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1. Self-organization and dewetting kinetics in sub-10 nm diblock copolymer line/space lithography

Author

Xavier Chevalier, Gwenaelle Pound-Lana, Cindy Gomes Correia, Sébastien Cavalaglio, Benjamin Cabannes-Boué, Frédéric Restagno, Guillaume Miquelard-Garnier, Sébastien Roland, Christophe Navarro, Guillaume Fleury, Marc Zelsmann, Arkema (Arkema), Laboratoire des technologies de la microélectronique (LTM ), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes (UGA), Laboratoire de Chimie des Polymères Organiques (LCPO), Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Team 4 LCPO : Polymer Materials for Electronic, Energy, Information and Communication Technologies, Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Commissariat à l'énergie atomique et aux énergies alternatives - Laboratoire d'Electronique et de Technologie de l'Information (CEA-LETI), Direction de Recherche Technologique (CEA) (DRT (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Laboratoire de Physique des Solides (LPS), Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS), Laboratoire Procédés et Ingénierie en Mécanique et Matériaux (PIMM), Conservatoire National des Arts et Métiers [CNAM] (CNAM), HESAM Université - Communauté d'universités et d'établissements Hautes écoles Sorbonne Arts et métiers université (HESAM)-HESAM Université - Communauté d'universités et d'établissements Hautes écoles Sorbonne Arts et métiers université (HESAM)-Centre National de la Recherche Scientifique (CNRS)-Arts et Métiers Sciences et Technologies, HESAM Université - Communauté d'universités et d'établissements Hautes écoles Sorbonne Arts et métiers université (HESAM), Groupement de recherches de Lacq (GRL), and This work was supported by the REX-7 project from Région Rhône Alpes and BPI France, by the French RENATECHnetwork, by the ANR LabEx Minos n°ANR-10-LABX-55–01and by the ANR project BONSAI n°ANR-21-CE09–0009

Subjects
wetting, Mechanical Engineering, Bioengineering, General Chemistry, block copolymers, [CHIM.POLY]Chemical Sciences/Polymers, kinetics, Mechanics of Materials, directed self-assembly, lithography, nanofabrication, thin film stability, General Materials Science, [PHYS.PHYS.PHYS-CHEM-PH]Physics [physics]/Physics [physics]/Chemical Physics [physics.chem-ph], [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, Electrical and Electronic Engineering
Abstract

In this work, we investigated the self-assembly of a lamellar block copolymer (BCP) under different wetting conditions. We explored the influence of the chemical composition of under-layers and top-coats on the thin film stability, self-assembly kinetics and BCP domain orientation. Three different chemistries were chosen for these surface affinity modifiers and their composition was tuned in order to provide either neutral wetting (i.e. an out-of-plane lamellar structure), or affine wetting conditions (i.e. an in-plane lamellar structure) with respect to a sub-10 nm PS-b-PDMSB lamellar system. Using such controlled wetting configurations, the competition between the dewetting of the BCP layer and the self-organization kinetics was explored. We also evaluated the spreading parameter of the BCP films with respect to the configurations of surface-energy modifiers and demonstrated that BCP layers are intrinsically unstable to dewetting in a neutral configuration. Finally, the dewetting mechanisms were evaluated with respect to the different wetting configurations and we clearly observed that the rigidity of the top-coat is a key factor to delay BCP film instability.

Published
2023

2. Effect of Uniaxial Fatigue Aging and Fabric Orientation on Low Impact Velocity Response of Glass Fibers/Elium Acrylic Composite Laminates

Author

Tomasz Libura, Rodrigue Matadi Boumbimba, Tadeusz Szymczak, Alexis Rusinek, Pierre Gerard, Zbigniew L. Kowalewski, Laboratoire d'Etude des Microstructures et de Mécanique des Matériaux (LEM3), Centre National de la Recherche Scientifique (CNRS)-Université de Lorraine (UL)-Arts et Métiers Sciences et Technologies, HESAM Université (HESAM)-HESAM Université (HESAM), Institute of Fundamental Technological Research PASPawi'nskiego 5B02 106 WarsawPoland, Motor Transport Institute, parent, Groupement de recherches de Lacq (GRL), Arkema (Arkema), and Université de Lorraine (UL)-Centre National de la Recherche Scientifique (CNRS)-Arts et Métiers Sciences et Technologies

Subjects
Cyclic stress, Technology, Thermoplastic, Materials science, low impact velocity, Composite number, Glass fiber, Thermosetting polymer, 02 engineering and technology, 01 natural sciences, Article, Woven fabric, 0103 physical sciences, fatigue aging, General Materials Science, Composite material, Acrylic resin, Elium acrylic, 010302 applied physics, chemistry.chemical_classification, Microscopy, QC120-168.85, QH201-278.5, composite laminates, Composite laminates, [SPI.MECA]Engineering Sciences [physics]/Mechanics [physics.med-ph], 021001 nanoscience & nanotechnology, Engineering (General). Civil engineering (General), TK1-9971, chemistry, Descriptive and experimental mechanics, visual_art, visual_art.visual_art_medium, Electrical engineering. Electronics. Nuclear engineering, TA1-2040, 0210 nano-technology, damage, glass fibers
Abstract

International audience; Impact resistance is one of the most critical features of composite structures, and therefore, its examination for a new material has a fundamental importance. This paper is devoted to the characterization of the fully recyclable thermoplastic ELIUM acrylic resin reinforced by glass fabric woven, which belongs to a new category of materials requiring advanced testing before their application in responsible elements of engineering structures. Its high strength, low weight as well as low production cost give excellent opportunities for its wide application in the automotive industry as a replacement of the thermoset-based laminates. The study presents an experimental work concerning the effect of damage due to low and high cyclic fatigue aging of two groups of specimens, first with the woven fabric orientations of [0°/90°]4 and secondly with [45°/45°]4, on the low impact velocity properties. The impact resistance was measured in terms of load peak, absorbed energy, penetration threshold and damage analysis. The low velocity impact results indicate that the uniaxial cyclic loading (fatigue aging) of the material leads to the reduction of impact resistance, especially at the high impact energy levels. Scanning Electron Microscopy (SEM) and Computed Tomography (CT) scan observations reveal that the damage area grows with the increase of both strain amplitude and impact energy.

Published
2021

3. A mesoscale modelling approach of glass fibre/Elium acrylic woven laminates for low velocity impact simulation

Author

Yao Koutsawa, G. Kinvi-Dossou, Pierre Gerard, A. Nyoungue, R. Matadi Boumbimba, Frédéric Lachaud, Napo Bonfoh, Laboratoire d'Etude des Microstructures et de Mécanique des Matériaux (LEM3), Université de Lorraine (UL)-Centre National de la Recherche Scientifique (CNRS)-Arts et Métiers Sciences et Technologies, HESAM Université (HESAM)-HESAM Université (HESAM), Luxembourg Institute of Science and Technology (LIST), Institut Clément Ader (ICA), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-IMT École nationale supérieure des Mines d'Albi-Carmaux (IMT Mines Albi), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-Institut Supérieur de l'Aéronautique et de l'Espace (ISAE-SUPAERO), Laboratoire de Génie Informatique, de Production et de Maintenance (LGIPM), Université de Lorraine (UL), Groupement de recherches de Lacq (GRL), Arkema (Arkema), HESAM Université - Communauté d'universités et d'établissements Hautes écoles Sorbonne Arts et métiers université (HESAM)-HESAM Université - Communauté d'universités et d'établissements Hautes écoles Sorbonne Arts et métiers université (HESAM), Institut Supérieur de l'Aéronautique et de l'Espace (ISAE-SUPAERO)-Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-IMT École nationale supérieure des Mines d'Albi-Carmaux (IMT Mines Albi), and Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)

Subjects
Materials science, Glass fiber, Mesoscale meteorology, 02 engineering and technology, Yarn, Composite laminates, [SPI.MECA]Engineering Sciences [physics]/Mechanics [physics.med-ph], 021001 nanoscience & nanotechnology, Microstructure, 020303 mechanical engineering & transports, 0203 mechanical engineering, Robustness (computer science), visual_art, Impact loading, Ceramics and Composites, visual_art.visual_art_medium, Laminated composites, Composite material, 0210 nano-technology, ComputingMilieux_MISCELLANEOUS, Civil and Structural Engineering
Abstract

International audience; This study presents a numerical mesoscale approach to simulate the damage and failure mechanisms of woven laminated composites under low velocity impact loading conditions. First, some measurements were made on samples to obtain a realistic reproduction of the microstructure. This allows relating failure mechanisms in composite laminates with their geometry and topology. A three-dimensional Hashin criterion was developed to investigate the impact behaviour, by accounting for both intralaminar and interlaminar damages. Four failure modes were considered relatively to fibre damage initiation in tension and compression and Puck criteria was employed to capture the initiation of the yarn’s matrix damage. The matrix surrounding undulated yarns were taken into account by an elastoplastic behaviour with maximum-stress failure criteria. Good correlation between numerical and experimental results demonstrated the robustness and the accuracy of the proposed multiscale approach.

Published
2020

4. Tridodecylamine, an efficient charge control agent in non-polar media for electrophoretic inks application

Author

Christophe Navarro, Guillaume Fleury, CyrilBrochon, Eric Cloutet, Georges Hadziioannou, Déborah Mirbel, Christophe Schatz, Amélie Noël, Laboratoire de Chimie des Polymères Organiques (LCPO), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Team 4 LCPO : Polymer Materials for Electronic, Energy, Information and Communication Technologies, Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Groupement de recherches de Lacq (GRL), and Arkema (Arkema)

Subjects
Analytical chemistry, General Physics and Astronomy, 02 engineering and technology, 010402 general chemistry, Charge control agent, 01 natural sciences, Pigment, Charge control, Inorganic pigments, Non-polar solvent, Range (particle radiation), Mineral oxides, Chemistry, Surfaces and Interfaces, General Chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Surface charging, 0104 chemical sciences, Surfaces, Coatings and Films, Solvent, Electrophoresis, [CHIM.POLY]Chemical Sciences/Polymers, Isoelectric point, Chemical engineering, visual_art, visual_art.visual_art_medium, Non polar, 0210 nano-technology, Electrophoretic ink
Abstract

International audience; In order to obtain efficient electrophoretic inks, Tridodecylamine (Dod3N), has been studied as charge controlagent (CCA) in a non-polar paraffin solvent (Isopar G) for various inorganic pigments (TiO2 and Fe2O3).All hydrophobic mineral oxides, i.e. treated with octyltrimethoxysilane (C8) or dodecyltrimethoxysilane(C12), were found to be negatively charged in presence of Dod3N. The electrophoretic mobilities ofinorganic pigments seemed to be strongly dependent of their isoelectric point (IEP) and also of the concentrationof dod3N with an optimum range between 10 and 20 mM depending on the pigments. Finally,an electrophoretic ink constituted of hydrophobic mineral oxides in presence of Dod3N was tested in adevice. Its efficiency as charge control agent to negatively charge hydrophobic particles was confirmedthrough good optical properties and fast response time (220 ms at 200 kV m−1).

Published
2018

5. Observations by in-situ X-ray synchrotron computed tomography of the microstructural evolution of semi-crystalline Polyamide 11 during deformation

Author

Lucien Laiarinandrasana, Gilles Hochstetter, Pierre-Alexis Poulet, Andrew King, Sébastien Joannès, Henry Proudhon, Centre des Matériaux (MAT), MINES ParisTech - École nationale supérieure des mines de Paris, Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Centre National de la Recherche Scientifique (CNRS), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Synchrotron SOLEIL (SSOLEIL), and Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Polymers and Plastics, Semi-crystalline polymers, In-situ SRCT tensile testing, 02 engineering and technology, Deformation (meteorology), 010402 general chemistry, 01 natural sciences, [SPI.MAT]Engineering Sciences [physics]/Materials, law.invention, Stress (mechanics), [SPI]Engineering Sciences [physics], law, Phase (matter), [SPI.MECA.MEMA]Engineering Sciences [physics]/Mechanics [physics.med-ph]/Mechanics of materials [physics.class-ph], Ultimate tensile strength, Composite material, Void morphology, ComputingMilieux_MISCELLANEOUS, Cavitation, Organic Chemistry, 021001 nanoscience & nanotechnology, Synchrotron, 0104 chemical sciences, Polyamide, Elongation, 0210 nano-technology, Polyamide 11, X-ray Synchrotron Radiation Computed Tomography
Abstract

International audience; This study deals with the cavitation of semi-crystalline Polyamide 11 during deformation. The link between the microstructural evolution and the material macroscopic behaviour is demonstrated thanks to tensile tests on small notched round bars using in-situ X-ray synchrotron computed tomography (SRCT). 3D rendering, image processing and both qualitative and quantitative data analyses are at the heart of this work so as to provide a comprehensive description of micro-mechanisms occurring in the material throughout the tensile tests. Whitening appeared whilst only few microvoids were observed via the tomographic scans in the central part of the specimen where the stress triaxiality is the highest. Significant stages – chronologically, denotching, renotching and a final denotching phase, resulting in the elongation of the central part of the specimen – are detailed. Corresponding evolution of the morphologies (in terms of growth and prolate and oblate shapes) of the void cloud, as well as of the individualized voids within the latter, are discussed.

Published
2016

6. Vibrating Magnetic Particles for Cancer Cells Destruction

Author

Morel, R., Caroline Thébault, Cécile Naud, Hélène Joisten, Selma Leulmi, Cécile Iss, Mélissa Morcrette, Guillaume Ortiz, Yanxia Hou, Thierry Livache, Roberto Calemczuk, Marie Carrière, Philippe Sabon, Isabelle JOUMARD, Stéphane Auffret, Bernard Dieny, SPINtronique et TEchnologie des Composants (SPINTEC), Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Direction de Recherche Fondamentale (CEA) (DRF (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Chimie pour la Reconnaissance et l’Etude d’Assemblages Biologiques (CREAB), SYstèmes Moléculaires et nanoMatériaux pour l’Energie et la Santé (SYMMES), Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Structures et propriétés d'architectures moléculaire (SPRAM - UMR 5819), Institut Nanosciences et Cryogénie (INAC), Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Chimie Interface Biologie pour l’Environnement, la Santé et la Toxicologie (CIBEST ), HOU-BROUTIN, Yanxia, Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Recherche Interdisciplinaire de Grenoble (IRIG), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
[PHYS]Physics [physics], ComputingMilieux_MISCELLANEOUS, [PHYS] Physics [physics]
Abstract

International audience

Published
2018

7. Sub-10 nm Features Obtained from Directed Self-Assembly of Semicrystalline Polycarbosilane-Based Block Copolymer Thin Films

Author

Georges Hadziioannou, Christophe Navarro, Guillaume Fleury, Muhammad Waseem Mumtaz, Giuseppe Portale, Cyril Brochon, Eric Cloutet, Caroline A. Ross, Karim Aissou, Laboratoire de Chimie des Polymères Organiques (LCPO), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Team 4 LCPO : Polymer Materials for Electronic, Energy, Information and Communication Technologies, Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), NWO DUBBLE CRG (ESRF, Netherlands Org Sci Res), European Synchrotron Radiation Facility (ESRF), Groupement de recherches de Lacq (GRL), Arkema (Arkema), MIT, Dept Mat Sci & Engn, Massachusetts Institute of Technology (MIT), and Macromolecular Chemistry & New Polymeric Materials

Subjects
chemistry.chemical_classification, Materials science, Mechanical Engineering, Polymer, DIBLOCK COPOLYMER, LITHOGRAPHY, law.invention, ARRAYS, RING-OPENING POLYMERIZATION, Crystallinity, chemistry.chemical_compound, Anionic addition polymerization, [CHIM.POLY]Chemical Sciences/Polymers, chemistry, Chemical engineering, Mechanics of Materials, law, Polymer chemistry, Copolymer, General Materials Science, TEMPLATES, Crystallization, Methyl methacrylate, Thin film, Lithography
Abstract

International audience; Highly-ordered arrays with sub-10 nm features are produced with topographical-directed self-assembly of low-molecular-weight poly(1,1-dimethyl silacyclobutane)block-poly(methyl methacrylate). This system turns out to be of high interest for lithographic applications since the domain orientation is solely controlled through the polymer layer thickness, while the promotion of the microphase separation is obtained by a short thermal annealing process under mild conditions.

Published
2015

8. Balancing Block Copolymer Thickness over Template Density in Graphoepitaxy Approach

Author

Laurent Pain, Raluca Tiron, Ahmed Gharbi, Jerome Hazart, Ian Cayrefourcq, Sandra Bos, F. Delachat, Antoine Fouquet, Xavier Chevalier, Patricia Pimenta Barros, Commissariat à l'énergie atomique et aux énergies alternatives - Laboratoire d'Electronique et de Technologie de l'Information (CEA-LETI), Direction de Recherche Technologique (CEA) (DRT (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Groupement de recherches de Lacq (GRL), Arkema (Arkema), and European Project: 688072,H2020,H2020-ICT-2015,IONS4SET(2016)

Subjects
010302 applied physics, Directed self assembly, Materials science, Polymers and Plastics, Atomic force microscopy, General Chemical Engineering, Density reduction, Organic Chemistry, Nanotechnology, block copolymer, 02 engineering and technology, 021001 nanoscience & nanotechnology, 01 natural sciences, pattern density, Template, Chemical-mechanical planarization, 0103 physical sciences, Materials Chemistry, Copolymer, planarization, [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, 0210 nano-technology, Directed Self-Assembly (DSA), graphoepitaxy
Abstract

International audience; Directed Self-Assembly (DSA) of Block Copolymers (BCP) is one of the most promising patterning solutions for sub-10 nm nodes. While significant achievements have been demonstrated in pattern fidelity for various applications (contact shrink, line patterning), some challenges still need to be overcome especially regarding the defect density reduction, in order to ensure DSA insertion in high-volume manufacturing. In particular, in the case of the graphoepitaxy approach, a remaining challenge is to solve the pattern-densities-related defect issue due to BCP film thickness variation inside the guiding template. In order to address this issue, a new DSA process flow called "DSA planarization" is employed for contact-hole patterning, and consists in overfilling the guiding pattern cavities with a thick BCP film, followed by a plasma etch-back step. This new approach ensures a uniform control of the final thickness of the BCP inside guiding cavities of different densities, as demonstrated herein by AFM measurement. Thus, defect-free isolated and dense patterns for both contact shrink and multiplication is simultaneously resolved. Furthermore, the simulation results of BCP self-assembly overfilling the templates demonstrate 2 that BCP domains are well directed in vertical cylinders ordering inside guiding cavities, which confirms the experimental results and the viability of this approach.

Published
2017

9. Un procédé catalytique pour une production industrielle de nanotubes de carbone. Genèse et perspectives d’évolution vers le graphène

Author

Beausoleil, Julien, Caussat, Brigitte, Delprat, Patrick, Haunold, Christophe, Serp, Philippe, Groupement de recherches de Lacq (GRL), Arkema (Arkema), Laboratoire de génie chimique [ancien site de Basso-Cambo] (LGC), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées, Institut National Polytechnique (Toulouse) (Toulouse INP), Laboratoire de chimie de coordination (LCC), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Génie Chimique (LGC), Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), Arkema (FRANCE), Centre National de la Recherche Scientifique - CNRS (FRANCE), Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Laboratoire de Génie Chimique - LGC (Toulouse, France), and Laboratoire de Chimie de Coordination - LCC (Toulouse, France)

Subjects
Nanotubes de carbone, [CHIM.GENI]Chemical Sciences/Chemical engineering, Graphène, Génie chimique, Nanomatériaux, [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, [CHIM.COOR]Chemical Sciences/Coordination chemistry, Catalyse, Génie des procédés, Lit fluidisé
Abstract

International audience; Des spécialistes de catalyse, de matériaux et du génie chimique de l’Institut National Polytechnique de Toulouse (Université de Toulouse) ont mis au point un procédé catalytique de production de nanotubes de carbone. Une collaboration nouée avec la société Arkema a alors permis de développer rapidement le procédé et de le faire évoluer pour le rendre facilement extrapolable à l’échelle industrielle. Courant 2011, il a été transposé avec succès par Arkema sur une unité industrielle particulièrement sécurisée qui permet une capacité de production de 400 t/an. Enfin, il a été récemment démontré que la grande flexibilité de ce procédé permet également d’envisager la synthèse catalytique de poudre de graphène à faible nombre de feuillets. Cette collaboration exemplaire entre une entreprise d’envergure internationale et des laboratoires académiques démontre que l’innovation, le développement économique et la compétitivité industrielle peuvent clairement bénéficier de la recherche publique et des apports de la science.

Published
2017

10. Straightforward integration flow of a silicon containing block copolymer for line-space patterning

Author

Legrain, A., Fleury, G., Mumtaz, M., Navarro, C., Arias-Zapata, J., Chevalier, X., Cayrefourcq, I., Zelsmann, M., Laboratoire des technologies de la microélectronique (LTM ), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Laboratoire de Chimie des polymères organiques (LCPO), Université Sciences et Technologies - Bordeaux 1 (UB)-École Nationale Supérieure de Chimie et de Physique de Bordeaux (ENSCPB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Chimie des Polymères Organiques (LCPO), Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Clot, Marielle, Centre National de la Recherche Scientifique (CNRS)-École Nationale Supérieure de Chimie et de Physique de Bordeaux (ENSCPB)-Université Sciences et Technologies - Bordeaux 1-Institut de Chimie du CNRS (INC), and Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC)

Subjects
[PHYS]Physics [physics], ComputingMilieux_MISCELLANEOUS, [PHYS] Physics [physics]
Abstract

International audience

Published
2017

11. Recent Achievements in sub-10 nm DSA lithography for Line/Space patterning

Author

Mary Ann Hockey, Guillaume Fleury, Laura Evangelio, Raluca Tiron, Ahmed Gharbi, Muhammad Waseem Mumtaz, Kui Xu, Christophe Navarro, Ian Cayrefourcq, Georges Hadziioannou, Fumi Ariura, Marc Zelsmann, Xavier Chevalier, Antoine Legrain, Marta Fernández-Regúlez, Francesc Pérez-Murano, Celia Nicolet, Laurent Pain, Groupement de recherches de Lacq (GRL), Arkema (Arkema), Arkema (ARKEMA), BREWER Sci Inc, Rolla, MO 65401 USA, BREWER Sci Inc, Laboratoire de Chimie des Polymères Organiques (LCPO), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Laboratoire des technologies de la microélectronique (LTM ), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Commissariat à l'énergie atomique et aux énergies alternatives - Laboratoire d'Electronique et de Technologie de l'Information (CEA-LETI), Direction de Recherche Technologique (CEA) (DRT (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Instituto de Microelectrònica de Barcelona (IMB-CNM), Centro Nacional de Microelectronica [Spain] (CNM)-Consejo Superior de Investigaciones Científicas [Madrid] (CSIC), Arkema, Colombes, European Project: 621277,EC:FP7:SP1-JTI,ENIAC-2013-2,PLACYD(2014), Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Clot, Marielle, ARKEMA FRANCE, Laboratoire de Chimie des polymères organiques (LCPO), Centre National de la Recherche Scientifique (CNRS)-École Nationale Supérieure de Chimie et de Physique de Bordeaux (ENSCPB)-Université Sciences et Technologies - Bordeaux 1-Institut de Chimie du CNRS (INC), SOITEC, and Université Sciences et Technologies - Bordeaux 1 (UB)-École Nationale Supérieure de Chimie et de Physique de Bordeaux (ENSCPB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Directed self assembly, [PHYS]Physics [physics], Materials science, Polymers and Plastics, Organic Chemistry, Nanotechnology, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, Space (mathematics), 01 natural sciences, [PHYS] Physics [physics], 0104 chemical sciences, Materials Chemistry, Multiple patterning, Line (text file), 0210 nano-technology, Lithography, ComputingMilieux_MISCELLANEOUS, Next-generation lithography
Abstract

International audience; Silicon-containing and modified PS-b-PMMA high-χ block copolymers materials were produced to achieve lamellar mesostructure as low as 14 nm intrinsic period (L$_0$) and ordered by graphoepitaxy or chemoepitaxy processes. Line Edge Roughness (LER) measurements of 2.5 nm (3 σ) can be extracted from CD-SEM pictures of poly [(1,1-dimethylsilacyclobutane)-b-styrene] after etching step. Materials integrations on a 300 mm track process are highlighted. In fingerprint, new BCPs LWR L/S values are 1.5/1.1 nm in comparison to a graphoepitaxy flow where the LWR L/S values are 2.0/1.1 nm. Alternative methods to create high-resolution guiding patterns for directed self-assembly of block co-polymers and the scale-up to obtain industrial BCPs meeting electronic requirement are also reported.

Published
2017

12. Flexural creep behaviour of long glass fibre reinforced polyamide 6.6 under thermal-oxidative environment

Author

E Lafranche, C Douchain, E Gamache, JP Ciolczyk, A Coulon, Patricia Krawczak, Département Technologie des Polymères et Composites & Ingénierie Mécanique (TPCIM), École des Mines de Douai (Mines Douai EMD), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-Ministère de l'Economie, des Finances et de l'Industrie, Institut Mines-Télécom [Paris] (IMT), Ecole nationale supérieure Mines-Télécom Lille Douai (IMT Lille Douai), HUTCHINSON, Hutchinson, Groupement de recherches de Lacq (GRL), and Arkema (Arkema)

Subjects
Thermal oxidation, Materials science, Flexural modulus, Mechanical Engineering, Glass fiber, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, [SPI]Engineering Sciences [physics], [CHIM.POLY]Chemical Sciences/Polymers, Flexural strength, Creep, Mechanics of Materials, Thermal, Polyamide, [SPI.MECA.MEMA]Engineering Sciences [physics]/Mechanics [physics.med-ph]/Mechanics of materials [physics.class-ph], Materials Chemistry, Ceramics and Composites, Injection moulding, Composite material, 0210 nano-technology, ComputingMilieux_MISCELLANEOUS
Abstract

This article aims to investigate the flexural creep behaviour as a function of temperature of long glass fibre polyamide 6.6 taking into account the thermal-oxidative degradation occurring during the test. The mould geometry has been chosen so as to reproduce some geometrical accidents (e.g. sharp frontal and tangential steps) occurring on industrial moulds. The nominal fibre content (10, 40 and 55 wt%), initial fibre length (short glass fibre, long glass fibre), load rate (up to 70%) and creep temperature (23℃, 100℃ and 130℃) have been considered to estimate the Findley’s model coefficients. A first investigation on the polyamide 6.6 degradation under thermo-oxidative environment has been led to understand the mechanisms of thermal-degradation of the polyamide 6.6 composites. The pure polyamide 6.6 matrix has shown a 20% increase of flexural modulus during the first period of ageing attributed to a combined chain scissions and cross-linking reactions. Then, a decrease of properties attributed to predominant chain scission mechanism was noticed after 1000 h of thermal exposure reaching up to 30% after 5000 h. In case of reinforced polyamide 6.6, the flexural properties tend to increase (+6.5%) up to 2000 h of exposure. The least square method has then permitted to evaluate the material coefficients from the experimental data; the instantaneous creep strain has been estimated from a power law representation. In any cases, the calculations are in a good accordance with experimental measurements.

Published
2016

13. Removal of poly(methyl methacrylate) in diblock copolymers films studied by grazing incidence small-angle X-ray scattering

Author

Ahmed Gharbi, Guillaume Freychet, Patrice Gergaud, Mireille Maret, Marta Fernández-Regúlez, Xavier Chevalier, Raluca Tiron, Commissariat à l'énergie atomique et aux énergies alternatives - Laboratoire d'Electronique et de Technologie de l'Information (CEA-LETI), Direction de Recherche Technologique (CEA) (DRT (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Science et Ingénierie des Matériaux et Procédés (SIMaP ), Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019]), Groupement de recherches de Lacq (GRL), and Arkema (Arkema)

Subjects
Materials science, Polymers and Plastics, Polymers, Scanning electron microscope, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, chemistry.chemical_compound, Engineering, copolymers, Materials Chemistry, Physical and Theoretical Chemistry, Methyl methacrylate, Nanoscopic scale, GISAXS, Small-angle X-ray scattering, self-assembly, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Poly(methyl methacrylate), 0104 chemical sciences, X-ray reflectivity, Crystallography, thin films, chemistry, Chemical engineering, visual_art, x-ray reflectivity, Chemical Sciences, visual_art.visual_art_medium, Grazing-incidence small-angle scattering, Self-assembly, 0210 nano-technology, scanning electron microscopy
Abstract

Self-assembly of diblock copolymers (BCP) into periodic arrays is a promising route to generate templates for the fabrication of nanoscopic elements, when one block is selectively removed. In cylindrical morphology polystyrene-block-poly(methyl methacrylate) (PS-b-PMMA) copolymer (BCP) films, the efficiency of different processes for removing the PMMA from cylinders is studied using grazing incidence small angle X-ray scattering (GISAXS), x-ray reflectivity and critical dimension scanning electron microscopy. The detailed analysis of the GISAXS patterns leads to the determination of the depth of cylindrical holes left by removal of the PMMA. It is found that the combination of a preliminary UV exposure followed by a wet treatment allows to remove totally the PMMA blocks. Furthermore, the optimization of both UV exposition time and solvent allows to preserve the PS matrix and interestingly for nanolithographic applications to decrease the process costs. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2016, 54, 1137–1144

Published
2016

14. Design of new block-copolymer systems to achieve thick-films with defect-free structures for applications of DSA into lithographic large nodes

Author

Guillaume Fleury, Ian Cayrefourcq, John Berron, Ahmed Gharbi, Celia Nicolet, Xavier Chevalier, Paul Coupillaud, Geoffrey Lombard, Julien Beausoleil, Raluca Tiron, Gilles Cunge, Philippe Bézard, Marc Zelsmann, Kaumba Sakavuyi, Christophe Navarro, Georges Hadziioannou, Groupement de recherches de Lacq (GRL), Arkema (Arkema), Laboratoire de Chimie des Polymères Organiques (LCPO), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Team 4 LCPO : Polymer Materials for Electronic, Energy, Information and Communication Technologies, Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), MINATEC, CNRS, LTM, Minatec Grenoble (CEA/ INP Grenoble), BREWER Sci Inc, Rolla, MO 65401 USA, BREWER Sci Inc, Commissariat à l'énergie atomique et aux énergies alternatives - Laboratoire d'Electronique et de Technologie de l'Information (CEA-LETI), Direction de Recherche Technologique (CEA) (DRT (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), ARKEMA FRANCE, Rue Estienne Orves, Colombes, Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire des technologies de la microélectronique (LTM ), and Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS)-Université Grenoble Alpes [2016-2019] (UGA [2016-2019])

Subjects
Directed self assembly, Early introduction, Materials science, Defect free, Nanotechnology, 02 engineering and technology, Orientation (graph theory), 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, [CHIM.POLY]Chemical Sciences/Polymers, Perpendicular, Copolymer, Tomography, ORIENTATION, 0210 nano-technology, Lithography
Abstract

Conference, San Jose CA, Feb 22-25, 2016. Sponsor(s) : SPIE; Tokyo Ohka Kogyo Co; International audience; Properties of new block copolymers systems, specifically designed to reach large periods for the features, are compared to the ones exhibited by classical PS-b-PMMA materials of same dimensions. Conducted studies, like free-surface defects analysis, mild-plasma tomography experiments, graphoepitaxy-guided structures, etch-transfer. indicate much better performances, in terms of achievable film-thicknesses with perpendicular features, defects levels, and dimensional uniformities, for the new system than for the classical PS-b-PMMA. These results clearly highlight unique and original solutions toward an early introduction of DSA technology into large lithographic nodes.

Published
2016

15. In situ mid-IR and UV–visible spectroscopies applied to the determination of kinetic parameters in the anionic copolymerization of styrene and isoprene

Author

Michel Fontanille, Christophe Navarro, Sébastien Quinebèche, Yves Gnanou, Laboratoire de Chimie des Polymères Organiques (LCPO), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Team 1 LCPO : Polymerization Catalyses & Engineering, and Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC)

Subjects
Polymers and Plastics, Organic Chemistry, Infrared spectroscopy, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, Photochemistry, Anionic copolymerization, 01 natural sciences, Ethylbenzene, 0104 chemical sciences, Styrene, chemistry.chemical_compound, [CHIM.POLY]Chemical Sciences/Polymers, Monomer, Reaction rate constant, chemistry, Polymerization, Kinetics of polymerization, Materials Chemistry, Copolymer, 0210 nano-technology, Isoprene, In situ infrared and UV-visible spectroscopies
Abstract

International audience; In situ MIR and UV-visible spectroscopies have been combined in a set-up that has been used to monitor anionic (co)polymerizations of styrene and isoprene. This experimental set-up gives access to the simultaneous and real time concentrations of monomers and actives species during the polymerization, through optical fibers probes immersed in the reaction medium. This method allows fast, accurate and reproducible measurements of the rate constants of the (co)polymerizations investigated even if it does not resort to high vacuum. The influence of some experimental factors has been examined using this method. Among the kinetic parameters governing the (co)polymerization of styrene and isoprene initiated by sec-butyllithium, the influence of the nature of solvent was investigated. It appears that the only reaction to depend on the nature of the aromatic solvent (k(ss,toluene) > k(ss,ethylbenzene)) is the propagation step of styrene.

Published
2009

16. Probing Self-Assembly of Cylindrical Morphology Block Copolymer Using in Situ and ex Situ Grazing Incidence Small-Angle X-ray Scattering: The Attractive Case of Graphoepitaxy

Author

G. Hadziioannou, Patrice Gergaud, Christophe Navarro, Raluca Tiron, Mireille Maret, Nathalie Boudet, Guillaume Fleury, Ahmed Gharbi, Vincent Jousseaume, Céline Lapeyre, Xavier Chevalier, Jonathan Pradelles, CNRS IPB, Lab Sci & Ingn Mat & Proc, Commissariat à l'énergie atomique et aux énergies alternatives - Laboratoire d'Electronique et de Technologie de l'Information (CEA-LETI), Direction de Recherche Technologique (CEA) (DRT (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Laboratoire de Chimie des Polymères Organiques (LCPO), Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Team 4 LCPO : Polymer Materials for Electronic, Energy, Information and Communication Technologies, Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), CRG & Grands instruments (NEEL - CRG), Institut Néel (NEEL), Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Centre National de la Recherche Scientifique (CNRS)-Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Centre National de la Recherche Scientifique (CNRS), Science et Ingénierie des Matériaux et Procédés [2007-2015] (SIMaP [2007-2015]), Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology [2007-2019] (Grenoble INP [2007-2019])-Institut National Polytechnique de Grenoble (INPG)-Centre National de la Recherche Scientifique (CNRS), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), CRG et Grands Instruments (CRG), and Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Centre National de la Recherche Scientifique (CNRS)-Université Joseph Fourier - Grenoble 1 (UJF)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Centre National de la Recherche Scientifique (CNRS)-Université Joseph Fourier - Grenoble 1 (UJF)

Subjects
Materials science, Polymers and Plastics, Annealing (metallurgy), 02 engineering and technology, 010402 general chemistry, 01 natural sciences, NANOSTRUCTURES, Inorganic Chemistry, chemistry.chemical_compound, THIN-FILMS, Materials Chemistry, Thin film, Composite material, Hydrogen silsesquioxane, ComputingMilieux_MISCELLANEOUS, GISAXS, MICRODOMAINS, chemistry.chemical_classification, Small-angle X-ray scattering, Scattering, Organic Chemistry, POLY(STYRENE-B-BUTADIENE), ORDER, [CHIM.MATE]Chemical Sciences/Material chemistry, Polymer, 021001 nanoscience & nanotechnology, LAMELLAE, 0104 chemical sciences, Crystallography, Nanolithography, [CHIM.POLY]Chemical Sciences/Polymers, chemistry, VAPOR, Grazing-incidence small-angle scattering, ORIENTATION, 0210 nano-technology, BEHAVIOR
Abstract

International audience; The self-assembly of polystyrene-block-poly(methyl methacrylate) (PS-b-PMMA) copolymer (BCP) films, leading to hexagonal arrays of perpendicular PMMA cylinders in a PS matrix, and its ordering kinetics were investigated using ex situ and in situ grazing incidence small-angle X-ray scattering (GISAXS). The ex situ measurements have provided accurate information about the structural changes in self-assembled BCP films with multiple processing parameters (PMMA removal process, film thickness, annealing treatment). Such structural information proves essential since BCP films are envisioned as template materials for density multiplication in nanolithography. Moreover, the temperature-dependent GISAXS measurements indicate that phase-separation starts around 140 degrees C and annealing up to 240 degrees C is required to form homogeneous self-assembled films within the short baking times required by industry. Furthermore, the guiding effect of an hydrogen silsesquioxane (HSQ) line grating commensurable with the polymer period on self-assembly (the so-called graphoepitaxy approach) was studied on silicon wafers presenting jointly patterned and unpatterned areas. When the line grating is aligned with the direction of the incident X-ray beam, the GISAXS pattern of the graphoepitaxial BCP film reveals the formation of a single domain extended over large areas. In contrast, the pattern of the BCP film self-assembled on the neighbor unpatterned area, comes from randomly oriented domains. Besides, the line grating does not only guide the BCP self-assembly, but as shown, also increases its ordering kinetics, demonstrating the high potentialities of graphoepitaxy.

Published
2014

17. Synthesis of Functional Polymer Particles by Dispersion Polymerization in Organic Media: A Tool Toward Stable Electrophoretic Inks

Author

Cyril Brochon, Georges Hadziioannou, Eric Cloutet, Antoine Charbonnier, Christophe Navarro, Laboratoire de Chimie des Polymères Organiques (LCPO), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Team 4 LCPO : Polymer Materials for Electronic, Energy, Information and Communication Technologies, Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Groupement de recherches de Lacq (GRL), and Arkema (Arkema)

Subjects
living radical polymerization (LRP), Polymers and Plastics, synthesis, Radical polymerization, 02 engineering and technology, 010402 general chemistry, Methacrylate, 01 natural sciences, electrophoretic ink, chemistry.chemical_compound, Polymer chemistry, dispersions, Materials Chemistry, macroinitiator, organic media, Acrylic acid, Dispersion polymerization, Acrylate, Organic Chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Electrophoresis, functional particle, Monomer, [CHIM.POLY]Chemical Sciences/Polymers, chemistry, Methacrylic acid, dispersion polymerization, 0210 nano-technology
Abstract

International audience; In this article, a simple route to obtain particles in one step from functional ionizable monomers in organic media by the use of acrylate-based macroinitiator synthesized by nitroxide-mediated radical polymerization is presented. Different positively ionizable monomers like 4-vinylpyridine, (dimethylamino)ethyl methacrylate, or negatively ionizable ones like methacrylic acid and acrylic acid were tested. Several parameters were studied to control the particles size, their stability in different organic media, and the possibility to crosslink them. Finally, well-defined, depending of conditions, functional latexes in organic media were produced in a simple way. This synthetic process constitutes the first step to produce electrophoretic inks for display applications such as electronic paper. (c) 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2013, 51, 4608-4617

Published
2013

18. Synergistic effect between few layer graphene and carbon nanotube supports for palladium catalyzing electrochemical oxidation of alcohols

Author

Philippe Serp, Bruno F. Machado, Julien Beausoleil, Werner Oberhauser, Marco Bellini, Revathi Bacsa, Francesco Vizza, Andrea Marchionni, Laboratoire de chimie de coordination (LCC), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie de Toulouse (ICT-FR 2599), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Department of Chemistry, Groupement de recherches de Lacq (GRL), and Arkema (Arkema)

Subjects
nanotube-graphene composites, Materials science, Inorganic chemistry, Energy Engineering and Power Technology, chemistry.chemical_element, electrooxidation, 02 engineering and technology, Carbon nanotube, fuel cells, 010402 general chemistry, Electrochemistry, 7. Clean energy, 01 natural sciences, law.invention, alcohols, chemistry.chemical_compound, law, [CHIM.COOR]Chemical Sciences/Coordination chemistry, Graphene, graphene, 021001 nanoscience & nanotechnology, Direct-ethanol fuel cell, palladium, 0104 chemical sciences, Fuel Technology, chemistry, Alcohol oxidation, Cyclic voltammetry, 0210 nano-technology, Ethylene glycol, Energy (miscellaneous), Nuclear chemistry, Palladium
Abstract

International audience; Few layer graphene (FLG), multi-walled carbon nanotubes (CNTs) and a nanotube-graphene composite (CNT-FLG) were used as supports for palladium nanoparticles. The catalysts, which were characterized by transmission electron microscopy, Raman spectroscopy and X-ray diffraction, were used as anodes in the electrooxidation of ethanol, ethylene glycol and glycerol in half cells and in passive direct ethanol fuelcells. Upon Pd deposition, a stronger interaction was found to occur between the metal and the nanotube-graphene composite and the particle size was significantly smaller in this material (6.3 nm), comparing with nanotubes and graphene alone (8 and 8.4 nm, respectively). Cyclic voltammetry experiments conducted with Pd/CNT, Pd/FLG and Pd/CNT-FLG in 10 wt% ethanol and 2 M KOH solution, showed high specific currents of 1.48, 2.29 and 2.51 mA·μg−1 Pd , respectively. Moreover, the results obtained for ethylene glycol and glycerol oxidation highlighted the excellent electrocatalytic activity of Pd/CNT-FLG in terms of peak current density (up to 3.70 mA·μg−1 Pd for ethylene glycol and 1.84 mA·μg−1 Pd for glycerol, respectively). Accordingly, Pd/CNT-FLG can be considered as the best performing one among the electrocatalysts ever reported for ethylene glycol oxidation, especially considering the low metal loading used in this work. Direct ethanol fuel cells at room temperature were studied by obtaining power density curves and undertaking galvanostatic experiments. The power density outputs using Pd/CNT, Pd/FLG and Pd/CNT-FLG were 12.1, 16.3 and 18.4 mW·cm−2, respectively. A remarkable activity for ethanol electrooxidation was shown by Pd/CNT-FLG anode catalyst. In a constant current experiment, the direct ethanol fuel cell containing Pd/CNT-FLG could continuously deliver 20 mA·cm−2 for 9.5 h during the conversion of ethanol into acetate of 30%, and the energy released from the cell was about 574 J.

Published
2013

19. Nanoscale Block Copolymer Ordering Induced by Visible Interferometric Micropatterning: A Route towards Large Scale Block Copolymer 2D Crystals

Author

Christophe Navarro, Karim Aissou, Jonah Shaver, Stéphane Grauby, Guillaume Fleury, Stefan Dilhaire, Gilles Pecastaings, Georges Hadziioannou, Jean-Michel Rampnoux, Cyril Brochon, Laboratoire de Chimie des Polymères Organiques (LCPO), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Team 4 LCPO : Polymer Materials for Electronic, Energy, Information and Communication Technologies, Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Laboratoire Ondes et Matière d'Aquitaine (LOMA), Université de Bordeaux (UB)-Centre National de la Recherche Scientifique (CNRS), Groupement de recherches de Lacq (GRL), Arkema (Arkema), and ANR-09-NANO-0026,MAGNIPHICO,Milieux magnétiques pour stockage d'information et processus lithographique basés sur les propriétés d'auto assemblage de copolymères séquencés(2009)

Subjects
Materials science, corrugated substrates, Polymers, Surface Properties, 02 engineering and technology, Grating, 010402 general chemistry, 01 natural sciences, chemistry.chemical_compound, Polymer chemistry, Copolymer, surface relief grating, General Materials Science, Thin film, Particle Size, Nanoscopic scale, Lithography, ComputingMilieux_MISCELLANEOUS, business.industry, Mechanical Engineering, 021001 nanoscience & nanotechnology, micropatterning, 0104 chemical sciences, Interferometry, block copolymers, [CHIM.POLY]Chemical Sciences/Polymers, Azobenzene, chemistry, 2D crystals, thin films, Mechanics of Materials, microstructures, Optoelectronics, Nanoparticles, 0210 nano-technology, business, Crystallization, Micropatterning
Abstract

We have overcome the cost and time consumption limitations of common lithography techniques used to control the self-assembly of block copolymers into highly ordered 2D arrays through the use of a guiding pattern created from a polymeric sub-layer. The guiding pattern is a sinusoidal surface-relief grating interferometrically inscribed onto an azobenzene containing copolymer sub-layer leading to a defect-free single grain of block copolymer domains.

Published
2013

20. Scaling-down lithographic dimensions with block-copolymer materials: 10-nm-sized features with poly(styrene)-block-poly(methylmethacrylate)

Author

Christophe Navarro, Guillaume Fleury, Ahmed Gharbi, Celia Nicolet, Raluca Tiron, Michaël Delalande, Jonathan Pradelles, Xavier Chevalier, Georges Hadziioannou, Gilles Cunge, Maxime Argoud, Groupement de recherches de Lacq (GRL), Arkema (Arkema), Commissariat à l'énergie atomique et aux énergies alternatives - Laboratoire d'Electronique et de Technologie de l'Information (CEA-LETI), Direction de Recherche Technologique (CEA) (DRT (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Laboratoire de Chimie des Polymères Organiques (LCPO), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Laboratoire des technologies de la microélectronique (LTM), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Joseph Fourier - Grenoble 1 (UJF)-Centre National de la Recherche Scientifique (CNRS), Team 4 LCPO : Polymer Materials for Electronic, Energy, Information and Communication Technologies, Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université Joseph Fourier - Grenoble 1 (UJF)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), and Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Nanotechnology, 02 engineering and technology, 01 natural sciences, Styrene, chemistry.chemical_compound, block-copolymer, 0103 physical sciences, Copolymer, PS-b-PMMA, Microelectronics, Electrical and Electronic Engineering, Thin film, Lithography, graphoepitaxy, 010302 applied physics, chemistry.chemical_classification, business.industry, Mechanical Engineering, Polymer, self-assembly, 021001 nanoscience & nanotechnology, Condensed Matter Physics, Atomic and Molecular Physics, and Optics, Electronic, Optical and Magnetic Materials, [CHIM.POLY]Chemical Sciences/Polymers, CMOS, chemistry, lithography, Self-assembly, 0210 nano-technology, business
Abstract

International audience; Poly(styrene)-block-poly(methylmethacrylate) (PS-b-PMMA) block-copolymers (BCP) systems synthesized on an industrial scale and satisfying microelectronic's requirements for metallic contents specifications are studied in terms of integration capabilities for lithographic applications. We demonstrate in particular that this kind of polymer can efficiently achieve periodic features close to 10 nm. These thin films can be transferred in various substrates through dry-etching techniques. The self-assembly optimization for each polymer is first performed on free-surface, leading to interesting properties, and the changes in self-assembly rules for low molecular-weight polymers are investigated and highlighted through different graphoepitaxy approaches. The improvements in self-assembly capabilities toward low periodic polymers, as well as the broad range of achievable feature sizes, make the PS-b-PMMA system very attractive for lithographic CMOS applications. We conclude by showing that high-chi polymer materials developed in Arkema's laboratories can be efficiently used to reduce the pattern's size beyond the ones of PS-b-PMMA based BCP's capabilities. (C) 2013 Society of Photo-Optical Instrumentation Engineers (SPIE)

Published
2013

21. Evaluation of thiocarbonyl and thioester moieties as thiol protecting groups for controlled radical polymerization

Author

Benoît Magny, Morgane Le Neindre, Renaud Nicolaÿ, Laboratoire Matière Molle et Chimie (MMC), Ecole Superieure de Physique et de Chimie Industrielles de la Ville de Paris (ESPCI Paris), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Centre National de la Recherche Scientifique (CNRS), Groupement de recherches de Lacq (GRL), and Arkema (Arkema)

Subjects
chemistry.chemical_classification, Nitroxide mediated radical polymerization, Polymers and Plastics, 010405 organic chemistry, Organic Chemistry, Radical polymerization, Bioengineering, 010402 general chemistry, Thioester, 01 natural sciences, Biochemistry, 0104 chemical sciences, Living free-radical polymerization, Polymerization, chemistry, Polymer chemistry, Moiety, [CHIM]Chemical Sciences, Reversible addition−fragmentation chain-transfer polymerization, Protecting group, ComputingMilieux_MISCELLANEOUS
Abstract

Thiol chemistry is a versatile and powerful tool for the preparation of functional polymers and materials. In that regard, xanthate, dithiocarbamate and thioacetate moieties were evaluated as thiol protecting groups for radical polymerization. Model reactions were conducted to study the effect of these moieties during RAFT polymerization of (meth)acrylates and styrene. The removal of these protecting groups by aminolysis was also investigated. The S-alkyl-O-ethyl dithiocarbonate moiety proved to be the best all-around protecting group since it did not induce any side reaction during controlled radical polymerization of all three types of monomers and could be easily and completely removed at room temperature. Monomers carrying a xanthate group were synthesized and used to prepare various (protected) polythiols with (meth)acrylate backbones by RAFT polymerization or ATRP. One-pot thiol deprotection and functionalization was carried out to exemplify the simplicity and efficiency of the present approach for the preparation of functional polymers and materials.

Published
2013

22. Pattern density multiplication by direct self assembly of block copolymers: Towards 300mm CMOS requirements

Author

Christophe Navarro, Michaël Delalande, Thierry Chevolleau, Christophe Couderc, Hervé Fontaine, Stéphanie Gaugiran, Gilles Cunge, Georges Hadziioannou, Guillaume Fleury, Raluca Tiron, Xavier Chevalier, Laurent Pain, Jonathan Pradelles, Commissariat à l'énergie atomique et aux énergies alternatives - Laboratoire d'Electronique et de Technologie de l'Information (CEA-LETI), Direction de Recherche Technologique (CEA) (DRT (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Hôpital Henri Mondor, Assistance publique - Hôpitaux de Paris (AP-HP) (AP-HP)-Hôpital Henri Mondor-Université Paris-Est Créteil Val-de-Marne - Paris 12 (UPEC UP12), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Laboratoire des technologies de la microélectronique (LTM), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Joseph Fourier - Grenoble 1 (UJF)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Chimie des Polymères Organiques (LCPO), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Team 4 LCPO : Polymer Materials for Electronic, Energy, Information and Communication Technologies, Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Université Joseph Fourier - Grenoble 1 (UJF)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Centre National de la Recherche Scientifique (CNRS)-Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC), and Centre National de la Recherche Scientifique (CNRS)-Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)

Subjects
Silicon, Computer science, chemistry.chemical_element, plasma etching, Nanotechnology, block copolymer, 02 engineering and technology, 01 natural sciences, 0103 physical sciences, directed self-assembly, Copolymer, PS-b-PMMA, Lithography, ComputingMilieux_MISCELLANEOUS, graphoepitaxy, 010302 applied physics, Plasma etching, business.industry, Lithography process, 021001 nanoscience & nanotechnology, Solvent, [CHIM.POLY]Chemical Sciences/Polymers, CMOS, chemistry, ISBN: 978-0-8194-8979-1, Optoelectronics, Self-assembly, 0210 nano-technology, business, Electron-beam lithography
Abstract

Conference on Alternative Lithographic Technologies IV Location: San Jose, CA Date: FEB 13-16, 2012 Sponsor(s): SPIE; International audience; In this paper we investigate the possibility to reach 300mm CMOS requirements by integrating graphoepitaxy of PS-b-PMMA self-assembly. Different schemes to integrate DSA process by using 193nm dry lithography or e-Beam lithography will be presented. Moreover, several challenges like solvent compatibility, bake kinetics and defectivity will be addressed. Concerning defectivity, we will propose a methodology in order to evaluate and optimize the long range order induced by graphoepitaxy of the block copolymer DSA. This approach affords the monitoring of the overall block copolymer self-assembly process and enables us to easily optimize the parameters required for a long-range order structuration, leading to a near zero-defects block copolymers self-assembled arrays. Transfer capabilities of the PS masks in the bulk silicon substrate by using plasma-etching will be also detailed, both with the film on bare silicon or organized with graphoepitaxy approaches. These results show the high potential of DSA to be integrated directly into the conventional CMOS lithography process in order to achieve high resolution and pattern density multiplication, at a low cost.

Published
2012

23. (0) Save to: more options Facile and versatile synthesis of rod-coil poly(3-hexylthiophene)-based block copolymers by nitroxide-mediated radical polymerization

Author

Mougnier, Sébastien Jun, Brochon, Cyril, Cloutet, Eric, Magnet, Stéphanie, Navarro, Christophe, Hadziioannou, Georges, Laboratoire de Chimie des Polymères Organiques (LCPO), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Team 4 LCPO : Polymer Materials for Electronic, Energy, Information and Communication Technologies, Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Groupement de recherches de Lacq (GRL), and Arkema (Arkema)

Subjects
block copolymers, nitroxide-mediated radical polymerization, [CHIM.POLY]Chemical Sciences/Polymers, conjugated polymers, macroinitiator, radical polymerization
Abstract

International audience; A well-defined and monofunctional poly(3-hexylthiophene)-based (P3HT) macroinitiator has been obtained through a clean, simple, and an efficient multistep synthesis process. The macroinitiator is obtained via intermolecular radical 1,2-addition onto an ?-acrylate-terminated P3HT macromonomer. In a second step, well-defined rod-coil block copolymers were obtained by nitroxide-mediated radical polymerization (NMRP) using the so-called Blocbuilder (R). The polymerization was found to be controlled with various monomers such as styrene, isoprene, 4-vinylpyridine, or methyl acrylate. This process constitutes a very promising way to obtain versatile and clean materials for organic electronics. (c) 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2012

Published
2012

24. Well-Defined Amphiphilic Block Copolymer Nanoobjects via Nitroxide-Mediated Emulsion Polymerization

Author

Laurence Couvreur, Emilie Groison, Ségolène Brusseau, Stéphanie Magnet, Rabi Inoubli, Franck D'Agosto, Bernadette Charleux, Laboratoire de Chimie, Catalyse, Polymères et Procédés, R 5265 (C2P2), Centre National de la Recherche Scientifique (CNRS)-École supérieure de Chimie Physique Electronique de Lyon (CPE)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Centre de recherche Rhône-Alpes (CRRA), and Arkema

Subjects
Nitroxide mediated radical polymerization, Molar mass, Materials science, Polymers and Plastics, Organic Chemistry, Emulsion polymerization, Nanoparticle, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Micelle, 0104 chemical sciences, Inorganic Chemistry, Nanofiber, Amphiphile, Polymer chemistry, Materials Chemistry, Copolymer, [CHIM]Chemical Sciences, 0210 nano-technology, ComputingMilieux_MISCELLANEOUS
Abstract

Water-soluble macroalkoxyamines are shown to be particularly well-suited initiators for nitroxide-mediated emulsion polymerization. They lead to the synthesis of amphiphilic block copolymers that self-assemble in situ into well-defined nanoobject morphologies, in agreement with the principles of polymerization-induced micellization. Depending on the molar mass of the hydrophobic block, the formed nanoparticles are hairy spherical micelles, nanofibers, or vesicles. The nanofibers are the most intriguing and spectacular structure and strongly affect the physicochemical properties of the aqueous dispersions.

Published
2012

26. Optimization of block copolymer self-assembly through graphoepitaxy: A defectivity study

Author

Jessy Bustos, Xavier Chevalier, Raluca Tiron, Christophe Navarro, Georges Hadziioannou, Guillaume Fleury, Jonathan Pradelles, Christophe Couderc, Laurent Pain, Stéphanie Magnet, Commissariat à l'énergie atomique et aux énergies alternatives - Laboratoire d'Electronique et de Technologie de l'Information (CEA-LETI), Direction de Recherche Technologique (CEA) (DRT (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Laboratoire de Chimie des Polymères Organiques (LCPO), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Team 4 LCPO : Polymer Materials for Electronic, Energy, Information and Communication Technologies, Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), and Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Nanotechnology, CONFINEMENT, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, BLENDS, THIN-FILMS, Materials Chemistry, Perpendicular, Copolymer, TEMPLATES, Electrical and Electronic Engineering, Instrumentation, Lithography, Spin coating, Delaunay triangulation, Process Chemistry and Technology, DIBLOCK COPOLYMER, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Surfaces, Coatings and Films, Electronic, Optical and Magnetic Materials, ARRAYS, ALIGNMENT, Template, [CHIM.POLY]Chemical Sciences/Polymers, Resist, Trench, PATTERNS, ORIENTATIONAL ORDER, 0210 nano-technology, DEVICE-ORIENTED STRUCTURES
Abstract

International audience; In this paper we report a synoptic methodology to evaluate and optimize the long-range order induced by graphoepitaxy of block copolymer (BCP) self-assembly. The authors focus the study on a BCP that produces hexagonally packed arrays of cylinders oriented perpendicular to the substrate with the copolymer film thickness greater than the trench depth. Prepatterned structures used in the graphoepitaxy approach have been generated by e-beam lithography on a commercial hydrogen silesquioxane resist. A suitable surface modification was accomplished by grafting a random polystyrene-r-poly(methyl methacrylate) copolymer on the prepatterned surfaces. The polystyrene-b-poly(methyl methacrylate) was spin-coated and annealed in order to generate the desired self-assembly. Since the self-assembly process is based on a thermodynamic mechanism, the induced defectivity needs to be reassessed with respect to the standard lithographic process. Using the cylinder center coordinates, a Delaunay triangulation is performed to find the nearest neighbors. This triangulation enables us to easily locate the disclinations which are characterized by having a number of nearest neighbors different from six. Thus, the number of defects can be quantified precisely. Additionally, this methodology affords an accurate evaluation of both the optimum mesa and trench critical dimensions yielding defect-free surfaces and may be extended to monitor the robustness of the BCP directed self-assembly process. Such diagnostics are critical in the implementation of large scale industrial processes.

Published
2011

27. Hazardous dichloromethane recovery in combined temperature and vacuum pressure swing adsorption process

Author

Serge Nicolas, Sylvain Giraudet, Olivier Baudouin, Laurence Le Coq, Stéphane Déchelotte, Alice Medevielle, Shivaji G. Ramalingam, Pierre Le Cloirec, Jerôme Saussac, Pascaline Pré, Département Systèmes Energétiques et Environnement (IMT Atlantique - DSEE), IMT Atlantique (IMT Atlantique), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT), Valorisation Energie-matière des Résidus et Traitement des Emissions (GEPEA-VERTE), Laboratoire de génie des procédés - environnement - agroalimentaire (GEPEA), Institut Universitaire de Technologie - Nantes (IUT Nantes), Université de Nantes (UN)-Université de Nantes (UN)-Université de Nantes - UFR des Sciences et des Techniques (UN UFR ST), Université de Nantes (UN)-Université de Nantes (UN)-Institut Universitaire de Technologie Saint-Nazaire (IUT Saint-Nazaire), Université de Nantes (UN)-Ecole Polytechnique de l'Université de Nantes (EPUN), Université de Nantes (UN)-École nationale vétérinaire, agroalimentaire et de l'alimentation Nantes-Atlantique (ONIRIS)-Centre National de la Recherche Scientifique (CNRS)-Université Bretagne Loire (UBL)-IMT Atlantique (IMT Atlantique), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-Institut Universitaire de Technologie - La Roche-sur-Yon (IUT La Roche-sur-Yon), Université de Nantes (UN)-Institut Universitaire de Technologie - Nantes (IUT Nantes), Université de Nantes (UN), ProSim. SA (ProSim. SA), ProSim. SA, 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), Arkema (Arkema), ProSim SA (FRANCE), Mines Nantes (Mines Nantes)-Université de Nantes - UFR des Sciences et des Techniques (UN UFR ST), Université de Nantes (UN)-Université de Nantes (UN)-Ecole Nationale Vétérinaire, Agroalimentaire et de l'alimentation Nantes-Atlantique (ONIRIS)-Centre National de la Recherche Scientifique (CNRS), Mines Nantes (Mines Nantes), Université européenne de Bretagne - European University of Brittany (UEB), Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Rennes 1 (UR1), Université de Rennes (UNIV-RENNES)-Université de Rennes (UNIV-RENNES)-Ecole Nationale Supérieure de Chimie de Rennes (ENSCR)-Institut National des Sciences Appliquées - Rennes (INSA Rennes), Institut National des Sciences Appliquées (INSA)-Université de Rennes (UNIV-RENNES)-Institut National des Sciences Appliquées (INSA), Groupement de recherches de Lacq (GRL), Université de Nantes (UN)-Université de Nantes (UN)-École nationale vétérinaire, agroalimentaire et de l'alimentation Nantes-Atlantique (ONIRIS)-Centre National de la Recherche Scientifique (CNRS), IMT Atlantique Bretagne-Pays de la Loire (IMT Atlantique), Université de Nantes (UN)-Ecole Nationale Vétérinaire, Agroalimentaire et de l'alimentation Nantes-Atlantique (ONIRIS)-Centre National de la Recherche Scientifique (CNRS)-Université Bretagne Loire (UBL)-IMT Atlantique Bretagne-Pays de la Loire (IMT Atlantique), Université de Rennes 1 (UR1), Université de Rennes (UNIV-RENNES)-Université de Rennes (UNIV-RENNES)-Institut National des Sciences Appliquées - Rennes (INSA Rennes), and Institut National des Sciences Appliquées (INSA)-Université de Rennes (UNIV-RENNES)-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)

Subjects
Environmental Engineering, Vacuum, Health, Toxicology and Mutagenesis, Thermal desorption, 02 engineering and technology, 010501 environmental sciences, 7. Clean energy, 01 natural sciences, Hazardous Substances, law.invention, chemistry.chemical_compound, [SPI]Engineering Sciences [physics], Adsorption, [CHIM.GENI]Chemical Sciences/Chemical engineering, law, [CHIM.ANAL]Chemical Sciences/Analytical chemistry, Desorption, medicine, Fixed bed, Pressure, Environmental Chemistry, [SPI.GPROC]Engineering Sciences [physics]/Chemical and Process Engineering, Process simulation, Breakthrough curve, Waste Management and Disposal, ComputingMilieux_MISCELLANEOUS, 0105 earth and related environmental sciences, Dichloromethane, chemistry.chemical_classification, Methylene Chloride, Volatile Organic Compounds, Waste management, [SDE.IE]Environmental Sciences/Environmental Engineering, Vacuum regeneration, Equipment Design, Models, Theoretical, 021001 nanoscience & nanotechnology, Pollution, Ignition system, Hydrocarbon, chemistry, Chemical engineering, Hot nitrogen, 0210 nano-technology, Simulation, Activated carbon, medicine.drug
Abstract

International audience; Organic vapors emitted from solvents used in chemical and pharmaceutical processes, or from hydrocarbon fuel storage stations at oil terminals, can be efficiently captured by adsorption onto activated carbon beds. To recover vapors after the adsorption step, two modes of regeneration were selected and could be possibly combined: thermal desorption by hot nitrogen flow and vacuum depressurization (VTSA). Because of ignition risks, the conditions in which the beds operate during the adsorption and regeneration steps need to be strictly controlled, as well as optimized to maintain good performances. In this work, the optimal conditions to be applied during the desorption step were determined from factorial experimental design (FED), and validated from the process simulation results. The regeneration performances were compared in terms of bed regeneration rate, concentration of recovered volatile organic compounds (VOC) and operating costs. As an example, this methodology was applied in case of dichloromethane. It has been shown that the combination of thermal and vacuum regeneration allows reaching 82% recovery of dichloromethane. Moreover, the vacuum desorption ended up in cooling the activated carbon bed from 93°C to 63°C and so that it significantly reduces the cooling time before starting a new cycle.

Published
2011

28. Influence of Rod-coil Block Copolymers on Bulk Heterojunction Organic Solar Cells: Correlation between Morphology and Photovoltaic Performance

Author

Deribew, Dargie Hailu, Nicolet, Célia, Renaud, Cédric, Brochon, Cyril, Fleury, Guillaume, Cloutet, Eric, Vignau, Laurence, Hadziioannou, Georges, Vignau, Laurence, Laboratoire de Chimie des Polymères Organiques (LCPO), Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Centre National de la Recherche Scientifique (CNRS), Groupement de recherches de Lacq (GRL), Arkema (Arkema), THEME 3, Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Centre National de la Recherche Scientifique (CNRS)-Université de Bordeaux (UB)-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Institut Polytechnique de Bordeaux-Centre National de la Recherche Scientifique (CNRS), ORGANIQUE / ELORGA, Laboratoire de l'intégration, du matériau au système (IMS), Université Sciences et Technologies - Bordeaux 1-Institut Polytechnique de Bordeaux-Centre National de la Recherche Scientifique (CNRS)-Université Sciences et Technologies - Bordeaux 1-Institut Polytechnique de Bordeaux-Centre National de la Recherche Scientifique (CNRS), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Team 3 LCPO : Polymer Self-Assembly & Life Sciences, Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), and Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Université Sciences et Technologies - Bordeaux 1-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Université Sciences et Technologies - Bordeaux 1

Subjects
[CHIM.POLY] Chemical Sciences/Polymers, [CHIM.POLY]Chemical Sciences/Polymers, [SPI.NANO] Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, ComputingMilieux_MISCELLANEOUS
Abstract

National audience

Published
2011

29. Polymerization-induced self-assembling of amphiphilic block copolymers in water

Author

Segolene Brusseau, Emilie Groison, Stephanie Boisse, Xuewei Zhang, Wenjing Zhang, Jutta Rieger, Muriel Lansalot, Agosto, Franck D., Bernadette Charleux, Stephanie Magnet, Raber Inoubli, Laurence Couvreur, Laboratoire de Chimie, Catalyse, Polymères et Procédés, R 5265 (C2P2), Centre National de la Recherche Scientifique (CNRS)-École supérieure de Chimie Physique Electronique de Lyon (CPE)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC), Chimie des polymères (LCP), Université Pierre et Marie Curie - Paris 6 (UPMC)-Institut Parisien de Chimie Moléculaire (IPCM), Université Pierre et Marie Curie - Paris 6 (UPMC)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Arkema, Université Claude Bernard Lyon 1 (UCBL), and Université de Lyon-Université de Lyon-École Supérieure de Chimie Physique Électronique de Lyon (CPE)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
[CHIM]Chemical Sciences, ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2011

30. Procédé de préparation d'un polymère d'au moins un monomère cyclique

Author

Bourissou, D., Delcroix, Damien, Martin-Vaca, B., Navarro, C., Laboratoire Hétérochimie Fondamentale et Appliquée (LHFA), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut de Chimie de Toulouse (ICT-FR 2599), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD), Groupement de recherches de Lacq (GRL), and Arkema (Arkema)

Subjects
[CHIM.ORGA]Chemical Sciences/Organic chemistry
Published
2009

31. Système organique pour la polymérisation par ouverture de cycle de carbonates cycliques pour l'obtention de (bio)polycarbonates

Author

Bourissou, D., Martin-Vaca, B., Delcroix, Damien, Navarro, C., Laboratoire Hétérochimie Fondamentale et Appliquée (LHFA), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut de Chimie de Toulouse (ICT-FR 2599), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD), Groupement de recherches de Lacq (GRL), and Arkema (Arkema)

Subjects
[CHIM.ORGA]Chemical Sciences/Organic chemistry
Published
2009

32. ROP de l'e-caprolactone organo-catalysée par les acides sulfoniques

Author

Bourissou, D., Delcroix, Damien, Gazeau-Bureau, Stephanie, Magnet, Stéphanie, Martin-Vaca, B., Navarro, C., Laboratoire Hétérochimie Fondamentale et Appliquée (LHFA), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut de Chimie de Toulouse (ICT-FR 2599), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD), Groupement de recherches de Lacq (GRL), and Arkema (Arkema)

Subjects
[CHIM.ORGA]Chemical Sciences/Organic chemistry
Published
2009

33. Influence of the Spinning Conditions on the Structure and Properties of Polyamide 12/Carbon Nanotube Composite Fibers

Author

Carine Perrot, Philippe Poulin, Cécile Zakri, Patrice Gaillard, Patrick M. Piccione, Centre de recherches Paul Pascal (CRPP), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université Sciences et Technologies - Bordeaux 1, Groupement de recherches de Lacq (GRL), and Arkema (Arkema)

Subjects
Materials science, Polymers and Plastics, Composite number, Nanoparticle, 02 engineering and technology, Carbon nanotube, fibers, 010402 general chemistry, 01 natural sciences, law.invention, law, nanocomposites, Materials Chemistry, Fiber, Composite material, polyamides, Spinning, chemistry.chemical_classification, General Chemistry, Polymer, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Surfaces, Coatings and Films, extrusion, chemistry, Polyamide, Extrusion, 0210 nano-technology
Abstract

The inclusion of nanoparticles in polymer fibers is potentially useful for improving or bringing new properties such as mechanical strength, electrical conductivity, piezoresistivity, and flame retardancy. In this study, composite fibers made of polyamide 12 and multiwall carbon nanotubes were investigated. The fibers were spun via a melt-spinning process and stretched at different draw ratios. The influence of several spinning factors, including spinning speed, extrusion rate, and draw ratio were investigated and correlated to the structure and properties of the fibers. X-ray diffraction analyses and mechanical tests indicated that the spinning speed barely affected the structure and mechanical properties of the fibers under tension. The spinning speed, however, is critical for future industrial applications because it determines the possible production rates. By contrast, drawing during spinning or after spinning strongly affected the polymer chain alignment and fiber mechanical properties. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009

Published
2009

34. Process for preparation of microgel particles by controlled radical polymerization in aqueous dispersion using nitroxide control agents

Author

Magnet, Stephanie, Charleux, Bernadette, Delaittre, Guillaume, Save, Maud, Groupement de recherches de Lacq (GRL), Arkema (Arkema), Chimie des polymères (LCP), Université Pierre et Marie Curie - Paris 6 (UPMC)-Institut Parisien de Chimie Moléculaire (IPCM), Université Pierre et Marie Curie - Paris 6 (UPMC)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Institut des sciences analytiques et de physico-chimie pour l'environnement et les materiaux (IPREM), Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université de Pau et des Pays de l'Adour (UPPA), and Université de Pau et des Pays de l'Adour (UPPA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
vinyl polymer microgel dispersion manuf phosphonate nitroxide mediator, [CHIM]Chemical Sciences
Abstract

The invention relates to a method for prepg. microgel particles according to a method of controlled radical polymn. in an aq. dispersion using particular control agents of the nitroxide type. Use in the biomedical field, and in the field of agrochem., cosmetics, surface coatings. Dispersions of microgel particulates with particle size ≤100 nm are manufd. in the absence of surfactants by (a) polymn. of ≥1 monomer in the presence of R2OCOCR1R3ON(CMe3)CH(CMe3)P(:O)(OEt)2or Z[CH(CH2CR1R3CO2R2)ON(CMe3)CH(CMe3)P(:O)(OEt)2]n [R1, R3 = C1-3 alkyl, R2 = H, C1-8 alkyl, Ph, alkali metal, or NH4, Z = arom. group or Z1[XC(O)]n, Z1 = polyfunctional group, X = O, N having a carbon-contg. group or H, or S, n ≥ 2] in an aq. media, (b) polymn. of a vinyl monomer different from the monomer in step (a) in the reaction medium contg. the macroinitiator from step (a), and (c) polymn. of a crosslinking monomer in the reaction medium from step (b), with ≥1 of the monomers from steps (a), (b), and (c) having ≥1 group selected from CO2H, SO3H, NH4, ethylene oxide, amino, and amide, with the group optionally existing in the presence of a salt. [on SciFinder(R)]

Published
2008

35. Norme NF X43-903. Mai 2008. Biosurveillance de l'environnement. Détermination d'un indice biologique de lichens épiphytes (IBLE)

Author

Van Haluwyn,, Garrec, Jean-Pierre, Asta,, Bernard,, Bispo, Antonio, Boisleux,, Casas,, Castell, Jean-François, Claveri,, Clochiatti,, Cuny,, Davranche,, Deguine,, Denayer,, Durif,, Estivie,, Flach-Malaspina,, Galsomies,, Gancet,, Gombert,, Lallemant,, Leblond,, Lenoir,, Lerique,, Pandard,, Rausch de Traubenberg, Anna, Signoret,, Association Française de Normalisation, ., Université de Lille, Droit et Santé, Ecologie et Ecophysiologie Forestières [devient SILVA en 2018] (EEF), Institut National de la Recherche Agronomique (INRA)-Université de Lorraine (UL), Laboratoire d'Ecologie Alpine (LECA), Université Joseph Fourier - Grenoble 1 (UJF)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), Université de Franche-Comté (UFC), Université Bourgogne Franche-Comté [COMUE] (UBFC), Agence de l'Environnement et de la Maîtrise de l'Energie (ADEME), VEOLIA France, Institut National Agronomique Paris Grignon (INAPG), BioMonitor [Chambley-Bussières], Partenaires INRAE, Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Association pour la Prévention de la Pollution Atmosphérique, Kali'air SAS, Institut National de l'Environnement Industriel et des Risques (INERIS), Gaz de France Suez (GDF Suez), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Université Bordeaux Montaigne (UBM), Aair Lichens, Muséum national d'Histoire naturelle (MNHN), Conseil régional Nord-Pas de Calais, Association Française de Normalisation (AFNOR), Université Joseph Fourier - Grenoble 1 (UJF)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry]), and Université Bordeaux Montaigne

Subjects
NORME FRANCAISE HOMOLOGUEE, AIR, [SDV]Life Sciences [q-bio], POLLUTION ATMOSPHERIQUE, CONTROLE
Abstract

Document non diffusable; National audience; Le présent document définit une méthode de détermination de l'Indice Biologique de Lichens Epiphytes (IBLE). Il s'applique aussi bien en milieu industriel, urbain, peri-urbain que rural, à l'exception du milieu forestier. Le présent document ne permet pas de donner une mesure directe de la concentration des contaminents atmosphériques.

Published
2008

36. Norme NF X43-902. Mai 2008. Biosurveillance de l'air. Biosurveillance passive de la qualité de l'air à l'aide de mousses autochtones : de la récolte à la préparation des échantillons

Author

van Haluwyn,, Garrec, Jean-Pierre, Asta,, Bernard,, Bispo, Antonio, Boisleux,, Casas,, Castell, Jean-François, Claveri,, Clochiatti,, Cuny,, Davranche,, Deguine,, Denayer,, Durif,, Estivie,, Flach Malaspina,, Galsomies,, Gancet,, Gombert,, Lallemant,, Leblond,, Lenoir,, Lerique,, Pandard,, Rausch de Traubenberg, Anna, Signoret,, Association Française de Normalisation, ., Université de Lille, Droit et Santé, Ecologie et Ecophysiologie Forestières [devient SILVA en 2018] (EEF), Institut National de la Recherche Agronomique (INRA)-Université de Lorraine (UL), Laboratoire d'Ecologie Alpine (LECA), Université Joseph Fourier - Grenoble 1 (UJF)-Centre National de la Recherche Scientifique (CNRS)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry]), Université de Franche-Comté (UFC), Université Bourgogne Franche-Comté [COMUE] (UBFC), Agence de l'Environnement et de la Maîtrise de l'Energie (ADEME), VEOLIA France, Institut National Agronomique Paris Grignon (INAPG), BioMonitor [Chambley-Bussières], Partenaires INRAE, Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Association pour la Prévention de la Pollution Atmosphérique, Kali'air SAS, Institut National de l'Environnement Industriel et des Risques (INERIS), Gaz de France Suez (GDF Suez), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Université Bordeaux Montaigne, Aair Lichens, Muséum national d'Histoire naturelle (MNHN), Conseil régional Nord-Pas de Calais, Association Française de Normalisation (AFNOR), Université Joseph Fourier - Grenoble 1 (UJF)-Université Savoie Mont Blanc (USMB [Université de Savoie] [Université de Chambéry])-Centre National de la Recherche Scientifique (CNRS), and Université Bordeaux Montaigne (UBM)

Subjects
MODE OPERATOIRE, ECHANTILLONAGE, AIR, [SDV]Life Sciences [q-bio], CONTROLE, MESURAGE
Abstract

Document non diffusable; National audience; Le présent document décrit une méthode pour l'échantillonnage et la préparation d'échantillons de mousses autochtones pour la bioaccumulation de substances caractérisant une pollution atmosphérique et définit les actions à mener depuis le prélèvement in situ de mousses sur toute surface horizontale jusqu'au conditionnement final et au transport des échantillons en vue de l'analyse des contaminants recherchés.

Published
2008

37. Organo-catalyzed ROP of C-caprolactone : methane sulfonic acid competes with trifluoromethane sulfonic acid

Author

Bourissou, D., Gazeau-Bureau, Stephanie, Martin-Vaca, B., Navarro, C., Delcroix, Damien, Magnet, Stéphanie, Laboratoire Hétérochimie Fondamentale et Appliquée (LHFA), Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut de Chimie de Toulouse (ICT-FR 2599), Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université Fédérale Toulouse Midi-Pyrénées-Institut de Chimie du CNRS (INC)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche pour le Développement (IRD), Groupement de recherches de Lacq (GRL), and Arkema (Arkema)

Subjects
[CHIM.ORGA]Chemical Sciences/Organic chemistry, ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
2008

38. Norme NF X 43-900. Mai 2008. Bio-indication de l'ozone par le tabac

Author

van Haluwyn, C, Garrec, Jean-Pierre, Asta,, Bernard,, Bispo, Antonio, Boisleux,, Casas,, Castell, Jean-François, Claveri,, Clochiatti,, Cuny,, Davranche,, Deguine,, Denayer,, Durif,, Estivie,, Flach-Malaspina,, Galsomies,, Gancet,, Gombert,, Lallemant,, Leblond,, Lenoir,, Lerique,, Pandard,, Rausch de Traubenberg, Anna, Signoret,, Université de Lille, Droit et Santé, Ecologie et Ecophysiologie Forestières [devient SILVA en 2018] (EEF), Institut National de la Recherche Agronomique (INRA)-Université de Lorraine (UL), Université Joseph Fourier - Grenoble 1 (UJF), Agence de l'Environnement et de la Maîtrise de l'Energie (ADEME), VEOLIA France, Institut National Agronomique Paris Grignon (INAPG), BioMonitor [Chambley-Bussières], Partenaires INRAE, Commissariat à l'énergie atomique et aux énergies alternatives (CEA), APPA Nord pas de Calais, Kali'air SAS, Institut National de l'Environnement Industriel et des Risques (INERIS), Gaz de France Suez (GDF Suez), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Université Bordeaux Montaigne, Aair Lichens, Muséum national d'Histoire naturelle (MNHN), Conseil régional Nord-Pas de Calais, Association pour l'Exploitation du Réseau de mesures des vallées de la Fensch, de l'Orne et de la Moselle, and Université Bordeaux Montaigne (UBM)

Subjects
EXAMEN VISUEL, NORME FRANCAISE HOMOLOGUEE, AIR, [SDV]Life Sciences [q-bio], CONTROLE, FEUILLE : BOTANIQUE, POURCENTAGE, ENVIRONNEMENT, POLLUTION ATMOSPHERIQUE
Abstract

Document non diffusable ; National audience; Le présent document définit une méthode de détermination des impacts d'élèments photo oxydants atmosphériques (essentiellement l'ozone) sur un bégétal de référence, le tabac (variétés "Bel W3" et "Bel C" dans un environnement donné. Il s'applique en atmosphère extérieure dans tout milieu, mais ne s'applique pas à l'estimation de la qualité de l'air intérieur des bâtiments. Il ne s'applique pas à la mesure directe de la concentration absolue en ozonne de l'air.

Published
2008

39. Norme NF X 43-901. Mai 2008. Biosurveillance de la qualité de l'air à l'aide de ray-grass : des cultures à la préparation des échantillons

Author

van Haluwyn, C, Garrec, Jean-Pierre, Asta,, Bernard,, Bispo, Antonio, Boisleux,, Casas,, Castell, Jean-François, Claveri,, Clochiatti,, Cuny,, Davranche,, Deguine,, Denayer,, Durif,, Estivie,, Flach-Malaspina,, Galsomies,, Gancet,, Gombert,, Lallemant,, Leblond,, Lenoir,, Lerique,, Pandard,, Rausch de Traubenberg, Anna, Signoret,, Université de Lille, Droit et Santé, Ecologie et Ecophysiologie Forestières [devient SILVA en 2018] (EEF), Institut National de la Recherche Agronomique (INRA)-Université de Lorraine (UL), Centre National de la Recherche Scientifique (CNRS), Université Joseph Fourier - Grenoble 1 (UJF), Agence de l'Environnement et de la Maîtrise de l'Energie (ADEME), VEOLIA France, Institut National Agronomique Paris Grignon (INAPG), BioMonitor [Chambley-Bussières], Partenaires INRAE, Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Association pour la Prévention de la Pollution Atmosphérique, Kali'air SAS, Institut National de l'Environnement Industriel et des Risques (INERIS), Gaz de France Suez (GDF Suez), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Université Bordeaux Montaigne, Aair Lichens, Muséum national d'Histoire naturelle (MNHN), Conseil régional Nord-Pas de Calais, and Université Bordeaux Montaigne (UBM)

Subjects
NORME FRANCAISE HOMOLOGUEE, AIR, [SDV]Life Sciences [q-bio], PREPARATION, CONTROLE, MODE OPERTAOIRE
Abstract

Document non diffusable ; National audience; Le présent document décrit une méthode de culture, d'exposition et de prélèvement d'une variété de graminées, dénommée ci-après ray-grass, en vue de l'étude de la bioaccumulation de substances caractérisant uen pollution atmosphérique. Il s'applique essentiellement à la mise en évidence d'une ou plusieurs sources ponctuelles de pollution et/ou de sa zone d'influence. Il offre aussi un outil de surveillance d'un site sur le long terme par la répétition d'une procédure clairement définie. La méthode décrite dans le présent document permet d'effectuer des comparaisons spatiales et temporelles.

Published
2008

40. Effect of multi-walled carbon nanotubes on the lamellae morphology of polyamide-6

Author

Patrick M. Piccione, Ludwik Leibler, Anne-Carine Brosse, Sylvie Tencé-Girault, Laboratoire Matière Molle et Chimie (MMC), Ecole Superieure de Physique et de Chimie Industrielles de la Ville de Paris (ESPCI Paris), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Centre National de la Recherche Scientifique (CNRS), Groupement de recherches de Lacq (GRL), and Arkema (Arkema)

Subjects
Materials science, Nanocomposite, Polymers and Plastics, Scanning electron microscope, Organic Chemistry, Nucleation, Nanotechnology, 02 engineering and technology, Carbon nanotube, 010402 general chemistry, 021001 nanoscience & nanotechnology, Epitaxy, 01 natural sciences, 0104 chemical sciences, law.invention, Crystal, Chemical engineering, law, Materials Chemistry, Lamellar structure, Crystallite, 0210 nano-technology, ComputingMilieux_MISCELLANEOUS
Abstract

We show that crystal organization on both micro and nanoscales can be profoundly modified by dispersing carbon nanotubes (CNTs) in polyamide-6 by melt compounding. X-ray diffraction and transmission and scanning electron microscopies all indicate that when CNTs are well dispersed, crystalline spherulites are not present and remarkably crystalline lamellae grow aligning perpendicularly to the surface of the nanotubes. Such an epitaxial growth induced by CNTs during melt processing is particular to polyamide-6 because of crystallographic matching of CNTs and polyamide-6 crystal lattices. Macroscopically this epitaxial nucleation and growth can be detected and quantified by examining the splitting of the exothermic peak in calorimetric (DSC) experiments. Using optical microscopy and image analysis we show that the amount of trans-crystalline epitaxial crystallites increases when CNTs' dispersion quality is improved.

Published
2008

41. Nanostructured latex particles synthesized by nitroxide-mediated controlled/living free-radical polymerization in emulsion

Author

Céline Farcet, Stéphanie Magnet, Bernadette Charleux, Julien Nicolas, Pierre Gerard, Anne-Valérie Ruzette, Chimie des polymères (LCP), Université Pierre et Marie Curie - Paris 6 (UPMC)-Institut Parisien de Chimie Moléculaire (IPCM), Institut de Chimie du CNRS (INC)-Université Pierre et Marie Curie - Paris 6 (UPMC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Laboratoire Matière Molle et Chimie (MMC), Ecole Superieure de Physique et de Chimie Industrielles de la Ville de Paris (ESPCI Paris), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Centre National de la Recherche Scientifique (CNRS), Centre de recherche, développement, applications et technique de l'ouest (CERDATO), Arkema (Arkema), Groupement de recherches de Lacq (GRL), and Université Pierre et Marie Curie - Paris 6 (UPMC)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS)

Subjects
[PHYS]Physics [physics], Nitroxide mediated radical polymerization, Molar mass, Materials science, Polymers and Plastics, Organic Chemistry, Emulsion polymerization, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, chemistry.chemical_compound, Living free-radical polymerization, Monomer, chemistry, Polymer chemistry, Materials Chemistry, Copolymer, Molar mass distribution, Methyl methacrylate, 0210 nano-technology, ComputingMilieux_MISCELLANEOUS
Abstract

Suspensions of diblock and triblock copolymer particles comprising a poly(n-butyl acrylate) first/central block and polystyrene or poly(methyl methacrylate) second/outer blocks were synthesized by nitroxide-mediated controlled/living free-radical emulsion polymerization. Monofunctional and difunctional alkoxyamines based on the nitroxide SG1 were used as initiators. For the sake of simplicity, sequential monomer additions were performed without any removal of unreacted monomer. Self-assembly of the obtained block copolymers was investigated both under the latex form as well as after different thermal treatments. AFM and TEM analyses revealed the occurrence of “onion-like” lamellar microphases directly inside latex particles for high enough copolymer molar masses and irrespective of molar mass distribution. This particular organization evolved towards more classical block copolymer morphologies upon solvent casting and/or thermal annealing of latex films.

Published
2007

42. Ni CVD Catalyst for the Selective Preparation of small-diameter herringbone-type Graphite Nanofibers and their use in catalysis

Author

Philippe, Régis, Kihn, Yolande, Caussat, Brigitte, Plee, Dominique, Kalck, Philippe, Serp, Philippe, Institut National Polytechnique de Toulouse - Toulouse INP (FRANCE), Université Toulouse III - Paul Sabatier - UT3 (FRANCE), Arkema (FRANCE), Centre National de la Recherche Scientifique - CNRS (FRANCE), Laboratoire de chimie de coordination (LCC), Institut de Chimie de Toulouse (ICT), Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Institut de Recherche pour le Développement (IRD)-Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Génie Chimique (LGC), Université Toulouse III - Paul Sabatier (UT3), Université de Toulouse (UT)-Université de Toulouse (UT)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT), Centre d'élaboration de matériaux et d'études structurales (CEMES), Institut National des Sciences Appliquées - Toulouse (INSA Toulouse), Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut National des Sciences Appliquées (INSA)-Université de Toulouse (UT)-Institut de Chimie de Toulouse (ICT), Université de Toulouse (UT)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Groupement de recherches de Lacq (GRL), and Arkema (Arkema)

Subjects
[CHIM.GENI]Chemical Sciences/Chemical engineering, [CHIM.POLY]Chemical Sciences/Polymers, Nickel, Graphite Nanofibers, Génie chimique, [CHIM.CATA]Chemical Sciences/Catalysis, Catalyse, CVD, Catalysis, Polymères
Abstract

International audience; Graphite nanofibers (GNF) constitute an interesting carbon material for catalytic applications. Indeed, in addition to their large mesoporosity, the peculiar orientation of the graphene layers may influence the metal-support interaction [1] and thus, results in specific catalytic activity. As far as the production of GNF is concerned, most of the catalytic CVD processes used afford ill-defined materials. Indeed, GNF diameters distribution is usually large (20-100nm) [2-4] and the resulting specific surface area is often in the range 50-100m²/g [5,6]. These two points can reduce the field of their applications as catalyst support in heterogeneous catalysis. In this work, we report the selective growth of small diameter herringbone-type GNF by C-CVD on catalysts produced by fluidized bed organometallic CVD. First results dealing with the catalytic performances of PtRu/GNF systems for the selective hydrogenation of cinnamaldehyde will be also presented.

Published
2006

43. Amphiphilic diblock copolymers with adhesive properties: I. Structure and swelling with water

Author

N.E. El-Bounia, R. Ober, Frédéric Nallet, K. Schierholz, Olivier Guerret, Yves Gnanou, Pascale Fabre, Eric Papon, Sylwia Poivet, G. Abraham, Centre de recherches Paul Pascal (CRPP), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de Chimie des polymères organiques (LCPO), Centre National de la Recherche Scientifique (CNRS)-École Nationale Supérieure de Chimie et de Physique de Bordeaux (ENSCPB)-Université Sciences et Technologies - Bordeaux 1-Institut de Chimie du CNRS (INC), Team 1 LCPO : Polymerization Catalyses & Engineering, Laboratoire de Chimie des Polymères Organiques (LCPO), Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Polytechnique de Bordeaux-Ecole Nationale Supérieure de Chimie, de Biologie et de Physique (ENSCBP)-Université de Bordeaux (UB)-Institut de Chimie du CNRS (INC), Laboratoire de physique des fluides organisés (LPFO), Collège de France (CdF (institution))-Centre National de la Recherche Scientifique (CNRS), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Groupement de recherches de Lacq, and TotalFinaElf

Subjects
Absorption of water, Materials science, Kinetics, Biophysics, 02 engineering and technology, polymers on surfaces, 010402 general chemistry, 01 natural sciences, Amphiphile, copolymers, medicine, Copolymer, General Materials Science, Soft matter, SOLVENTS, macromolecular and polymers solutions, FREE-RADICAL POLYMERIZATION, Small-angle X-ray scattering, fungi, CAVITATION, Surfaces and Interfaces, General Chemistry, 021001 nanoscience & nanotechnology, DIFFUSION, 0104 chemical sciences, BLOCK-COPOLYMERS, [CHIM.POLY]Chemical Sciences/Polymers, Chemical engineering, Adhesive, Swelling, medicine.symptom, 0210 nano-technology, [PHYS.COND.CM-SCM]Physics [physics]/Condensed Matter [cond-mat]/Soft Condensed Matter [cond-mat.soft], TRANSITION, Biotechnology
Abstract

International audience; We study asymmetric block copolymers with the simple diblock AB architecture, in the case where the longer block A is both hydrophobic and "soft", whereas the shorter block B is hydrophilic and "hard". Materials with such a particular combination of physico-chemical and mechanical properties have distinctive advantages, in particular for designing water-compatible adhesive materials. The phase diagram is established, combining NMR and SAXS characterisations of the materials. The swelling with water is monitored through gravimetry and "time-resolved" SAXS. Indications of maintained adhesive properties in a wet environment are given.

Published
2006

44. Comparison of risk patterns in carcinoma and melanoma of the skin in men: a multi-centre case-case-control study

Author

Carmen Enid Martínez, Roberto Zanetti, Lorenzo Gafà, R Mossotti, G Fabbrocini, C Barbera, Adoración Nieto, H. Sancho-Garnier, A. Miranda, M Mercier, Carmen Navarro, D I Loria, A Chiarugi, Stefano Rosso, Anne Østerlind, R Greinert, Piedmont Cancer Registry-CPO, Centro Meteorológico en Illes Balears, Centro Meteorologico en Illes Balears, Carcinogénèse épithéliale : facteurs prédictifs et pronostiques - UFC ( CEF2P / CARCINO ), Centre Hospitalier Régional Universitaire [Besançon] ( CHRU Besançon ) -Université Bourgogne Franche-Comté ( UBFC ) -Université de Franche-Comté ( UFC ), ARKEMA, Arkema, Laboratoire d'Astrophysique de Marseille ( LAM ), Centre National de la Recherche Scientifique ( CNRS ) -Institut national des sciences de l'Univers ( INSU - CNRS ) -Aix Marseille Université ( AMU ) -Centre National d'Etudes Spatiales ( CNES ), Carcinogénèse épithéliale : facteurs prédictifs et pronostiques - UFC (EA 3181) (CEF2P / CARCINO), Université de Franche-Comté (UFC), Université Bourgogne Franche-Comté [COMUE] (UBFC)-Université Bourgogne Franche-Comté [COMUE] (UBFC)-Centre Hospitalier Régional Universitaire de Besançon (CHRU Besançon), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Laboratoire d'Astrophysique de Marseille (LAM), Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences de l'Univers (INSU - CNRS)-Aix Marseille Université (AMU)-Centre National d'Études Spatiales [Toulouse] (CNES), Carcinogénèse épithéliale : facteurs prédictifs et pronostiques - UFC (UR 3181) (CEF2P / CARCINO), Centre Hospitalier Régional Universitaire de Besançon (CHRU Besançon)-Université de Franche-Comté (UFC), and Université Bourgogne Franche-Comté [COMUE] (UBFC)-Université Bourgogne Franche-Comté [COMUE] (UBFC)

Subjects
Male, Cancer Research, Skin Neoplasms, Epidemiology, basal-cell carcinoma, MESH : Aged, [ SDV.CAN ] Life Sciences [q-bio]/Cancer, 030207 dermatology & venereal diseases, 0302 clinical medicine, Risk Factors, MESH: Risk Factors, MESH : Carcinoma, Squamous Cell, skin and connective tissue diseases, MESH: Aged, MESH: Middle Aged, skin cancer, Eye Color, integumentary system, MESH : Eye Color, MESH: Carcinoma, Squamous Cell, Middle Aged, MESH : Adult, MESH: Case-Control Studies, MESH : Risk Factors, 3. Good health, Oncology, Epidermoid carcinoma, 030220 oncology & carcinogenesis, case–case–control, Carcinoma, Squamous Cell, Adult, medicine.medical_specialty, MESH : Case-Control Studies, MESH: Eye Color, MESH: Melanoma, MESH : Sex Factors, MESH : Male, MESH : Melanoma, [SDV.CAN]Life Sciences [q-bio]/Cancer, MESH: Carcinoma, Basal Cell, MESH: Nevus, sun exposure, 03 medical and health sciences, Sex Factors, Case-case-control, MESH: Sex Factors, MESH : Nevus, melanoma, medicine, Carcinoma, Humans, Nevus, Basal cell carcinoma, MESH : Middle Aged, Risk factor, Hair Color, Aged, MESH: Humans, business.industry, MESH: Skin Neoplasms, MESH : Skin Neoplasms, MESH : Humans, Case-control study, squamous-cell carcinoma, MESH: Adult, MESH: Hair Color, medicine.disease, Dermatology, MESH : Carcinoma, Basal Cell, MESH: Male, Surgery, Carcinoma, Basal Cell, Case-Control Studies, Skin cancer, business, MESH : Hair Color
Abstract

International audience; We directly compared risk factors between 214 histologically confirmed melanomas (CMM), 215 basal-cell carcinomas (BCC) and 139 squamous-cell carcinomas (SCC) in a multiple case-case-control study with 349 controls from patients without dermatological disease admitted to the same hospitals. Subjects with fair hair had a significant risk increase for all types of tumours at a comparable level (OR(adj) for blonde hair: CMM 2.3; SCC 2.4; BCC 2.3). The effect of pale eyes was significant and similar for CMM and BCC (OR(adj) 2.6). Intermittent sun exposure measured in hours spent at beach during holidays was significant for both CMM (OR(adj) 2.6 for more than 7000 lifelong hours) and BCC (OR(adj) 2.1 for more than 7000 lifelong hours), while SCC exhibited a significant risk increase for chronic exposure to sunlight measured in hours of outdoor work (OR(adj) 2.2 for more than 6000 lifelong hours). In the case-case comparison using a multinomial logistic regression model, we found a statistically significant risk difference for pale eyes, and number of naevi in the CMM group, compared to other skin cancers. For intermittent sun exposure, there was a significant risk difference of BCC when compared to the risk of SCC. Factors influencing risk of SCC are different, with chronic exposure to sun playing a major role in causing this type of carcinoma.

Published
2006

45. Synthesis of dimethylalkylamines from acids and esters over promoted copper catalysts

Author

Barrault, Joël, Delahay, Gerard, Essayem, Nadine, Gaizi, Z., Forquy, Christian, Brouard, René, Laboratoire de Catalyse en Chimie Organique (LCO), Université de Poitiers-Centre National de la Recherche Scientifique (CNRS), Groupement de Recherches de Lacq (GRL), Elf Aquitaine, and CECA-ATOCHEM

Subjects
copper, amines, [CHIM.CATA]Chemical Sciences/Catalysis, fatty acids, ComputingMilieux_MISCELLANEOUS
Abstract

International audience

Published
1991

46. Pillars fabrication by DSA lithography: material and process options

Author

Christophe Navarro, G. Reynaud, Patricia Pimenta-Barros, C. Nicolet, Marta Fernández-Regúlez, M. Perego, Laurent Pain, Ahmed Gharbi, R. Tiron, Ian Cayrefourcq, E. Amat, Francesc Pérez-Murano, O. Saouaf, Commissariat à l'énergie atomique et aux énergies alternatives - Laboratoire d'Electronique et de Technologie de l'Information (CEA-LETI), Direction de Recherche Technologique (CEA) (DRT (CEA)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA), Groupement de recherches de Lacq (GRL), Arkema (Arkema), Laboratorio MDM (IMM-CNR), Consiglio Nazionale delle Ricerche [Roma] (CNR), Centro Nacional de Microelectronica [Spain] (CNM), European Project: 688072,H2020,H2020-ICT-2015,IONS4SET(2016), and National Research Council of Italy | Consiglio Nazionale delle Ricerche (CNR)

Subjects
010302 applied physics, Fabrication, Materials science, Silicon, Annealing (metallurgy), chemistry.chemical_element, block copolymer, self-assembly, 02 engineering and technology, 021001 nanoscience & nanotechnology, 01 natural sciences, law.invention, Anti-reflective coating, chemistry, law, Etching (microfabrication), 0103 physical sciences, lithography, Self-assembly, Dry etching, [SPI.NANO]Engineering Sciences [physics]/Micro and nanotechnologies/Microelectronics, Composite material, 0210 nano-technology, pillars, Lithography
Abstract

International audience; We investigate the fabrication of sub-20 nm pillars by DSA lithography using PS-cylinder-forming PS-b-PMMA block copolymer (BCP). The approach is based on the removal of PMMA-matrix by either dry or wet etching to form PS pillars which act as a soft etching mask that can be further transferred to an intermediate hard one and then to the substrate. The process conditions of BCP self-assembly were optimized in terms of annealing temperature, brush layer composition and film thickness. It was demonstrated that PS/PMMA volume fractions of 50/50 in the PS-r-PMMA brush layer is the most adapted to obtain standing PS cylinders. Top-down SEM images showed a hexagonal array of PS cylinders in a PMMA matrix with a natural period of 33.5 nm (determined by Fast Fourier Transform FFT method) and CD around 15 nm. Both wet and dry etching strategies for PMMA removal were discussed. It was shown that UV exposure followed by organic solvent development is necessary to decrease pattern collapsing during PMMA removal step which is the most critical issue for pillar fabrication. PMMA removal by dry etching was shown to completely avoid this pattern collapsing. Finally, pillars etching transfer to typical organic Si containing antireflective coating and spin on carbon (SiARC/SOC) hard mask and then to the silicon substrate was demonstrated. Si pillars of 15 nm CD and 70 nm height were obtained with a straight profile shape.(c) SPIE 2019

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47. Lung inflammation and lack of genotoxicity in the comet and micronucleus assays of industrial multiwalled carbon nanotubes Graphistrength(©) C100 after a 90-day nose-only inhalation exposure of rats.

Author

Pothmann D, Simar S, Schuler D, Dony E, Gaering S, Le Net JL, Okazaki Y, Chabagno JM, Bessibes C, Beausoleil J, Nesslany F, and Régnier JF

Subjects
Aerosols, Animals, Bronchoalveolar Lavage Fluid immunology, DNA Damage, DNA Glycosylases metabolism, Dose-Response Relationship, Drug, Female, Inflammation Mediators immunology, Inflammation Mediators metabolism, Lung immunology, Lung metabolism, Lung pathology, Male, No-Observed-Adverse-Effect Level, Particle Size, Pneumonia immunology, Pneumonia metabolism, Pneumonia pathology, Predictive Value of Tests, Rats, Wistar, Risk Assessment, Time Factors, Comet Assay, Inhalation Exposure adverse effects, Lung drug effects, Micronuclei, Chromosome-Defective chemically induced, Micronucleus Tests, Nanotubes, Carbon toxicity, Pneumonia chemically induced
Abstract

Background: Graphistrength (©) C100 multiwalled carbon nanotubes (MWCNT) provide superior electrical and mechanical properties for various applications. The evaluation of the intrinsic hazard properties of Graphistrength(©) C100 is an essential step for safe use. A general feature of multiwalled carbon nanotubes after inhalation or intratracheal exposures is the induction of an inflammatory reaction in the lungs sometimes associated with local genotoxic effects., Methods: After investigating different parameters for the aerosol generation and performing a 5-day inhalation range finding study, male and female Wistar rats were exposed nose-only for 90 days to target concentrations of 0.05, 0.25 and 5.0 mg/m(3) air of Graphistrength (©) C100 and sacrificed 24 h and 90 days after the last exposure. Broncho-alveolar lavage fluid (BALF) was also collected and analyzed for inflammatory parameters. Twenty-four hours post-exposure, chromosomal aberrations in the bone marrow cells were evaluated by the micronucleus test and DNA damages in the lung, kidney and liver cells by both the standard and the human 8-oxoguanine DNA N-glycosylase 1 (hOGG1)-modified comet assay. All studies were performed according to the OECD test guidelines., Results: An inflammatory lung reaction and the release of inflammatory factors in the BALF were observed in all rats exposed to 5.0 mg/m(3), associated with changes in the differential white blood cells counts. The slight changes in BALF parameters at 0.25 mg/m(3) recovered and signs of lung clearance of the MWCNT were observed. No pathological changes were observed on the pleura. Neither increase in the number of micronucleated polychromatic erythrocytes nor increase in percent DNA damage were observed at any concentration., Conclusions: Lung inflammation characteristic of an overload with insoluble particles was observed after a 90-day exposure to 5.0 mg/m(3) of Graphistrength (©) C100. Clear signs of clearance and recovery were observed at 0.25 mg/m(3). No genotoxicity was detected locally in lung and distally in bone marrow, liver and kidney. Therefore, Graphistrength (©) C100 appears of low concern in term of local and systemic genotoxicity and a No-Observed Adverse Effect Concentration (NOAEC) of 0.25 mg/m(3) (0.28 mg/m(3) as actual concentration) was established for the repeated-dose toxicity.

Published
2015
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