akademia Nauk = Polish Academy of Sciences (PAN), Université de Lille, CNRS, Centrale Lille, ENSCL, Univ. Artois, Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181, and RIKEN Center for Life Science Technologies [RIKEN CLST]
Subjects: Nuclear and High Energy Physics, Magnetic Resonance Spectroscopy, Radiation, GIPAW, Dopamine, Structure elucidation, NMR crystallography, General Chemistry, [CHIM.MATE]Chemical Sciences/Material chemistry, [CHIM.THER]Chemical Sciences/Medicinal Chemistry, Fast MAS, DFT, Solid-state NMR, HMQC, Pharmaceutical, [CHIM.THEO]Chemical Sciences/Theoretical and/or physical chemistry, [CHIM.CRIS]Chemical Sciences/Cristallography, QD, Histidine, Protons, Nuclear Magnetic Resonance, Biomolecular, Instrumentation, QC
Abstract: International audience; Analysis of short-to-intermediate range intermolecular interactions offers a great way of characterizing the solid-state organization of small molecules and materials. This can be achieved by two-dimensional (2D) homo- and heteronuclear correlation NMR spectroscopy, for example, by carrying out experiments at high magnetic fields in conjunction with fast magic-angle spinning (MAS) techniques. But, detecting 2D peaks for heteronuclear dipolar coupled spin pairs separated by greater than 3 Å is not always straightforward, particularly when low-gamma quadrupolar nuclei are involved. Here, we present a 2D correlation NMR experiment that combines the advantages of heteronuclear-multiple quantum coherence (HMQC) and proton-based spin-diffusion (SD) pulse sequences using radio-frequency-driven-recouping (RFDR) to probe inter and intramolecular 1H-X (X = 14N, 35Cl) interactions. This experiment can be used to acquire 2D 1H{X}-HMQC filtered 1H–1H correlation as well as 2D 1H-X HMQC spectra. Powder forms of dopamine·HCl and l-histidine·HCl·H2O are characterized at high fields (21.1 T and 18.8 T) with fast MAS (60 kHz) using the 2D HMQC-SD-RFDR approach. Solid-state NMR results are complemented with NMR crystallography analyses using the gauge-including projector augmented wave (GIPAW) approach. For histidine·HCl·H2O, 2D peaks associated with 14N–1H–1H and 35Cl–1H–1H distances of up to 4.4 and 3.9 Å have been detected. This is further corroborated by the observation of 2D peaks corresponding to 14N–1H–1H and 35Cl–1H–1H distances of up to 4.2 and 3.7 Å in dopamine·HCl, indicating the suitability of the HMQC-SD-RFDR experiments for detecting medium-range proximities in molecular solids.
Published: 2022

25. Lactide Lactone Chain Shuttling Copolymerization Mediated by an Aminobisphenolate Supported Aluminum Complex and Al(OiPr)3: Access to New Polylactide Based Block Copolymers

Author: Julie Meimoun, Choltirosn Sutapin, Grégory Stoclet, Audrey Favrelle, Pascal Roussel, Marc Bria, Suwabun Chirachanchai, Fanny Bonnet, Philippe Zinck, Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Biotechnology Program, Faculty of Science, Chulalongkorn University, 254 Phayathai Road, Pathumwan, Bangkok 10330, Thailand., Unité Matériaux et Transformations - UMR 8207 (UMET), Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), ANR-21-CE06-0024,PLANAVETTE,Copolymérisation statistique par navette d'esters cycliques, une voie d'accès à de nouveaux copolymères multiblocs à base de PLA(2021), Centrale Lille Institut (CLIL)-Université d'Artois (UA)-Centrale Lille-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Lille, Institut de Chimie du CNRS (INC)-Institut National de la Recherche Agronomique (INRA)-Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Ecole Nationale Supérieure de Chimie de Lille (ENSCL), and Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL)
Subjects: Catalysts, 010405 organic chemistry, Copolymers, Ring-opening polymerization, General Chemistry, [CHIM.MATE]Chemical Sciences/Material chemistry, 010402 general chemistry, 01 natural sciences, Biochemistry, Catalysis, 0104 chemical sciences, Lactones, Colloid and Surface Chemistry, [CHIM.POLY]Chemical Sciences/Polymers, Copolymerization
Abstract: International audience; The chain shuttling ring-opening copolymerization of L-lactide with epsilon-caprolactone has been achieved using two aluminum catalysts presenting different selectivities and benzyl alcohol as chain transfer agent. A newly synthesized aminobispheno-late supported aluminum complex affords the synthesis of lactone rich poly(L-lactide-co-lactone) statistical copolymeric blocks, while Al(OiPr)3 produces semi-crystalline poly(L-lactide) rich blocks. Transalkoxylation is shown to operate efficient-ly. The crystalline ratio and glass transition temperatures of these new class of polylactide based block copolymers can be tuned by adjusting the catalysts and the comonomers ratio.
Published: 2021

26. Multiscale investigation of the crystallization mechanisms and solute redistribution during annealing of a Fe64B24Y4Nb6Al0.4 metallic glass

Author: Ahmed Addad, Maya Marinova, Xavier Sauvage, Marie-NoËlle Avettand-Fènoël, Unité Matériaux et Transformations - UMR 8207 (UMET), Institut de Chimie du CNRS (INC)-Institut National de la Recherche Agronomique (INRA)-Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Ecole Nationale Supérieure de Chimie de Lille (ENSCL), Groupe de physique des matériaux (GPM), Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche sur les Matériaux Avancés (IRMA), Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), and Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)
Subjects: Materials science, D. transmission electron microscopy, Nucleation, 02 engineering and technology, Atom probe, 01 natural sciences, Annealing (glass), law.invention, law, Phase (matter), 0103 physical sciences, Materials Chemistry, Crystallization, 010302 applied physics, Amorphous metal, Mechanical Engineering, A. Fe based metallic glass, Metals and Alloys, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Microstructure, Atom probe tomography, Chemical engineering, Mechanics of Materials, D. X-ray diffractometry, 0210 nano-technology, Glass transition, Primary crystallization
Abstract: International audience; The mechanisms and the sequence of crystallization of a Fe64B24Y4Nb6Al0.4 metallic glass were investigated experimentally. To this end, the microstructure of the metallic glass after interrupted isothermal treatments at a temperature between glass transition and primary crystallization was studied by complementary techniques, namely atom probe tomography, transmission electron microscopy and X-ray diffractometry. During the early stages of crystallization of the glass, some nanometric (Fe,Nb)B crystals nucleate first by rejecting Y at their interface, which hinders their growth. The Fe62B14Y3 dendritic phase starts growing in a second step. Longer annealings lead to the development of chemical gradients in the amorphous matrix surrounding Fe62B14Y3 crystals, which favors the nucleation of additional nanometric (Fe,Nb)2.4B crystals.
Published: 2021

27. Molecular beam epitaxial growth of multilayer 2D-boron nitride on Ni substrates from borazine and plasma-activated nitrogen

Author: Jawad Hadid, Ivy Colambo, Jose Avila, Alexandre Plaud, Christophe Boyaval, Dominique Deresmes, Nicolas Nuns, Pavel Dudin, Annick Loiseau, Julien Barjon, Xavier Wallart, Dominique Vignaud, EPItaxie et PHYsique des hétérostructures - IEMN (EPIPHY - IEMN), Institut d’Électronique, de Microélectronique et de Nanotechnologie - UMR 8520 (IEMN), Centrale Lille-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Université Polytechnique Hauts-de-France (UPHF)-JUNIA (JUNIA), Université catholique de Lille (UCL)-Université catholique de Lille (UCL)-Centrale Lille-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Université Polytechnique Hauts-de-France (UPHF)-JUNIA (JUNIA), Université catholique de Lille (UCL)-Université catholique de Lille (UCL), University of the Philippines Los Baños (UP Los Baños), Synchrotron SOLEIL (SSOLEIL), Centre National de la Recherche Scientifique (CNRS), Université Paris-Saclay, ONERA, CNRS, Laboratoire d'étude des microstructures (LEM), ONERA-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS), Groupe d'Etude de la Matière Condensée (GEMAC), Université de Versailles Saint-Quentin-en-Yvelines (UVSQ)-Centre National de la Recherche Scientifique (CNRS), Centrale de Micro Nano Fabrication - IEMN (CMNF - IEMN), Plateforme de Caractérisation Multi-Physiques - IEMN (PCMP - IEMN), Institut des Molécules et de la Matière Condensée de Lille (IMMCL), Université de Lille, Sciences et Technologies-Centrale Lille-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), ONERA, Université Paris Saclay [Châtillon], ONERA-Université Paris-Saclay, The financial supports by the 2DHetero FLAG-ERA project and the French RENATECH network are greatly acknowledged. The authors thanks S. Ben Salk for providing an exfoliated hBN sample., Renatech Network, CMNF, PCMP PCP, and ANR-19-GRF1-0007,2DHetero,hBN/Graphene 2D Heterostructures: from scalable growth to integration(2019)
Subjects: Mechanics of Materials, Mechanical Engineering, General Materials Science, Bioengineering, General Chemistry, [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, Electrical and Electronic Engineering, [SPI.MAT]Engineering Sciences [physics]/Materials
Abstract: 2D boron nitride (2D-BN) was synthesized by gas-source molecular beam epitaxy on polycrystalline and monocrystalline Ni substrates using gaseous borazine and active nitrogen generated by a remote plasma source. The excess of nitrogen atoms allows to overcome the thickness self-limitation active on Ni when using borazine alone. The nucleation density and the shape of the 2D-BN domains are clearly related to the Ni substrate preparation and to the growth parameters. Based on spatially-resolved photoemission spectroscopy and on the detection of the π plasmon peak, we discuss the origin of the N1s and B1s components and their relationship with an electronic coupling at the interface. After optimization of the growth parameters, a full 2D-BN coverage is obtained, although the material thickness is not evenly distributed. The 2D-BN presents a granular structure on (111) oriented Ni grains, showing a rather poor cristallographic quality. On the contrary, high quality 2D-BN is found on (101) and (001) Ni grains, where triangular islands are observed whose lateral size is limited to ∼20 μm.
Published: 2022

28. Labeling and probing the silica surface using mechanochemistry and 17O NMR spectroscopy

Author: Philippe Gaveau, Dinu Iuga, Emilie Thomassot, Julien Trébosc, Danielle Laurencin, Mark E. Smith, Nicolas Fabregue, Frederic Mentink-Vigier, Ieva Goldberga, Thomas-Xavier Métro, Kuizhi Chen, Zhehong Gan, Chia-Hsin Chen, Bruno Alonso, Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier (ICGM ICMMM), Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Centre National de la Recherche Scientifique (CNRS)-Université de Montpellier (UM)-Université Montpellier 1 (UM1)-Université Montpellier 2 - Sciences et Techniques (UM2)-Institut de Chimie du CNRS (INC), National High Magnetic Field Laboratory (NHMFL), Florida State University [Tallahassee] (FSU), Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Centrale Lille Institut (CLIL)-Université d'Artois (UA)-Centrale Lille-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Lille, Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), Centre de Recherches Pétrographiques et Géochimiques (CRPG), Institut national des sciences de l'Univers (INSU - CNRS)-Université de Lorraine (UL)-Centre National de la Recherche Scientifique (CNRS), University of Warwick [Coventry], University of Southampton, Institut des Biomolécules Max Mousseron [Pôle Chimie Balard] (IBMM), Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Institut de Chimie du CNRS (INC)-Université de Montpellier (UM)-Centre National de la Recherche Scientifique (CNRS), Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM), Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier (ICGM), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), and Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)
Subjects: Analytical chemistry, Hot Paper, surface chemistry, 02 engineering and technology, [CHIM.INOR]Chemical Sciences/Inorganic chemistry, 010402 general chemistry, Mass spectrometry, 01 natural sciences, Catalysis, Isotopic labeling, chemistry.chemical_compound, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Mechanochemistry, TheoryofComputation_ANALYSISOFALGORITHMSANDPROBLEMCOMPLEXITY, Reactivity (chemistry), O-17, Spectroscopy, ComputingMilieux_MISCELLANEOUS, Fumed silica, Full Paper, 17O, Organic Chemistry, General Chemistry, [CHIM.MATE]Chemical Sciences/Material chemistry, Full Papers, 021001 nanoscience & nanotechnology, 3. Good health, 0104 chemical sciences, solid state NMR spectroscopy, Solid-state nuclear magnetic resonance, chemistry, silica, Siloxane, mechanochemistry, 0210 nano-technology
Abstract: In recent years, there has been increasing interest in developing cost‐efficient, fast, and user‐friendly 17O enrichment protocols to help to understand the structure and reactivity of materials by using 17O NMR spectroscopy. Here, we show for the first time how ball milling (BM) can be used to selectively and efficiently enrich the surface of fumed silica, which is widely used at industrial scale. Short milling times (up to 15 min) allowed modulation of the enrichment level (up to ca. 5 %) without significantly changing the nature of the material. High‐precision 17O compositions were measured at different milling times by using large‐geometry secondary‐ion mass spectrometry (LG‐SIMS). High‐resolution 17O NMR analyses (including at 35.2 T) allowed clear identification of the signals from siloxane (Si−O−Si) and silanols (Si−OH), while DNP analyses, performed by using direct 17O polarization and indirect 17O{1H} CP excitation, agreed with selective labeling of the surface. Information on the distribution of Si−OH environments at the surface was obtained from 2D 1H−17O D‐HMQC correlations. Finally, the surface‐labeled silica was reacted with titania and using 17O DNP, their common interface was probed and Si−O−Ti bonds identified., A fast, user‐friendly17O enrichment approach by ball milling was developed to selectively enrich the surface of fumed silica. A variety of high‐resolution solid‐state 17O NMR experiments (ultra‐high magnetic field (35.2 T), 17O MQMAS, 2D 17O−1H D‐HMQC, 17O DNP), demonstrate that siloxane and different silanol bonds present at the surface, including H‐bonded and isolated silanols, can be labeled and characterized in detail.
Published: 2021

29. Efficient transfer of DNP-enhanced 1H magnetization to half-integer quadrupolar nuclei in solids at moderate spinning rate

Author: Hiroki Nagashima, Olivier Lafon, Julien Trébosc, Jean-Paul Amoureux, Yoshihiro Kon, National Institute of Advanced Industrial Science and Technology (AIST), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), and ANR-18-CE08-0015,ThinGlass,Amélioration raisonnée de la conductivité des films minces de LiPON en élucidant leur structure à l'échelle atomique(2018)
Subjects: half-integer quadrupolar nuclei, adiabatic pulse, 010405 organic chemistry, Chemistry, General Chemistry, 010402 general chemistry, Polarization (waves), 01 natural sciences, Molecular physics, 0104 chemical sciences, Magnetization, Dipole, Solid-state nuclear magnetic resonance, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, solid-state NMR, General Materials Science, Half-integer, DNP, Insensitive nuclei enhanced by polarization transfer, Adiabatic process, Spinning
Abstract: We show herein how the proton magnetization enhanced by dynamic nuclear polarization (DNP) can be efficiently transferred at moderate magic-angle spinning (MAS) frequencies to half-integer quadrupolar nuclei, S ≥ 3/2, using the Dipolar-mediated Refocused Insensitive Nuclei Enhanced by Polarization Transfer (D-RINEPT) technique, in which a symmetry-based SR412 recoupling scheme built from adiabatic inversion 1 H pulses reintroduces the 1 H-S dipolar couplings, while suppressing the 1 H-1 H ones. The use of adiabatic pulses also improves the robustness to offsets and radiofrequency (rf)-field inhomogeneity. Furthermore, the efficiency of the polarization transfer is further improved by using 1 H composite pulses and continuous-wave irradiations between the recoupling blocks, as well as by manipulating the S satellite transitions during the first recoupling block. Furthermore, in the case of large 1 H-S dipolar couplings, the D-RINEPT variant with two pulses on the quadrupolar channel results in an improved transfer efficiency. We compare here the performances of this new adiabatic scheme with those of its parent version with single π pulses, as well as with those of PRESTO and CPMAS transfers. This comparison is performed using simulations as well as DNP-enhanced 27 Al, 95 Mo, and 17 O NMR experiments on isotopically unmodified γ-alumina, hydrated titania-supported MoO3 , Mg(OH)2 , and l-histidine·HCl·H2 O. The introduced RINEPT method outperforms the existing methods, both in terms of efficiency and robustness to rf-field inhomogeneity and offset.
Published: 2021

30. Playing on 3D spatial distribution of Cu-Co (oxide) nanoparticles in inorganic mesoporous sieves:Impact on catalytic performance toward the cinnamaldehyde hydrogenation

Author: Alexandru Chirieac, Sandrine Arii-Clacens, Brandusa Dragoi, Jérémy Dhainaut, Adrian Ungureanu, Sébastien Royer, Emil Dumitriu, Carmen Ciotonea, Maya Marinova, Stéphane Pronier, Jean-Philippe Dacquin, Université de Lille, CNRS, Centrale Lille, ENSCL, Univ. Artois, Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS], Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Centrale Lille Institut (CLIL)-Université d'Artois (UA)-Centrale Lille-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Lille, Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), and Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)
Subjects: 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Catalysis, law.invention, chemistry.chemical_compound, Transition metal oxide, Mesoporous support, Supported catalyst, Bimetallic catalyst, Hydrogenation reaction, Transition metal, law, Calcination, Bimetallic strip, Incipient wetness impregnation, Cinnamyl alcohol, Process Chemistry and Technology, [CHIM.CATA]Chemical Sciences/Catalysis, 021001 nanoscience & nanotechnology, 0104 chemical sciences, chemistry, Chemical engineering, 0210 nano-technology, Mesoporous material, Dispersion (chemistry)
Abstract: International audience; The preparation of supported bimetallic materials based on transition metals has attracted much interest since their use as catalysts towards hydrogenation processes for the production of fine chemicals or environmental depollution processes. The synthesis procedure proposed in this study allows to obtain bimetallic materials with high dispersion of the active sites, control of the chemical composition and localization as well as good thermal resistance against sintering. In this line, a series of materials based on Cu and Co supported on SBA-15 were prepared by the optimization of the drying step during incipient wetness impregnation, the ratio of Cu-Co was studied and the monometallic materials were used for comparison. The physico-chemical properties of freshly calcined and reduced materials were investigated by ICP-EOS, nitrogen physisorption, ex-situ and in-situ XRD, TEM-EDX, TPR and XPS. The materials showed improved dispersion at low copper ratio, due to the stabilization of CuxCo(1-x)Co2O4 spinel phase, promoting a high dispersion of confined NPs of 9 nm within the large pores of the SBA-15. Subsequent stabilization of the Cu and Co NPs is observed by in situ-XRD, and the collected HAADF micrographs clearly evidence a high dispersion of the copper within the bimetallic NPs. However, when copper is exceeding the CuCo ratio of 4:1, larger NPs of CuO located outside the silica mesopores are observed. Subsequent catalytic performances were investigated in the hydrogenation reaction of cinnamaldehyde (CNA), in two different pressure regimes (1 bar and 10 bars). For the reaction under pressure, CuCo1:4 showed the highest conversion with 67 mol % after 150 min of reaction, while the selectivity to the cinnamyl alcohol (CNOL) was of 47 mol %. The same catalyst showed a conversion of 99 mol % in atmospheric pressure after 24 h of reaction and the selectivity to CNOL reached 72 mol %. Such results confirm that our modified IWI protocol using mild drying step is valuable towards the preparation of confined bimetallic nanoparticles within mesoporous sieves. High stability of such confined nanoparticles allow reduction of the active elements up to the metallic state, which strongly promotes the catalytic performance towards CNA hydrogenation reaction.
Published: 2021

31. Isonitrile ruthenium and iron PNP complexes: synthesis, characterization and catalytic assessment for base-free dehydrogenative coupling of alcohols

Author: Duc Hanh Nguyen, Delphine Merel, Xavier Trivelli, Régis Gauvin, Frédéric Capet, Nicolas Merle, Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Centrale Lille Institut (CLIL)-Université d'Artois (UA)-Centrale Lille-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Lille, Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), Institut de Recherche de Chimie Paris (IRCP), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Ministère de la Culture (MC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), and Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Ministère de la Culture (MC)
Subjects: 010405 organic chemistry, Hydride, Isocyanide, Cationic polymerization, chemistry.chemical_element, isonitrile. Supporting Information Placeholder, [CHIM.CATA]Chemical Sciences/Catalysis, 010402 general chemistry, Metathesis, 01 natural sciences, Medicinal chemistry, Catalysis, 0104 chemical sciences, Pincer movement, Ruthenium, Inorganic Chemistry, chemistry.chemical_compound, Deprotonation, iron, chemistry, Bromide, pincer ligands, Dehydrogenation, ruthenium
Abstract: Neutral and ionic ruthenium and iron aliphatic PNPH-type pincer complexes (PNPH= NH(CH2CH2PiPr2)2) bearing benzyl, n-butyl or tert-butyl isocyanide ancillary ligands have been prepared and characterized. Reaction of [RuCl2(PNPH)]2 with one equivalent CN-R per ruthe-nium center affords complexes [Ru(PNPH)Cl2(CNR)] (R= benzyl, 1a, R= n-butyl, 1b, R= t-butyl, 1c), with cationic [Ru(PNPH)(Cl)(CNR)2]Cl 2a-c as side-products. Complexes 2a-c are selectively prepared upon reaction of [RuCl2(PNPH)]2 with 2 equiva-lents of isonitrile per ruthenium center. Dichloride species 1a-c react with excess NaBH4 to afford [Ru(PNPH)(H)(BH4)(CN-R)] 3a-c, analogues to benchmark Takasago catalyst [Ru(PNP)(H)(BH4)(CO)]. Reaction of 1a-c with a single equivalent of NaBH4 under protic conditions results in formation of hydrido chloride derivatives [Ru(PNPH)(H)(Cl)(CN-R)] (4a-c), from which 3a-c can be prepared upon reaction with excess NaBH4. Use of one equivalent of NaHBEt3 with 4a and 4c affords bishydrides [Ru(PNPH)(H)2(CN-R)] 5a and 5c. In the case of bulkier t-butylisonitrile, two isomers were observed by NMR, with the PNP framework in either meridional or facial confor-mation. Deprotonation of 4c by KOtBu generates amido derivative [Ru(PNP’)(H)(CN-t-Bu)] (6, PNP’= -N(CH2CH2PiPr2)2), unstable in solution. Addition of excess benzylisonitrile to 4a provides cationic hydride [Ru(PNPH)(H)(CN-CH2Ph)2]Cl (7). Concerning iron chemis-try, [Fe(PNPH)Br2] reacts one equivalent benzylisonitrile to afford [Fe(PNPH)(Br)(CNCH2Ph)2]Br (8). The outer-sphere bromide anion can be exchanged by salt metathesis with NaBPh4 to generate [Fe(PNPH)(Br)(CNCH2Ph)2](BPh4) (9). Cationic hydride species [Fe(PNPH)(H)(CN-t-Bu)2](BH4) (10) is prepared from consecutive addition of excess CN-t-Bu and NaBH4 on [Fe(PNPH)Br2]. Ruthenium complexes 3a-c are active in acceptorless alcohol dehydrogenative coupling into ester under base-free conditions. From kinetic follow-up, the trend in initial activity is 3a ≈ 3b > [Ru(PNPH)(H)(BH4)(CO)] >> 3c; for robustness, [Ru(H)(BH4)(CO)(PNPH)] > 3a > 3b >> 3c. Hy-potheses are given to account for the observed deactivation. Complexes 3b, 3c, 4a, 4c, 5c, 7, cis-8 and 9 were characterized by X-ray crystallography.
Published: 2021

32. Azobenzene: a Visible‐Light Chemical Actinometer for the Characterization of Fluidic Photosystems

Author: Xavier Trivelli, François Xavier Cantrelle, Laëtitia Chausset-Boissarie, Maël Penhoat, Mélanie Roseau, Vincent De Waele, Miniaturisation pour la Synthèse, l’Analyse et la Protéomique - USR 3290 (MSAP), Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Institut de Chimie du CNRS (INC), Laboratoire Avancé de Spectroscopie pour les Intéractions la Réactivité et l'Environnement - UMR 8516 (LASIRE), Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Centrale Lille Institut (CLIL), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), Biologie Structurale Intégrative (ERL 9002 - BSI ), Institut Pasteur de Lille, Réseau International des Instituts Pasteur (RIIP)-Réseau International des Instituts Pasteur (RIIP)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Facteurs de Risque et Déterminants Moléculaires des Maladies liées au Vieillissement - U 1167 (RID-AGE), Réseau International des Instituts Pasteur (RIIP)-Réseau International des Instituts Pasteur (RIIP)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Université de Lille-Centre Hospitalier Régional Universitaire [Lille] (CHRU Lille), The authors gratefully acknowledge the CNRS, Lille University and ANR (ANR-19-CE07-0014) for the financial support., ANR-19-CE07-0014,FloRyn,Photochimie en flux continu et intermédiaires réactifs à courte durée de vie une combinaison gagnante(2019), Chausset-Boissarie, laetitia, Photochimie en flux continu et intermédiaires réactifs à courte durée de vie une combinaison gagnante - - FloRyn2019 - ANR-19-CE07-0014 - AAPG2019 - VALID, Miniaturisation pour la Synthèse, l’Analyse et la Protéomique - UAR 3290 (MSAP), Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), and Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)
Subjects: azo compounds, actinometry, 010402 general chemistry, Photochemistry, 01 natural sciences, Biochemistry, Catalysis, law.invention, Inorganic Chemistry, chemistry.chemical_compound, law, Drug Discovery, [CHIM] Chemical Sciences, [CHIM]Chemical Sciences, Fluidics, Physical and Theoretical Chemistry, microfluidic photoreactor, visible light, Photosystem, Actinometer, photochemistry, 010405 organic chemistry, [CHIM.ORGA]Chemical Sciences/Organic chemistry, Organic Chemistry, [CHIM.ORGA] Chemical Sciences/Organic chemistry, 0104 chemical sciences, Characterization (materials science), azobenzene, Azobenzene, chemistry, Visible spectrum
Abstract: International audience; (E)-Azobenzene is introduced as a suitable chemical actinometer in the visible spectral range (440–540 nm) for photon flux determination of fluidic microphotoreactors or for assessing efficiency of visible light photo-induced reactions, its evaluation is straightforward without tedious analytics. Photoisomerization quantum yields (ΦE→Z) of (E)-azobenzene were accurately determined upon irradiation at several wavelengths and in different solvents based on well-known diarylethene.
Published: 2021

33. Surface molecular imprinting over supported metal catalysts for size-dependent selective hydrogenation reactions

Author: Vitaly V. Ordomsky, Olga V. Safonova, Willinton Y. Hernández, Dan Wu, Ahmed Addad, Andrei Y. Khodakov, Evgeny I. Vovk, Walid Baaziz, Bang Gu, Maya Marinova, Ovidiu Ersen, Nicolas Nuns, Wen-Juan Zhou, Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut de chimie et procédés pour l'énergie, l'environnement et la santé (ICPEES), Université de Strasbourg (UNISTRA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Matériaux et Nanosciences Grand-Est (MNGE), Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Eco-Efficient Products & Processes Laboratory (E2P2L), RHODIA-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Chimie - UMR5182 (LC), École normale supérieure de Lyon (ENS de Lyon)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Physique et Chimie des Matériaux de Strasbourg (IPCMS), Université de Strasbourg (UNISTRA)-Centre National de la Recherche Scientifique (CNRS)-Matériaux et Nanosciences Grand-Est (MNGE), Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Réseau nanophotonique et optique, Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Centre National de la Recherche Scientifique (CNRS), Paul Scherrer Institute (PSI), Unité Matériaux et Transformations - UMR 8207 (UMET), Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Centrale Lille Institut (CLIL)-Université d'Artois (UA)-Centrale Lille-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Lille, Université de Strasbourg (UNISTRA)-Matériaux et nanosciences d'Alsace (FMNGE), Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), Eco-Efficient Products &Processes Laboratory (E2PL2), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-RHODIA, Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-École normale supérieure - Lyon (ENS Lyon)-Institut de Chimie du CNRS (INC), Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut National de la Santé et de la Recherche Médicale (INSERM)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)-Réseau nanophotonique et optique, Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Centre National de la Recherche Scientifique (CNRS)-Université de Strasbourg (UNISTRA), and Institut de Chimie du CNRS (INC)-Institut National de la Recherche Agronomique (INRA)-Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)
Subjects: Steric effects, chemistry.chemical_classification, Chemistry, Process Chemistry and Technology, Bioengineering, 02 engineering and technology, Polymer, 010402 general chemistry, 021001 nanoscience & nanotechnology, Heterogeneous catalysis, 01 natural sciences, Biochemistry, Combinatorial chemistry, Catalysis, 0104 chemical sciences, Adsorption, Molecule, [CHIM]Chemical Sciences, 0210 nano-technology, Selectivity, Molecular imprinting, ComputingMilieux_MISCELLANEOUS
Abstract: Molecular imprinting of polymer matrices enables the creation of template-shaped cavities with high affinity for molecules of given shape and size. Here we introduce a surface molecular imprinting strategy to control the hydrogenation selectivity of various aromatic molecules over a supported palladium catalyst. This strategy involves the sequential adsorption over the metal surface of an aromatic template molecule followed by poisoners, resulting in the formation of non-poisoned active islands of predetermined shape and size. Because of steric constraints, these active islands exhibit high selectivity in the chemical conversion of aromatic molecules that correspond in size and shape to the templates. The elaborated strategy enables a practical application relevant to selective hydrogenation and removal of carcinogenic benzene from mixtures of aromatics. Molecular imprinting can facilitate size- and shape-selective reactions beyond traditional approaches based on porous materials, but is still not fully established for heterogeneous catalysts. Here a molecular imprinting approach is introduced to generate a supported palladium catalyst for the selective hydrogenation of benzene from mixtures of aromatic molecules.
Published: 2021

34. Hydrodeoxygenation of m-cresol over Pd/Al-SBA-15 catalysts: Effect of Al content on the deoxygenation reaction pathways

Author: Camila A. Teles, Carmen Ciotonea, Nicolas. Gomes, Vinicius O.O. Gonçalves, Adrian Ungureanu, Cezar Catrinescu, Maya Marinova, Jean-Marc Clacens, Sébastien Royer, Fábio B. Noronha, Frédéric Richard, Institut de Chimie des Milieux et Matériaux de Poitiers (IC2MP), Université de Poitiers-Institut national des sciences de l'Univers (INSU - CNRS)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Unité de Chimie Environnementale et Interactions sur le Vivant (UCEIV), Université du Littoral Côte d'Opale (ULCO), Universidade Federal do Rio de Janeiro (UFRJ), 'Gheorghe Asachi' Technical University of Iasi (TUIASI), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), and ANR-16-IDEX-0004,ULNE,ULNE(2016)
Subjects: SBA-15, HDO M-cresol Palladium, [CHIM.ORGA]Chemical Sciences/Organic chemistry, aluminium, Process Chemistry and Technology, [CHIM.CATA]Chemical Sciences/Catalysis, acidity, Catalysis
Abstract: International audience; The effect of aluminium content (x = 5, 20 and 40 wt %) in SBA-15 type silica supports used to obtain Pd/xAl-SBA-15 catalysts was evaluated in the HDO reaction of m-cresol at 300 ◦C, under atmospheric and high (30 bar) pressure. Aluminium incorporation was performed using the two-step pH-adjustment method, affording the deposition of Al phases over silica previously precipitated. Pd was thereafter deposed using incipient wetnessimpregnation. Physico-chemical properties of the catalysts were investigated by XRD, N2 physisorption, H2 chemisorption, DRIFTS of adsorbed pyridine, STEM-EDX mapping coupled to HAADF imaging. The acidity (Brønsted and Lewis sites) generated by the incorporation of aluminium at low content (i.e. 5 wt %) onto the SBA-15 structure resulted in the improvement of HDO of m-cresol, with an increase in selectivity toward thedeoxygenated products, toluene under atmospheric pressure (38 % for the Pd/SBA vs. 77 % for the Pd/Al5-SBA) and methylcyclohexane under high pressure (14 % for the Pd/SBA vs. 30 % for Pd/Al5-SBA). The selectivity into methylcyclohexanone was also affected by the total pressure: 5 % under atmospheric pressure vs 64 % under 30 bar over Pd/Al5-SBA). However, under atmospheric pressure, at higher Al contents, side reactions catalyzed by acid sites were promoted, such as isomerization and disproportionation reactions, which were not observed under high pressure. Besides that, the increase of quantity of Al leaded to the decrease of the surface accessibility and hence drop on the reactions rate over both pressure conditions. This work demonstrated the efficiency of Pd catalyst in HDO reaction which can be obtained by a precise adjustment of the quantity of Al in the SBA catalyticsupport.
Published: 2022

35. Rubrolone production by Dactylosporangium vinaceum: biosynthesis, modulation and possible biological function

Author: David Hot, Nicolas Willand, Delphine Beury, Ségolène Caboche, Baptiste Villemagne, Sophie Moureu, Florence Maurier, Hervé Drobecq, Eva Desmecht, Ghaffar Muharram, Adrien Herledan, Xavier Trivelli, Ruben C. Hartkoorn, Thibault Caradec, Peggy Bouquet, Centre d’Infection et d’Immunité de Lille - INSERM U 1019 - UMR 9017 - UMR 8204 (CIIL), Centre National de la Recherche Scientifique (CNRS)-Centre Hospitalier Régional Universitaire [Lille] (CHRU Lille)-Université de Lille-Institut National de la Santé et de la Recherche Médicale (INSERM)-Institut Pasteur de Lille, Réseau International des Instituts Pasteur (RIIP)-Réseau International des Instituts Pasteur (RIIP), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), Plateformes Lilloises en Biologie et Santé - UMS 2014 - US 41 (PLBS), Institut Pasteur de Lille, Réseau International des Instituts Pasteur (RIIP)-Réseau International des Instituts Pasteur (RIIP)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Université de Lille-Centre Hospitalier Régional Universitaire [Lille] (CHRU Lille)-Centre National de la Recherche Scientifique (CNRS), Médicaments et molécules pour agir sur les Systèmes Vivants - U 1177 (M2SV), Réseau International des Instituts Pasteur (RIIP)-Réseau International des Instituts Pasteur (RIIP)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Université de Lille, We are thankful for the support from the NMR facility, where the Bruker 600 AVANCEIII HD equipped with a 5 mm cryo-probe HDCNF (CP-QCI) spectrometer was cofunded by the European Union with the European Regional Development Fund (ERDF), by the Hauts de France Regional Council (contract no. 17003781), Métropole Européenne de Lille (contract no. 2016_ESR_05), the French State (contract no. 2017-R3-CTRLPhase 1), the Pasteur Institute of Lille, the Lille University and the French CNRS., Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), and Plateformes Lilloises en Biologie et Santé - UAR 2014 - US 41 (PLBS)
Subjects: Pyridines, [SDV]Life Sciences [q-bio], Antimicrobial peptides, Computational biology, Dactylosporangium, Biosynthesis, Applied Microbiology and Biotechnology, Genome, Silent cluster, Actinobacteria, 03 medical and health sciences, chemistry.chemical_compound, Gene cluster, 030304 developmental biology, Whole genome sequencing, 0303 health sciences, Biological Products, Natural product, biology, 030306 microbiology, Conjugation, Micromonosporaceae, General Medicine, biology.organism_classification, Rubrolone, chemistry, Multigene Family, Transcriptional modulation, Bacteria, Biotechnology
Abstract: Rare actinomycetes are likely treasure troves for bioactive natural products, and it is therefore important that we enrich our understanding of biosynthetic potential of these relatively understudied bacteria. Dactylosporangium are a genus of such rare Actinobacteria that are known to produce a number of important antibacterial compounds, but for which there are still no fully assembled reference genomes, and where the extent of encoded biosynthetic capacity is not defined. Dactylosporangium vinaceum (NRRL B-16297) is known to readily produce a deep wine red-coloured diffusible pigment of unknown origin, and it was decided to define the chemical identity of this natural product pigment, and in parallel use whole genome sequencing and transcriptional analysis to lay a foundation for understanding the biosynthetic capacity of these bacteria. Results show that the produced pigment is made of various rubrolone conjugates, the spontaneous product of the reactive pre-rubrolone, produced by the bacterium. Genome and transcriptome analysis identified the highly expressed biosynthetic gene cluster (BGC) for pre-rubrolone. Further analysis of the fully assembled genome found it to carry 24 additional BGCs, of which the majority were poorly transcribed, confirming the encoded capacity of this bacterium to produce natural products but also illustrating the main bottleneck to exploiting this capacity. Finally, analysis of the potential environmental role of pre-rubrolone found it to react with a number of amine containing antibiotics, antimicrobial peptides and siderophores pointing to its potential role as a "minesweeper" of xenobiotic molecules in the bacterial environment. KEY POINTS: • D. vinaceum encodes many BGC, but the majority are transcriptionally silent. • Chemical screening identifies molecules that modulate rubrolone production. • Pre-rubrolone is efficient at binding and inactivating many natural antibiotics.
Published: 2021

36. Phosphorylation and O-GlcNAcylation of the PHF-1 Epitope of Tau Protein Induce Local Conformational Changes of the C-Terminus and Modulate Tau Self-Assembly Into Fibrillar Aggregates

Author: Cantrelle, François-Xavier, Loyens, Anne, Trivelli, Xavier, Reimann, Oliver, Despres, Clément, Gandhi, Neha, Hackenberger, Christian, Landrieu, Isabelle, Smet-Nocca, Caroline, Facteurs de Risque et Déterminants Moléculaires des Maladies liées au Vieillissement - U 1167 (RID-AGE), Institut Pasteur de Lille, Réseau International des Instituts Pasteur (RIIP)-Réseau International des Instituts Pasteur (RIIP)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Université de Lille-Centre Hospitalier Régional Universitaire [Lille] (CHRU Lille), Biologie Structurale Intégrative (ERL 9002 - BSI ), Réseau International des Instituts Pasteur (RIIP)-Réseau International des Instituts Pasteur (RIIP)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Centre de Recherche Jean-Pierre AUBERT Neurosciences et Cancer - U837 (JPArc), Université Lille Nord de France (COMUE)-Institut National de la Santé et de la Recherche Médicale (INSERM)-Université de Lille, Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Leibniz Forschungsinstitut für Molekulare Pharmakolgie = Leibniz Institute for Molecular Pharmacology [Berlin, Allemagne] (FMP), Leibniz Association, Humboldt University Of Berlin, Queensland University of Technology [Brisbane] (QUT), This work was supported by the Mizutani Foundation for Glycoscience (2018 Research Grant number 180122), the program PHC Procope/DAAD 2015 (project 33334TK) and by grants from the LabEx (Laboratory of Excellence) DISTALZ (Development of Innovative Strategies for a Transdisciplinary approach to Alzheimer’s disease). The NMR facilities were funded by the Council of Région Nord, CNRS, Pasteur Institute of Lille, European Community (FEDER), French Research Ministry and the University of Lille and by the CTRL CPER cofounded by the European Union with the European Regional Development Fund (ERDF), by the Hauts-de-France Regional Council, Métropole Européenne de Lille, and French State. We acknowledge support from the TGE RMN THC (FR-3050, France), Lille NMR and RPE Health and Biology core facility., Centre de Recherche Jean-Pierre AUBERT Neurosciences et Cancer - U1172 Inserm - U837 (JPArc), Institut National de la Santé et de la Recherche Médicale (INSERM)-Université Lille Nord de France (COMUE)-Université de Lille, Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), Humboldt-Universität zu Berlin, and Landrieu, Isabelle
Subjects: phosphorylation, [SDV.BBM.BP] Life Sciences [q-bio]/Biochemistry, Molecular Biology/Biophysics, macromolecular substances, protein aggregation, [SDV.BBM.BP]Life Sciences [q-bio]/Biochemistry, Molecular Biology/Biophysics, NMR spectroscopy, mental disorders, O-GlcNAc glycosylation, ddc:610, microtubule-associated protein tau, [SDV.BBM.BC]Life Sciences [q-bio]/Biochemistry, Molecular Biology/Biochemistry [q-bio.BM], 610 Medizin und Gesundheit, [SDV.BBM.BC] Life Sciences [q-bio]/Biochemistry, Molecular Biology/Biochemistry [q-bio.BM], Alzheimer’s disease, Neuroscience, Original Research
Abstract: International audience; Phosphorylation of the neuronal microtubule-associated Tau protein plays a critical role in the aggregation process leading to the formation of insoluble intraneuronal fibrils within Alzheimer’s disease (AD) brains. In recent years, other posttranslational modifications (PTMs) have been highlighted in the regulation of Tau (dys)functions. Among these PTMs, the O -β-linked N-acetylglucosaminylation ( O -GlcNAcylation) modulates Tau phosphorylation and aggregation. We here focus on the role of the PHF-1 phospho-epitope of Tau C-terminal domain that is hyperphosphorylated in AD (at pS396/pS404) and encompasses S400 as the major O -GlcNAc site of Tau while two additional O -GlcNAc sites were found in the extreme C-terminus at S412 and S413. Using high resolution NMR spectroscopy, we showed that the O -GlcNAc glycosylation reduces phosphorylation of PHF-1 epitope by GSK3β alone or after priming by CDK2/cyclin A. Furthermore, investigations of the impact of PTMs on local conformation performed in small peptides highlight the role of S404 phosphorylation in inducing helical propensity in the region downstream pS404 that is exacerbated by other phosphorylations of PHF-1 epitope at S396 and S400, or O -GlcNAcylation of S400. Finally, the role of phosphorylation and O -GlcNAcylation of PHF-1 epitope was probed in in-vitro fibrillization assays in which O -GlcNAcylation slows down the rate of fibrillar assembly while GSK3β phosphorylation stimulates aggregation counteracting the effect of glycosylation.
Published: 2021

37. Development of Fe-Ni/SiO2 bimetallic catalysts for furfural hydrogenation using a high-throughput screening approach

Author: Shi, D., Mamede, Anne-Sophie, Wojcieszak, Robert, Marinova, Maya, Paul, Sébastien, Marceau, Eric, Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), and Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)
Subjects: [CHIM]Chemical Sciences
Abstract: International audience
Published: 2021

38. Mitochondrial O-GlcNAc Transferase Interacts with and Modifies Many Proteins and Its Up-Regulation Affects Mitochondrial Function and Cellular Energy Homeostasis

Author: Tony Lefebvre, Anna Krześlak, Anne-Sophie Vercoutter-Edouart, Joanna Oracz, Fabrice Bray, Grażyna Budryn, Piotr Ciesielski, Karolina Kozal, Dorota Żyżelewicz, Stéphanie Flament, Paweł Jóźwiak, Piotr K. Zakrzewski, Université de Lille, CNRS, Unité de Glycobiologie Structurale et Fonctionnelle (UGSF) - UMR 8576, University of Lódź, Łódź University of Technology, Unité de Glycobiologie Structurale et Fonctionnelle UMR 8576 [UGSF], Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), Unité de Glycobiologie Structurale et Fonctionnelle (UGSF), Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Unité de Glycobiologie Structurale et Fonctionnelle - UMR 8576 (UGSF), and Université de Lille-Centre National de la Recherche Scientifique (CNRS)
Subjects: 0301 basic medicine, Cancer Research, Mitochondrial DNA, Cell, [SDV.CAN]Life Sciences [q-bio]/Cancer, Mitochondrion, Article, 03 medical and health sciences, 0302 clinical medicine, breast cancer, Downregulation and upregulation, energy metabolism, medicine, [SDV.BBM.BC]Life Sciences [q-bio]/Biochemistry, Molecular Biology/Biochemistry [q-bio.BM], glucose, Inner mitochondrial membrane, RC254-282, O-GlcNAc, Chemistry, Neoplasms. Tumors. Oncology. Including cancer and carcinogens, Translation (biology), Cell biology, mitochondria, 030104 developmental biology, medicine.anatomical_structure, Oncology, Mitochondrial matrix, 030220 oncology & carcinogenesis, mOGT, Target protein
Abstract: Simple Summary O-GlcNAcylation is a dynamic post-translational modification of proteins involved in the control of intracellular signaling pathways in response to changes in nutrient availability, especially glucose concentration. To date, most research has focused on O-GlcNAcylation of proteins by the nuclear-cytoplasmic isoform of O-GlcNAc transferase (ncOGT), while the role of mitochondrial OGT (mOGT) and its effect on O-GlcNAcylation of mitochondrial proteins are poorly understood. The aim of our study was to investigate the effect of mOGT on O-GlcNAcylation of mitochondrial proteins, mitochondrial function, and energy metabolism of breast cancer cells. Herein, we used two independent proteomics-based approaches to identify mOGT-interacting partners and proteins modified by mOGT. Based on our findings, we propose that O-GlcNAcylation of proteins by mOGT is a part of the mechanism by which glucose affects mitochondrial function and cellular bioenergetics. Abstract O-GlcNAcylation is a cell glucose sensor. The addition of O-GlcNAc moieties to target protein is catalyzed by the O-Linked N-acetylglucosamine transferase (OGT). OGT is encoded by a single gene that yields differentially spliced OGT isoforms. One of them is targeted to mitochondria (mOGT). Although the impact of O-GlcNAcylation on cancer cells biology is well documented, mOGT’s role remains poorly investigated. We performed studies using breast cancer cells with up-regulated mOGT or its catalytic inactive mutant to identify proteins specifically modified by mOGT. Proteomic approaches included isolation of mOGT protein partners and O-GlcNAcylated proteins from mitochondria-enriched fraction followed by their analysis by mass spectrometry. Moreover, we analyzed the impact of mOGT dysregulation on mitochondrial activity and cellular metabolism using a variety of biochemical assays. We found that mitochondrial OGT expression is glucose-dependent. Elevated mOGT expression affected the mitochondrial transmembrane potential and increased intramitochondrial ROS generation. Moreover, mOGT up-regulation caused a decrease in cellular ATP level. We identified many mitochondrial proteins as mOGT substrates. Most of these proteins are localized in the mitochondrial matrix and the inner mitochondrial membrane and participate in mitochondrial respiration, fatty acid metabolism, transport, translation, apoptosis, and mtDNA processes. Our findings suggest that mOGT interacts with and modifies many mitochondrial proteins, and its dysregulation affects cellular bioenergetics and mitochondria function.
Published: 2021

39. Major routes in the photocatalytic methane conversion into chemicals and fuels under mild conditions

Author: Ordomsky, Vitaly, Zhang, Songwei, Li, Jerry Pui Ho, Zhao, Jingpeng, Wu, Dan, Yuan, Biao, Hernández, Willinton Yesid, Zhou, Wen-Juan, He, Tao, Yu, Yi, Yang, Yong, Li, Tao, Hu, Di, Khodakov, Andrei, Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), ShanghaiTech University [Shanghai], Solvay (France), Laboratoire de Chimie - UMR5182 (LC), École normale supérieure de Lyon (ENS de Lyon)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Beihang University (BUAA), Centrale Lille Institut (CLIL)-Université d'Artois (UA)-Centrale Lille-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Lille, Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-École normale supérieure - Lyon (ENS Lyon)-Institut de Chimie du CNRS (INC), and Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL)
Subjects: 02 engineering and technology, 010402 general chemistry, 7. Clean energy, 01 natural sciences, Catalysis, Methane, chemistry.chemical_compound, [CHIM]Chemical Sciences, ComputingMilieux_MISCELLANEOUS, General Environmental Science, Methane reformer, business.industry, Chemistry, Process Chemistry and Technology, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Renewable energy, Chemical engineering, 13. Climate action, Anaerobic oxidation of methane, Carbon dioxide, Photocatalysis, Methanol, 0210 nano-technology, business, Selectivity
Abstract: Methane is one of the most abundant molecules on Earth. Most of the state-of-the-art methane chemical conversion technologies require high temperatures, they are accompanied by insufficient selectivity, carbon deposition and major production of carbon dioxide. Development of the methane conversion technologies at mild conditions is important for the rational utilization of renewable and fossil feedstocks and for the environment. The goal of this review is to perform a comparative analysis of low temperature methane photocatalytic conversion routes such as methane oxidation, methane reforming and methane coupling. Methane photocatalytic reforming and selective oxidation currently exhibit the highest conversion rates, while methane coupling shows the highest selectivity. The most promising routes could be methane oxidation to methanol, which simultaneously exhibits higher productivity and selectivity. Further improvements in the methane conversion can be achieved by the design of new materials, photoreactors and operating modes, such as photochemical looping and combining photocatalysis with electrocatalysis.
Published: 2021

40. Lignin Compounds to Monoaromatics: Selective Cleavage of C−O Bonds over a Brominated Ruthenium Catalyst

Author: Deizi V. Peron, Vitaly V. Ordomsky, Wen-Juan Zhou, Andrei Y. Khodakov, Maya Marinova, Zhen Yan, Dan Wu, Olga V. Safonova, Qiyan Wang, Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Eco-Efficient Products & Processes Laboratory (E2P2L), RHODIA-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Paul Scherrer Institute (PSI), Laboratoire de Chimie - UMR5182 (LC), École normale supérieure de Lyon (ENS de Lyon)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Centrale Lille Institut (CLIL)-Université d'Artois (UA)-Centrale Lille-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Lille, Eco-Efficient Products &Processes Laboratory (E2PL2), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-RHODIA, Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-École normale supérieure - Lyon (ENS Lyon)-Institut de Chimie du CNRS (INC), Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), The Swiss Light Source (SLS) (SLS-PSI), Unité Matériaux et Transformations - UMR 8207 (UMET), and Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)
Subjects: Depolymerization, 010405 organic chemistry, Aryl, Diphenyl ether, Aromaticity, General Chemistry, General Medicine, Heterogeneous catalysis, 010402 general chemistry, 01 natural sciences, Catalysis, 3. Good health, 0104 chemical sciences, chemistry.chemical_compound, chemistry, Polymer chemistry, [CHIM]Chemical Sciences, Benzene, Bond cleavage, ComputingMilieux_MISCELLANEOUS
Abstract: The cleavage of C-O linkages in aryl ethers in biomass-derived lignin compounds without hydrogenation of the aromatic rings is a major challenge for the production of sustainable mono-aromatics. Conventional strategies over the heterogeneous metal catalysts require the addition of homogeneous base additives causing environmental problems. Herein, we propose a heterogeneous Ru/C catalyst modified by Br atoms for the selective direct cleavage of C-O bonds in diphenyl ether without hydrogenation of aromatic rings reaching the yield of benzene and phenol as high as 90.3 % and increased selectivity to mono-aromatics (97.3 vs. 46.2 % for initial Ru) during depolymerization of lignin. Characterization of the catalyst indicates selective poisoning by Br of terrace sites over Ru nanoparticles, which are active in the hydrogenation of aromatic rings, while the defect sites on the edges and corners remain available and provide higher intrinsic activity in the C-O bond cleavage.
Published: 2021

41. Dissimilar aluminium – galvanized steel magnetic pulse welds: Ballistic origin of the interface and mechanical properties

Author: AVETTAND-FÈNOËL, Marie-Noëlle, Racineux, G., Marinova, Maya, Taillard, R., Unité Matériaux et Transformations - UMR 8207 (UMET), Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut de Chimie du CNRS (INC)-Institut National de la Recherche Agronomique (INRA)-Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Ecole Nationale Supérieure de Chimie de Lille (ENSCL), and Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL)
Subjects: [SPI.MAT]Engineering Sciences [physics]/Materials
Published: 2021

42. Efficiency and durability of protective treatments on cultural heritage copper corrosion layers

Author: Emilande Apchain, Philippe Dillmann, Albert Noumowe, Jean-Paul Gallien, Pascal Berger, Nicolas Nuns, Delphine Neff, Laboratoire Archéomatériaux et Prévision de l'Altération (LAPA - UMR 3685), Nanosciences et Innovation pour les Matériaux, la Biomédecine et l'Energie (ex SIS2M) (NIMBE UMR 3685), Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut de Recherches sur les Archéomatériaux (IRAMAT), Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de mécanique et matériaux du génie civil (L2MGC), Fédération INSTITUT DES MATÉRIAUX DE CERGY-PONTOISE (I-MAT), CY Cergy Paris Université (CY)-CY Cergy Paris Université (CY), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Laboratoire d'Etudes des Eléments Légers (LEEL - UMR 3685), Fondation des Sciences du Patrimoine ne (EUR-17-EURE-0021), ANR-10-LABX-0094,PATRIMA,Tangible heritage(2010), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Université Bordeaux Montaigne-Université de Technologie de Belfort-Montbeliard (UTBM), and Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL)
Subjects: Materials science, 020209 energy, General Chemical Engineering, chemistry.chemical_element, 02 engineering and technology, Corrosion, 0202 electrical engineering, electronic engineering, information engineering, General Materials Science, protective treatments, copper alloys, microcrystalline wax, Microcrystalline wax, Wax, atmospheric corrosion, Metallurgy, General Chemistry, Penetration (firestop), [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Durability, Copper, 6. Clean water, chemistry, visual_art, copper, visual_art.visual_art_medium, decanoate solution, Leaching (metallurgy), Erosion corrosion of copper water tubes, 0210 nano-technology
Abstract: International audience; To protect copper artefacts of the cultural heritage from atmospheric degradation protective treatment must be applied. Two types of protective treatments: microcrystalline wax (Cosmolloïd wax) and decanoate solution (HC10) were tested. Two aspects were considered: the penetration of the treatments in the corrosion layers, and its durability. Equivalent efficiencies for both treatments were demonstrated. The penetration of the treatments seems to depend essentially on its application mode. Re-corrosion experiments of treated samples under immersion in D2O demonstrate that the efficiency and the durability with time or after water leaching depend on the penetration of the treatments in the corrosion layers.
Published: 2021

43. Design of a metallic glass dispersion in pure copper by friction stir processing

Author: Avettand-Fènoël, M.-N., Netto, N., Simar, A., Marinova, M., Taillard, R., Univ. Lille - UMET, Unité Matériaux et Transformations, UCL - SST/IMMC/IMAP - Materials and process engineering, Univ. Lille - IMEC, Institut Michel-Eugène Chevreul, Unité Matériaux et Transformations - UMR 8207 (UMET), Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Faculté de Médecine et Médecine Dentaire [UCLouvain], Université Catholique de Louvain = Catholic University of Louvain (UCL), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), and University of Lille
Subjects: Metallic glass reinforcement, Mechanical Engineering, Metals and Alloys, Mechanical properties, [CHIM.MATE]Chemical Sciences/Material chemistry, Friction stir processing, Metallic glass reinforcement [A], Friction stir processing phase transformations [B], Copper [A], Mechanics of Materials, Mechanical properties [C], [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], Materials Chemistry, Phase transformations, Microstructure, Copper, Microstructure [C]
Abstract: International audience; Multipass friction stir processing of Fe based metallic glass ribbons interspersed between Cu plates was performed. From the first pass, the process entailed on the one hand the decrease of the Cu mean grain size in the nugget by a factor of about 5 and on the other hand the fracture, the refinement and the partial crystallization of the amorphous reinforcement. Cu diffusion also led to marked Cu enrichments in the Fe based metallic glass whose mean Cu content reached 2.7 at%. Beside the metallic glass based reinforcements, some nanometric polycrystalline copper oxides were formed and dispersed within the nugget. The nugget also experienced dynamic recovery and dynamic recrystallization which was in particular favored by the accumulation of dislocations around the reinforcements. Finally, the greater number of passes, the harder the nugget becomes.
Published: 2022

44. Thermal stability, phase transformations and mechanical properties of a Fe64B24Y4Nb6 metallic glass

Author: Roland Taillard, Marie-NoËlle Avettand-Fènoël, Wei Jiang, Maya Marinova, Unité Matériaux et Transformations - UMR 8207 (UMET), Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), University of Science and Technology of China [Hefei] (USTC), Institut de Chimie du CNRS (INC)-Institut National de la Recherche Agronomique (INRA)-Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Ecole Nationale Supérieure de Chimie de Lille (ENSCL), and Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL)
Subjects: Materials science, Alloy, 02 engineering and technology, engineering.material, 010402 general chemistry, 01 natural sciences, Indentation hardness, law.invention, Differential scanning calorimetry, law, Materials Chemistry, Crystallization, Composite material, High-resolution transmission electron microscopy, Amorphous metal, Mechanical Engineering, Metals and Alloys, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Amorphous solid, Metallic glass, Thermal stability, Crystallization, Microstructure, Instrumented microhardness, Mechanics of Materials, engineering, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], 0210 nano-technology, Glass transition
Abstract: Fe64B24Y4Nb6 metallic glass ribbon and its bulk counterpart were characterized by conventional and high rate differential scanning calorimetry, electron probe microanalysis, in-situ X-ray diffractometry, high resolution transmission electron microscopy and instrumented microhardness. The metallic glass possesses a high glass forming ability. It is thermally stable up to 585 °C while primary crystallization of Fe2B and FeB occurs at 677 °C. Estimated by the Kissinger and Moynihan’s methods, the activation energy of glass transition was shown to be lower than that of primary crystallization. After total crystallization, the bulk alloy contains a terminal Fe solid solution, Fe2B, FeB, Fe3B8Nb7 and BFe14Y2 phases while the ribbon contains additional yttria as well. The loading and unloading curves as well as the indentation features are very suitable in order to evidence the effect of the various crystallization events on the mechanical behavior of the bulk alloy. The hardness of the amorphous and fully crystallized bulk alloys amount to 1198 ± 21 and 461 ± 65 HV0.5, respectively and their reduced Young modulus are close to 174 ± 5 GPa. The deformation ability of the fully crystallized alloy is twice that of the glassy alloy.
Published: 2021

45. Microencapsulation of benzalkonium chloride enhanced its antibacterial and antibiofilm activity against Listeria monocytogenes and Escherichia coli

Author: Nour-Eddine Chihib, Alexandre Fadel, Fouzia Jbilou, charafeddine Jama, Alexandre Barras, Adem Gharsallaoui, Simon Khelissa, Université de Lille, CNRS, INRA, ENSCL, Unité Matériaux et Transformations - UMR 8207 [UMET], Laboratoire d’Océanologie et de Géosciences (LOG) - UMR 8187 [LOG], Institut d’Électronique, de Microélectronique et de Nanotechnologie - UMR 8520 [IEMN], Unité Matériaux et Transformations - UMR 8207 (UMET), Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), Laboratoire d'automatique, de génie des procédés et de génie pharmaceutique (LAGEPP), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-École Supérieure Chimie Physique Électronique de Lyon-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), Institut d’Électronique, de Microélectronique et de Nanotechnologie - UMR 8520 (IEMN), Centrale Lille-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Université Polytechnique Hauts-de-France (UPHF)-JUNIA (JUNIA), NanoBioInterfaces - IEMN (NBI - IEMN), Centrale Lille-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Université Polytechnique Hauts-de-France (UPHF)-JUNIA (JUNIA)-Centrale Lille-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Université Polytechnique Hauts-de-France (UPHF)-JUNIA (JUNIA), Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Université de Lyon-Université de Lyon-École Supérieure de Chimie Physique Électronique de Lyon (CPE)-Centre National de la Recherche Scientifique (CNRS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Université catholique de Lille (UCL)-Université catholique de Lille (UCL), and Université catholique de Lille (UCL)-Université catholique de Lille (UCL)-Centrale Lille-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Université Polytechnique Hauts-de-France (UPHF)-JUNIA (JUNIA)
Subjects: food.ingredient, Pectin, medicine.disease_cause, antibiofilm activity, benzalkonium chloride, Escherichia coli, Listeria monocytogenes, microencapsulation, Applied Microbiology and Biotechnology, 03 medical and health sciences, Benzalkonium chloride, food, Anti-Infective Agents, medicine, Food microbiology, Food science, Cytotoxicity, 030304 developmental biology, 0303 health sciences, 030306 microbiology, Chemistry, Biofilm, food and beverages, General Medicine, [SDV.MP.BAC]Life Sciences [q-bio]/Microbiology and Parasitology/Bacteriology, Anti-Bacterial Agents, [SDV.SP.PG]Life Sciences [q-bio]/Pharmaceutical sciences/Galenic pharmacology, Biofilms, Food Microbiology, Antibacterial activity, Benzalkonium Compounds, Biotechnology, medicine.drug
Abstract: International audience; Aims: In this study, benzalkonium chloride (BAC) microcapsules were developed for surface disinfection purpose and were evaluated against Listeria monocytogenes and Escherichia coli biofilms.Methods and Results: Microcapsules were prepared with two different strategies: uncomplexed BAC‐microcapsules (UBM), containing BAC and maltodextrins and complexed BAC‐microcapsules (CBM) containing BAC complexed by pectin and maltodextrins. The minimum inhibitory concentrations (MICs) of free and microencapsulated BAC was investigated against two food pathogens: L. monocytogenes and E. coli. The antibiofilm activities of UBM and CBM against L. monocytogenes and E. coli biofilms formed on stainless steel at 37°C were evaluated and compared to BAC used under its free form. MICs of encapsulated BAC were up to 4‐fold lower than those of free BAC. The UBM and CBM showed higher antibiofilm effect when compared to the free BAC.Conclusions: Overall, results demonstrated that microencapsulation enhanced the antibacterial activity of BAC against L. monocytogenes and E. coli biofilms.Significance and Impact of the Study: The application of such BAC microcapsule‐based delivery systems can improve surface disinfection procedures and reduce the required BAC concentrations and the related cytotoxicity of this antimicrobial compound.
Published: 2021

46. Novel procedure for studying laser-surface material interactions during scanning laser ablation cleaning processes on Cu-based alloys

Author: Víctor J. Rico, Ruth Lahoz, Delphine Neff, Emma Angelini, Sabrina Grassini, Elisabetta Di Francia, Nicolas Nuns, Politecnico di Torino = Polytechnic of Turin (Polito), Instituto de Nanociencia y Materiales de Aragón (INMA), Consejo Superior de Investigaciones Científicas [Madrid] (CSIC)-Universidad de Zaragossa, Laboratoire Archéomatériaux et Prévision de l'Altération (LAPA - UMR 3685), Nanosciences et Innovation pour les Matériaux, la Biomédecine et l'Energie (ex SIS2M) (NIMBE UMR 3685), Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), IRAMAT - Laboratoire Archéomatériaux et Prévision de l'Altération (IRAMAT-LAPA), Institut de Recherche sur les Archéomatériaux (IRAMAT), Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS), Instituto de Ciencia de Materiales de Sevilla (ICMSE), Universidad de Sevilla / University of Sevilla-Consejo Superior de Investigaciones Científicas [Madrid] (CSIC), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), European Federation of Corrosion (EFC) – EUROCORR Young Scientist Grant Selection Committee 2016, the FEDER program through AEI-MICINN (PID2019-110430GB-C21) and Junta de Andalucía (PAIDI-2020 through project P18-RT-3480, Consejo Superior de Investigaciones Científicas (España), Agencia Estatal de Investigación (España), Ministerio de Ciencia, Innovación y Universidades (España), and Junta de Andalucía
Subjects: Controlled atmosphere, Materials science, General Physics and Astronomy, chemistry.chemical_element, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Oxygen, Corrosion, law.invention, Copper alloys, law, Spectroscopy, Laser ablation, Surfaces and Interfaces, General Chemistry, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Laser, 0104 chemical sciences, Surfaces, Coatings and Films, Surface interaction mechanisms, ToF-SIMS, Chemical engineering, chemistry, 0210 nano-technology, Selectivity, Layer (electronics)
Abstract: Laser ablation is an effective method to clean Cu-based alloys. A novel procedure of characterisation was developed involving O isotopes evaluated by ToF-SIMS spectroscopy to assess the driving mechanisms of laser-surface interactions. The presence of re-oxidised compounds was detected, discerning between the oxygen from the corrosion layer and the one introduced by the interaction with the laser (that was generated in a controlled atmosphere of O diluted in N). A set of samples treated with different laser conditions were characterised by FESEM and μRaman. The results have shown that re-oxidation phenomenon can occur and its selectivity depends on the laser conditions., Dr. R. Lahoz wishes to acknowledge professional support of the CSIC Interdisciplinary Thematic Platform “Open Heritage: Research and Society (PTI-PAIS)”. Dr. E. Di Francia would like to acknowledge the European Federation of Corrosion (EFC) – EUROCORR Young Scientist Grant Selection Committee 2016 that stimulated the initial collaboration that subsequently produced this research. Dr. V. Rico thanks the FEDER program through AEI-MICINN (PID2019-110430GB-C21) and Junta de Andalucía (PAIDI-2020 through project P18-RT-3480) for financial support.
Published: 2021

47. EPR imaging of sinapyl alcohol and its application to the study of plant cell wall lignification

Author: Hervé Vezin, Hania Ahouari, Cédric Lion, Christophe Biot, Clémence Simon, Simon Hawkins, Unité de Glycobiologie Structurale et Fonctionnelle (UGSF), Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Laboratoire Avancé de Spectroscopie pour les Intéractions la Réactivité et l'Environnement - UMR 8516 (LASIRE), Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Centrale Lille Institut (CLIL), Unité de Glycobiologie Structurale et Fonctionnelle UMR 8576 (UGSF), Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Université de Lille, CNRS, Unité de Glycobiologie Structurale et Fonctionnelle UMR 8576 [UGSF], Laboratoire Avancé de Spectroscopie pour les Intéractions la Réactivité et l'Environnement - UMR 8516 [LASIRE], Institut National de la Recherche Agronomique (INRA)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), and Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Centrale Lille Institut (CLIL)
Subjects: 010402 general chemistry, 01 natural sciences, Catalysis, law.invention, Cell wall, Cyclic N-Oxides, chemistry.chemical_compound, law, Cell Wall, Flax, Materials Chemistry, Electron paramagnetic resonance, Molecular Structure, Phenylpropionates, 010405 organic chemistry, fungi, Metals and Alloys, Electron Spin Resonance Spectroscopy, food and beverages, General Chemistry, Fluorescence, 0104 chemical sciences, Surfaces, Coatings and Films, Electronic, Optical and Magnetic Materials, [SDV.BBM.BC]Life Sciences [q-bio]/Biochemistry, Molecular Biology/Biomolecules [q-bio.BM], chemistry, Sinapyl alcohol, Ceramics and Composites, Biophysics, Monolignol, [PHYS.PHYS.PHYS-CHEM-PH]Physics [physics]/Physics [physics]/Chemical Physics [physics.chem-ph], Bioorthogonal chemistry
Abstract: International audience; In bioimaging, bioorthogonal chemistry is most often used to visualize chemical reporters by fluorescence in their native environment. Herein, we show that TEMPO-based probes can be ligated to monolignol reporters by Diels–Alder chemistry in plant cell walls, paving the way for the study of lignification by EPR spectroscopy and imaging.
Published: 2021

48. STEM-EELS Investigation of Planar Defects in Olivine in the Allende Meteorite

Author: Marinova, Maya, Leroux, Hugues, Cuvillier, Priscille, Gloter, Alexandre, Jacob, Damien, Unité Matériaux et Transformations - UMR 8207 (UMET), Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), Laboratoire de Physique des Solides (LPS), Centre National de la Recherche Scientifique (CNRS)-Université Paris-Sud - Paris 11 (UP11), Université de Lille, CNRS, INRA, ENSCL, Institut Chevreul - FR2638, Unité Matériaux et Transformations - UMR 8207 [UMET], Unité Matériaux et Transformations (UMET) - UMR 8207, Laboratoire de Physique des Solides [LPS], Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), and Université Paris-Sud - Paris 11 (UP11)-Centre National de la Recherche Scientifique (CNRS)
Subjects: HAADF, lcsh:Mineralogy, lcsh:QE351-399.2, STEM-EELS, HAADF, olivine, Allende, planar defects, [SDU.ASTR]Sciences of the Universe [physics]/Astrophysics [astro-ph], [SDU.STU]Sciences of the Universe [physics]/Earth Sciences, [PHYS.PHYS.PHYS-GEO-PH]Physics [physics]/Physics [physics]/Geophysics [physics.geo-ph], [CHIM.MATE]Chemical Sciences/Material chemistry, STEM-EELS, Allende, [PHYS.COND.CM-MS]Physics [physics]/Condensed Matter [cond-mat]/Materials Science [cond-mat.mtrl-sci], planar defects, [PHYS.ASTR]Physics [physics]/Astrophysics [astro-ph], olivine
Abstract: The present study focuses on a detailed structural investigation at atomic scale of the planar defects that appear in the olivine grains in the Allende meteorite, and it aims to clarify their nature and the related formation mechanism. The investigation was performed using advanced spectro-microscopy techniques such as atomically resolved high-angle annular dark field (HAADF) images coupled with electron energy loss spectroscopy in the scanning transmission electron microscopy mode (STEM-EELS). Two prominent structural features appear in the investigated olivine grains: (i) Exsolution platelets with a thickness between 2 and 10 nm with the spinel structure and chemical composition expressed as a solid solution between magnetite, chromite, and MgAl2O4. (ii) Thinner planar defects appeared with thickness between 2 to 4 atomic planes, which were rich in Fe and had a strong Fe3+ contribution. The structure of these defects was described by the crystalline lattice of the olivine grains with small distortion of the measured cationic distances, which can be related to Fe3+-Si substitution in the tetrahedral sites. Those metastable defects should have preceded the formation of the thicker spinel exsolutions and could have formed during an oxidizing event in the Allende parent body.
Published: 2021

49. Indirect NMR detection via proton of nuclei subject to large anisotropic interactions, such as 14N, 195Pt, and 35Cl, using the T-HMQC sequence

Author: Racha Bayzou, Julien Trébosc, Ivan Hung, Zhehong Gan, Olivier Lafon, Jean-Paul Amoureux, Université de Lille, CNRS, Centrale Lille, ENSCL, Univ. Artois, Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS], Université de Lille, Sciences et Technologies, National High Magnetic Field Laboratory [NHMFL], Unité de Catalyse et Chimie du Solide (UCCS) - UMR 8181, Bruker, Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), National High Magnetic Field Laboratory (NHMFL), Florida State University [Tallahassee] (FSU), and ANR-18-CE08-0015,ThinGlass,Amélioration raisonnée de la conductivité des films minces de LiPON en élucidant leur structure à l'échelle atomique(2018)
Subjects: [CHIM.THEO]Chemical Sciences/Theoretical and/or physical chemistry, General Physics and Astronomy, Physical and Theoretical Chemistry
Abstract: International audience; Recently, the T-hetero-nuclear multiple quantum coherence (T-HMQC) sequence using the TRAPDOR (transfer of population in double resonance) recoupling has been introduced for the indirect detection via protons of quadrupolar nuclei with spin I = 1 (14N) or 3/2 (35Cl) in solids at fast magic-angle spinning (MAS). The sequence is simple as it only uses four rectangular pulses and exhibits low t1-noise because the recoupling pulses are applied to the indirectly detected isotope, I. We demonstrate that this sequence is applicable for the detection via protons of spin-1/2 nuclei subject to large chemical shift anisotropy, such as 195Pt. We also report the proton detection of double-quantum (2Q) coherences of 14N nuclei using this sequence. This 2Q version is more robust to the adjustment of the magic angle and the instabilities of the MAS frequencies than its parent single-quantum (1Q) version since the 2Q coherences are not broadened by the first-order quadrupole interaction. In practice, than its 1Q counterpart for the indirect detection of 14N nuclei, the 2Q variant benefits from a slightly higher resolution and comparable sensitivity. In this article, we derive for the first time the Hamiltonian that describes the spin dynamics during the TRAPDOR recoupling. This Hamiltonian demonstrates the importance of the adiabaticity parameter as well as the role of third-order terms in the effective Hamiltonian. The effects of offsets, radio-frequency field, and recoupling time on the efficiency of the T-HMQC sequence are analyzed numerically as well as with experimental detection via protons of 195Pt nuclei in a mixture of cis- and trans-platin and that of 14N and 35Cl isotopes in l-histidine HCl.
Published: 2022

50. Phyllosilicate‐derived Nickel‐cobalt Bimetallic Nanoparticles for the Catalytic Hydrogenation of Imines, Oximes and N‐heteroarenes

Author: Carmen Ciotonea, Maya Marinova, Jérémy Dhainaut, Adrian Ungureanu, Christophe Michon, Nisrine Hammi, Sébastien Royer, Abdelkrim El Kadib, Université de Lille, CNRS, Centrale Lille, ENSCL, Univ. Artois, Unité de Catalyse et Chimie du Solide - UMR 8181 [UCCS], 'Gheorghe Asachi' Technical University of Iasi [TUIASI], Institut Michel Eugène Chevreul - FR 2638 (IMEC), Université d'Artois (UA)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), Euromed Research Center. Engineering Division [Fès], Université Euro Méditerranéenne de Fès (UEMF), Unité de Catalyse et Chimie du Solide - UMR 8181 (UCCS), Centrale Lille Institut (CLIL)-Université d'Artois (UA)-Centrale Lille-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Lille, 'Gheorghe Asachi' Technical University of Iasi (TUIASI), Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier (ICGM ICMMM), Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Centre National de la Recherche Scientifique (CNRS)-Université de Montpellier (UM)-Université Montpellier 1 (UM1)-Université Montpellier 2 - Sciences et Techniques (UM2)-Institut de Chimie du CNRS (INC), Laboratoire d'innovation moléculaire et applications (LIMA), Université de Strasbourg (UNISTRA)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Université d'Artois (UA)-Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier (ICGM), and Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Institut de Chimie du CNRS (INC)-Université de Montpellier (UM)-Centre National de la Recherche Scientifique (CNRS)
Subjects: Nanoparticle, chemistry.chemical_element, 010402 general chemistry, 01 natural sciences, Catalysis, Inorganic Chemistry, Nickel, bimetallic nanoparticle, phyllosilicates, Physical and Theoretical Chemistry, Bimetallic strip, 010405 organic chemistry, [CHIM.ORGA]Chemical Sciences/Organic chemistry, Organic Chemistry, Substrate (chemistry), Cobalt, [CHIM.CATA]Chemical Sciences/Catalysis, [CHIM.MATE]Chemical Sciences/Material chemistry, 0104 chemical sciences, chemistry, hydrogenation, Mesoporous material, Selectivity, Chimie/Catalyse, Nuclear chemistry
Abstract: International audience; The development of cost-effective, noble metal-free catalytic systems for the hydrogenation of unsaturated aliphatic, aromatic, and heterocyclic compounds is fundamental for future valorisation of general feedstock. With this aim, we report here the preparation of highly dispersed bimetallic Ni/Co nanoparticles (NPs), by a one-pot deposition-precipitation of Ni and Co phases onto mesoporous SBA-15 silica. By adjusting the chemical composition in the starting mixture, three supported catalysts with different Ni to Co weight ratios were obtained, which were further subjected to treatments under reducing conditions at high temperatures. Characterization of the resulting solids evidenced a homogenous distribution of Ni and Co elements forming the NPs, the best results being obtained for Ni/Co-2:2 samples, for which 50 wt.% Ni-50 wt.% Co NPs are found located on the surface of the residual phyllosilicate. Ni/Co-2:2, presenting the best performances for the hydrogenation of 2-methyl-quinoline, was further evaluated in the catalytic hydrogenation of selected imines, oximes and N-heretoarenes. Due to the high dispersion of bimetallic Ni-Co NPs, excellent properties (activity and selectivity) in the conversion of the selected substrate are reported.
Published: 2020

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