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1. Gas barrier properties of polylactide/cellulose nanocrystals nanocomposites

Author

Hajar Faraj, Nadège Follain, Cyrille Sollogoub, Giana Almeida, Corinne Chappey, Stéphane Marais, Sylvie Tencé-Girault, Fabrice Gouanvé, Eliane Espuche, and Sandra Domenek

Subjects
PLA, CNC, Nanocomposites, Gas barrier properties, Nielsen model, Biocomposites, Polymers and polymer manufacture, TP1080-1185
Abstract

The development of polylactide (PLA)/cellulose nanocrystals (CNC) nanocomposites in the aim to increase gas barrier properties has been widely studied, but gave rise to conflicting results. To better understand the underlying gas transport mechanisms, PLA/CNC nanocomposites were produced at concentrations between 5 and 50 wt%. The role of the PLA/CNC interface for the permeability was investigated using three different CNC surface grafts, namely lauric acid (slightly interacting with PLA), stearic acid (non-interacting with PLA), and poly glycidyl methacrylate bearing a reactive epoxy end-group (crosslinking with PLA). While PLA/CNC composites contained a large number of aggregates, homogenously dispersed nanocomposites were obtained with surface modified CNCs even at high concentration of CNC (up to 30 wt%). All nanocomposites had better O2 and CO2 barrier properties than PLA. Surprisingly, the nanocomposites prepared with surface grafted CNC did not perform better than the ones prepared with neat CNC. The diffusion coefficient was successfully modeled with Nielsen's law, showing the importance of the shape factor and resulting tortuosity for the barrier performance notwithstanding PLA/CNC surface compatibility. The analysis of the dual-mode O2 sorption isotherm showed the creation of a similar quantity of supplementary sorption sites in nanocomposites prepared with neat or lauric acid grafted CNC. PGMA grafts induced a higher number of sorption sites. The most important advantage of CNC surface grafts was the shielding of CNC against water vapor uptake. As a result, the O2 barrier properties could be maintained constant up to 90% relative humidity.

Published
2022
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2. Novel Poly(Vinylidene Fluoride)/Montmorillonite Polymer Inclusion Membrane: Application to Cr(VI) Extraction from Polluted Water

Author

Ferhat Sellami, Ounissa Kebiche-Senhadji, Stéphane Marais, Charles Lanel, and Kateryna Fatyeyeva

Subjects
polymer inclusion membrane, Cr(VI) removal, montmorillonite, membrane rigidity, stability, Chemical technology, TP1-1185, Chemical engineering, TP155-156
Abstract

Novel hybrid polymer inclusion membranes (PIMs) based on poly(vinylidene fluoride) (PVDF) (polymer matrix) and Aliquat 336 (ion carrier) and containing native sodium (Cloisite Na+ (CNa)) and organo-modified (Cloisite 30B (C30B)) Montmorillonites were elaborated and tested for the removal of toxic Cr(VI) ions from the aqueous solution. The influence of the nanoclay incorporation on the physicochemical properties of PVDF-based PIMs was studied and the resulting membrane transport properties of the Cr(VI) ions were investigated in detail. The water contact angle measurements reveal that the incorporation of the CNa nanofiller affects the membrane wettability as less hydrophilic surface is obtained in this case—~47° in the presence of CNa as compared with ~15° for PIMs with C30B. The membrane rigidity is found to be dependent on the type and size of the used Montmorillonite. The increase of Young’s modulus is higher when CNa is incorporated in comparison with C30B. The stiffness of the PIM is strongly increased with CNa amount (four times higher with 30 wt %) which is not the case for C30B (only 1.5 times). Higher Cr(VI) permeation flux is obtained for PIMs containing CNa (~2.7 µmol/(m2·s)) owing to their porous structure as compared with membranes loaded with C30B and those without filler (~2 µmol/(m2·s) in both cases). The PIM with 20 wt % of native sodium Montmorillonite revealed satisfactory stability during five cycles of the Cr(VI) transport due to the high membrane rigidity and hydrophobicity. Much lower macromolecular chain mobility in this case allows limiting the carrier loss, thus increasing the membrane stability. On the contrary, a deterioration of the transport performance is recorded for the membrane filled with C30B and that without filler. The obtained results showed the possibility to extend the PIM lifetime through the incorporation of nanoparticles that diminish the carrier loss (Aliquat 336) from the membrane into the aqueous phase by limiting its mobility within the membrane by tortuosity effect and membrane stiffening without losing its permselective properties.

Published
2021
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3. Structural and Barrier Properties of Compatibilized PE/PA6 Multinanolayer Films

Author

Quentin Lozay, Quentin Beuguel, Nadège Follain, Laurent Lebrun, Alain Guinault, Guillaume Miquelard-Garnier, Sylvie Tencé-Girault, Cyrille Sollogoub, Eric Dargent, and Stéphane Marais

Subjects
PE/PA6 multinanolayer films, barrier properties, forced assembly coextrusion process, interphase, mechanical properties, serial model of diffusion, Chemical technology, TP1-1185, Chemical engineering, TP155-156
Abstract

The barrier performance and structural lightening of organic materials are increasingly desired and constitute a major challenge for manufacturers, particularly for transport and packaging. A promising technique which tends to emerge in recent years is that of multinanolayer coextrusion. The advantage is that it can produce multilayers made of thousands of very thin layers, leading to new properties due to crystalline morphology changes induced by confinement. This paper is focusing on the study of multinanolayered films with alternated polyethylene (PE), compatibilizer (PEgMA) and polyamide 6 (PA6) layers and made by a forced assembly coextrusion process equipped with layer multiplying elements (LME). PE/PA6 multilayer films consisting of 5 to 2049 layers (respectively 0 to 9 LME) were successfully obtained with well-organized multilayered structure. The evolution of the morphology and the microstructure of these two semi-crystalline polymers, when the thickness of each polymer layer decreases from micro-scale to nano-scale, was correlated to the water and gas transport properties of the PE/PA multilayers. The expected improvement of barrier properties was limited due to the on-edge orientation of crystals in very thin PE and PA6 layers. Despite this change of crystalline morphology, a slight improvement of the gas barrier properties was shown by comparing experimental results with permeabilities predicted on the basis of a serial model developed by considering a PE/PA6 interphase. This interphase observed by TEM images and the on-edge crystal orientation in multilayers were evidenced from mechanical properties showing an increase of the stiffness and the strength.

Published
2021
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4. Biodegradable PLA/PBSA Multinanolayer Nanocomposites: Effect of Nanoclays Incorporation in Multinanolayered Structure on Mechanical and Water Barrier Properties

Author

Tiphaine Messin, Nadège Follain, Quentin Lozay, Alain Guinault, Nicolas Delpouve, Jérémie Soulestin, Cyrille Sollogoub, and Stéphane Marais

Subjects
biodegradable polymers, coextrusion, multilayer film, barrier properties, montmorillonite fillers, Chemistry, QD1-999
Abstract

Biodegradable PLA/PBSA multinanolayer nanocomposites were obtained from semi-crystalline poly(butylene succinate-co-butylene adipate) (PBSA) nanolayers filled with nanoclays and confined against amorphous poly(lactic acid) (PLA) nanolayers in a continuous manner by applying an innovative coextrusion technology. The cloisite 30B (C30B) filler incorporation in nanolayers was considered to be an improvement of barrier properties of the multilayer films additional to the confinement effect resulting to forced assembly during the multilayer coextrusion process. 2049-layer films of ~300 µm thick were processed containing loaded PBSA nanolayers of ~200 nm, which presented certain homogeneity and were mostly continuous for the 80/20 wt% PLA/PBSA composition. The nanocomposite PBSA films (monolayer) were also processed for comparison. The presence of exfoliated and intercalated clay structure and some aggregates were observed within the PBSA nanolayers depending on the C30B content. A greater reduction of macromolecular chain segment mobility was measured due to combined effects of confinement effect and clays constraints. The absence of both polymer and clays interdiffusions was highlighted since the PLA glass transition was unchanged. Besides, a larger increase in local chain rigidification was evidenced through RAF values due to geometrical constraints initiated by close nanoclay contact without changing the crystallinity of PBSA. Tortuosity effects into the filled PBSA layers adding to confinement effects induced by PLA layers have caused a significant improvement of water barrier properties through a reduction of water permeability, water vapor solubility and water vapor diffusivity. The obtaining barrier properties were successfully correlated to microstructure, thermal properties and mobility of PBSA amorphous phase.

Published
2020
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5. Polyimide/Ionic Liquid Composite Membranes for Middle and High Temperature Fuel Cell Application: Water Sorption Behavior and Proton Conductivity

Author

Kateryna Fatyeyeva, Sergiy Rogalsky, Stanislav Makhno, Oksana Tarasyuk, Jorge Arturo Soto Puente, and Stéphane Marais

Subjects
porous polyimide membrane, ionic liquid, conductivity, vapour sorption, thermal stability, Chemical technology, TP1-1185, Chemical engineering, TP155-156
Abstract

Four water insoluble room-temperature protic ionic liquids (PILs) based on the N-alkylimidazolium cation with the alkyl chain length from 1 to 4 and bis(trifluoromethylsulfonyl)imide anion were synthesized and their chemical structure was confirmed by the 1H NMR and 19F NMR analysis. PILs were revealed to be thermally stable up to 360 and 400 °C. At the same time, the proton conductivity of PILs was found to be dependent mostly on the temperature and, to a less extent, on the type of the cation, i.e., the increase of the conductivity from ~3 × 10−4 S/cm at 25 °C to 2 × 10−2 S/cm at 150 °C was observed. The water vapour sorption capacity of PILs was evaluated as a function of relative humidity and the influence of the alkyl chain length on the phase behaviour in the PIL-water system was discussed. The composite polyimide/PILs membranes were prepared by the PIL immobilization in the porous polymer (Matrimid® 5218) film. The composite membranes showed a high level of proton conductivity (~10−3 S/cm) at elevated temperatures (up to 160 °C). The obtained results reveal that the elaborated composite polyimide/PIL membranes are promising candidates for the application as proton exchange membrane at middle and high temperatures.

Published
2020
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6. Novel Ionic Conducting Composite Membrane Based on Polymerizable Ionic Liquids

Author

Ghania Azzouz, Corinne Chappey, Kateryna Fatyeyeva, Stéphane Marais, Yaroslav L. Kobzar, Annie-Claude Gaumont, Laurence Lecamp, Isabelle Dez, Hashim Albadri, and Jocelyne Levillain

Subjects
chemistry.chemical_classification, Materials science, Polymers and Plastics, Synthetic membrane, Organic chemistry, Ionic bonding, General Chemistry, Polymer, Electrolyte, Article, fuel cell, chemistry.chemical_compound, QD241-441, Membrane, Chemical engineering, chemistry, Polymerization, Ionic liquid, photopolymerization, Thermal stability, conductivity, polymerizable ionic liquid, polymer membranes
Abstract

In this work, the design and characterization of new supported ionic liquid membranes, as medium-temperature polymer electrolyte membranes for fuel-cell application, are described. These membranes were elaborated by the impregnation of porous polyimide Matrimid® with different synthesized protic ionic liquids containing polymerizable vinyl, allyl, or methacrylate groups. The ionic liquid polymerization was optimized in terms of the nature of the used (photo)initiator, its quantity, and reaction duration. The mechanical and thermal properties, as well as the proton conductivities of the supported ionic liquid membranes were analyzed in dynamic and static modes, as a function of the chemical structure of the protic ionic liquid. The obtained membranes were found to be flexible with Young’s modulus and elongation at break values were equal to 1371 MPa and 271%, respectively. Besides, these membranes exhibited high thermal stability with initial decomposition temperatures &gt, 300 °C. In addition, the resulting supported membranes possessed good proton conductivity over a wide temperature range (from 30 to 150 °C). For example, the three-component Matrimid®/vinylimidazolium/polyvinylimidazolium trifluoromethane sulfonate membrane showed the highest proton conductivity—~5 × 10−2 mS/cm and ~0.1 mS/cm at 100 °C and 150 °C, respectively. This result makes the obtained membranes attractive for medium-temperature fuel-cell application.

Published
2021

7. Novel Poly(Vinylidene Fluoride)/Montmorillonite Polymer Inclusion Membrane: Application to Cr(VI) Extraction from Polluted Water

Author

Kateryna Fatyeyeva, Charles Lanel, Ferhat Sellami, Stéphane Marais, and Ounissa Kebiche-Senhadji

Subjects
Aqueous solution, membrane rigidity, Process Chemistry and Technology, Chemical technology, Aqueous two-phase system, Filtration and Separation, montmorillonite, TP1-1185, Aliquat 336, Membrane transport, Permeation, stability, Article, polymer inclusion membrane, chemistry.chemical_compound, Membrane, Montmorillonite, Chemical engineering, chemistry, Chemical Engineering (miscellaneous), TP155-156, Fluoride, Cr(VI) removal
Abstract

Novel hybrid polymer inclusion membranes (PIMs) based on poly(vinylidene fluoride) (PVDF) (polymer matrix) and Aliquat 336 (ion carrier) and containing native sodium (Cloisite Na+ (CNa)) and organo-modified (Cloisite 30B (C30B)) Montmorillonites were elaborated and tested for the removal of toxic Cr(VI) ions from the aqueous solution. The influence of the nanoclay incorporation on the physicochemical properties of PVDF-based PIMs was studied and the resulting membrane transport properties of the Cr(VI) ions were investigated in detail. The water contact angle measurements reveal that the incorporation of the CNa nanofiller affects the membrane wettability as less hydrophilic surface is obtained in this case—~47° in the presence of CNa as compared with ~15° for PIMs with C30B. The membrane rigidity is found to be dependent on the type and size of the used Montmorillonite. The increase of Young’s modulus is higher when CNa is incorporated in comparison with C30B. The stiffness of the PIM is strongly increased with CNa amount (four times higher with 30 wt %) which is not the case for C30B (only 1.5 times). Higher Cr(VI) permeation flux is obtained for PIMs containing CNa (~2.7 µmol/(m2·s)) owing to their porous structure as compared with membranes loaded with C30B and those without filler (~2 µmol/(m2·s) in both cases). The PIM with 20 wt % of native sodium Montmorillonite revealed satisfactory stability during five cycles of the Cr(VI) transport due to the high membrane rigidity and hydrophobicity. Much lower macromolecular chain mobility in this case allows limiting the carrier loss, thus increasing the membrane stability. On the contrary, a deterioration of the transport performance is recorded for the membrane filled with C30B and that without filler. The obtained results showed the possibility to extend the PIM lifetime through the incorporation of nanoparticles that diminish the carrier loss (Aliquat 336) from the membrane into the aqueous phase by limiting its mobility within the membrane by tortuosity effect and membrane stiffening without losing its permselective properties.

Published
2021

8. Structural and Barrier Properties of Compatibilized PE/PA6 Multinanolayer Films

Author

Sylvie Tencé-Girault, Quentin Beuguel, Quentin Lozay, Nadège Follain, Cyrille Sollogoub, Laurent Lebrun, Guillaume Miquelard-Garnier, Stéphane Marais, Alain Guinault, Eric Dargent, Polymères Biopolymères Surfaces (PBS), Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Groupe de physique des matériaux (GPM), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche sur les Matériaux Avancés (IRMA), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Rouen Normandie (UNIROUEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-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), ANR-16-CE08-0035,IMMUNE,Matériaux Innovants par procédé d'extrusion multi-nanocouches(2016), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Polymères, biopolymères, membranes (PBM), Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), and Normandie Université (NU)

Subjects
Morphology (linguistics), Materials science, barrier properties, Filtration and Separation, 02 engineering and technology, mechanical properties, Sciences de l'ingénieur, lcsh:Chemical technology, 010402 general chemistry, 01 natural sciences, Article, chemistry.chemical_compound, [CHIM]Chemical Sciences, Chemical Engineering (miscellaneous), General Materials Science, lcsh:TP1-1185, lcsh:Chemical engineering, Composite material, ComputingMilieux_MISCELLANEOUS, PE/PA6 multinanolayer films, chemistry.chemical_classification, Thin layers, Process Chemistry and Technology, lcsh:TP155-156, forced assembly coextrusion process, [CHIM.MATE]Chemical Sciences/Material chemistry, Polymer, Polyethylene, interphase, 021001 nanoscience & nanotechnology, Microstructure, 0104 chemical sciences, serial model of diffusion, [CHIM.POLY]Chemical Sciences/Polymers, chemistry, Polyamide, Interphase, 0210 nano-technology, Layer (electronics)
Abstract

The barrier performance and structural lightening of organic materials are increasingly desired and constitute a major challenge for manufacturers, particularly for transport and packaging. A promising technique which tends to emerge in recent years is that of multinanolayer coextrusion. The advantage is that it can produce multilayers made of thousands of very thin layers, leading to new properties due to crystalline morphology changes induced by confinement. This paper is focusing on the study of multinanolayered films with alternated polyethylene (PE), compatibilizer (PEgMA) and polyamide 6 (PA6) layers and made by a forced assembly coextrusion process equipped with layer multiplying elements (LME). PE/PA6 multilayer films consisting of 5 to 2049 layers (respectively 0 to 9 LME) were successfully obtained with well-organized multilayered structure. The evolution of the morphology and the microstructure of these two semi-crystalline polymers, when the thickness of each polymer layer decreases from micro-scale to nano-scale, was correlated to the water and gas transport properties of the PE/PA multilayers. The expected improvement of barrier properties was limited due to the on-edge orientation of crystals in very thin PE and PA6 layers. Despite this change of crystalline morphology, a slight improvement of the gas barrier properties was shown by comparing experimental results with permeabilities predicted on the basis of a serial model developed by considering a PE/PA6 interphase. This interphase observed by TEM images and the on-edge crystal orientation in multilayers were evidenced from mechanical properties showing an increase of the stiffness and the strength.

Published
2021
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9. Biodegradable PLA/PBSA Multinanolayer Nanocomposites: Effect of Nanoclays Incorporation in Multinanolayered Structure on Mechanical and Water Barrier Properties

Author

Nadège Follain, Jérémie Soulestin, Tiphaine Messin, Nicolas Delpouve, Alain Guinault, Stéphane Marais, Cyrille Sollogoub, Quentin Lozay, Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Polymères, biopolymères, membranes (PBM), Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU), Université de Rouen Normandie (UNIROUEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-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), Groupe de physique des matériaux (GPM), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche sur les Matériaux Avancés (IRMA), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Rouen Normandie (UNIROUEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Département Technologie des Polymères et Composites & Ingénierie Mécanique (TPCIM), École des Mines de Douai (Mines Douai EMD), and Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT)-Ministère de l'Économie, des Finances et de l'Industrie [Paris, France]

Subjects
Materials science, General Chemical Engineering, barrier properties, 02 engineering and technology, coextrusion, 010402 general chemistry, 01 natural sciences, Article, lcsh:Chemistry, Crystallinity, montmorillonite fillers, Monolayer, [CHIM]Chemical Sciences, General Materials Science, ComputingMilieux_MISCELLANEOUS, chemistry.chemical_classification, Nanocomposite, Polymer, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Microstructure, Biodegradable polymer, 0104 chemical sciences, Amorphous solid, [CHIM.POLY]Chemical Sciences/Polymers, Chemical engineering, chemistry, lcsh:QD1-999, biodegradable polymers, multilayer film, 0210 nano-technology, Glass transition
Abstract

Biodegradable PLA/PBSA multinanolayer nanocomposites were obtained from semi-crystalline poly(butylene succinate-co-butylene adipate) (PBSA) nanolayers filled with nanoclays and confined against amorphous poly(lactic acid) (PLA) nanolayers in a continuous manner by applying an innovative coextrusion technology. The cloisite 30B (C30B) filler incorporation in nanolayers was considered to be an improvement of barrier properties of the multilayer films additional to the confinement effect resulting to forced assembly during the multilayer coextrusion process. 2049-layer films of ~300 &micro, m thick were processed containing loaded PBSA nanolayers of ~200 nm, which presented certain homogeneity and were mostly continuous for the 80/20 wt% PLA/PBSA composition. The nanocomposite PBSA films (monolayer) were also processed for comparison. The presence of exfoliated and intercalated clay structure and some aggregates were observed within the PBSA nanolayers depending on the C30B content. A greater reduction of macromolecular chain segment mobility was measured due to combined effects of confinement effect and clays constraints. The absence of both polymer and clays interdiffusions was highlighted since the PLA glass transition was unchanged. Besides, a larger increase in local chain rigidification was evidenced through RAF values due to geometrical constraints initiated by close nanoclay contact without changing the crystallinity of PBSA. Tortuosity effects into the filled PBSA layers adding to confinement effects induced by PLA layers have caused a significant improvement of water barrier properties through a reduction of water permeability, water vapor solubility and water vapor diffusivity. The obtaining barrier properties were successfully correlated to microstructure, thermal properties and mobility of PBSA amorphous phase.

Published
2020
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10. The Impact of Reactive Ionic Liquids Addition on the Physicochemical and Sorption Properties of Poly(Vinyl Alcohol)-Based Films

Author

Guoqiang Li, Kateryna Fatyeyeva, Zbigniew Rafiński, Stéphane Marais, Joanna Kujawa, Andrzej Wolan, Krzysztof Dzieszkowski, Corinne Chappey, Edyta Rynkowska, and Wojciech Kujawski

Subjects
sorption kinetics, Vinyl alcohol, Thermogravimetric analysis, Materials science, Polymers and Plastics, Synthetic membrane, Sorption, General Chemistry, Article, poly(vinyl alcohol), lcsh:QD241-441, chemistry.chemical_compound, Membrane, lcsh:Organic chemistry, chemistry, Chemical engineering, Bromide, Ionic liquid, Fourier transform infrared spectroscopy, reactive ionic liquids, polymer membranes
Abstract

A new type of hybrid polymeric-based film containing 1-(1,3-diethoxy-1,3-dioxopropan-2-ylo)-3-methylimidazolium bromide (RIL1_Br) and 1-(2-etoxy-2-oxoethyl)-3-methylimidazolium bromide (RIL2_Br) reactive ionic liquids was elaborated. Poly(vinyl alcohol) (PVA)-based films with 9–33 wt % of RILs were subsequently characterized using Fourier transform infrared spectroscopy with attenuated total reflectance (FTIR-ATR), scanning electron microscopy (SEM), atomic force microscopy (AFM), thermogravimetric analysis (TGA) and TGA-FTIR. PVA-RIL films were also studied in tensile tests, contact angle and sorption measurements. RIL incorporation enhanced thermal and mechanical stability of PVA membranes due to the hydrogen bonds between RILs and polymer chains. Membrane swelling behavior in water (H2O), ethanol (EtOH), and propan-2-ol (IPA) and the kinetics of water sorption process revealed that PVA-RILs membranes possess the highest affinity towards water. It was pointed out that both the RIL type and the RIL amount in the polymer matrix have significant influence on the membrane swelling behavior and the water sorption kinetics.

Published
2020

11. Polyimide/Ionic Liquid Composite Membranes for Middle and High Temperature Fuel Cell Application: Water Sorption Behavior and Proton Conductivity

Author

Sergiy Rogalsky, Jorge Arturo Soto Puente, Kateryna Fatyeyeva, Stanislav Makhno, Oksana Tarasyuk, and Stéphane Marais

Subjects
Materials science, Proton exchange membrane fuel cell, Filtration and Separation, 02 engineering and technology, Conductivity, 010402 general chemistry, lcsh:Chemical technology, 01 natural sciences, Article, thermal stability, chemistry.chemical_compound, Chemical Engineering (miscellaneous), Thermal stability, porous polyimide membrane, lcsh:TP1-1185, lcsh:Chemical engineering, Alkyl, ionic liquid, vapour sorption, chemistry.chemical_classification, Process Chemistry and Technology, lcsh:TP155-156, Sorption, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Membrane, Chemical engineering, chemistry, Ionic liquid, conductivity, 0210 nano-technology, Polyimide
Abstract

Four water insoluble room-temperature protic ionic liquids (PILs) based on the N-alkylimidazolium cation with the alkyl chain length from 1 to 4 and bis(trifluoromethylsulfonyl)imide anion were synthesized and their chemical structure was confirmed by the 1H NMR and 19F NMR analysis. PILs were revealed to be thermally stable up to 360 and 400 &deg, C. At the same time, the proton conductivity of PILs was found to be dependent mostly on the temperature and, to a less extent, on the type of the cation, i.e., the increase of the conductivity from ~3 &times, 10&minus, 4 S/cm at 25 &deg, C to 2 &times, 2 S/cm at 150 &deg, C was observed. The water vapour sorption capacity of PILs was evaluated as a function of relative humidity and the influence of the alkyl chain length on the phase behaviour in the PIL-water system was discussed. The composite polyimide/PILs membranes were prepared by the PIL immobilization in the porous polymer (Matrimid&reg, 5218) film. The composite membranes showed a high level of proton conductivity (~10&minus, 3 S/cm) at elevated temperatures (up to 160 &deg, C). The obtained results reveal that the elaborated composite polyimide/PIL membranes are promising candidates for the application as proton exchange membrane at middle and high temperatures.

Published
2020

12. Imidazolium-based protic ionic liquids with perfluorinated anions: Influence of chemical structure on thermal properties

Author

Kateryna Fatyeyeva, Ya. L. Kobzar, A. Martin, Stéphane Marais, H. Oulyadi, and Y. Prykhodko

Subjects
chemistry.chemical_classification, Thermogravimetric analysis, Chemistry, Chemical structure, Condensed Matter Physics, Atomic and Molecular Physics, and Optics, Electronic, Optical and Magnetic Materials, chemistry.chemical_compound, Differential scanning calorimetry, Polymer chemistry, Ionic liquid, Materials Chemistry, Side chain, Thermal stability, Physical and Theoretical Chemistry, Fourier transform infrared spectroscopy, Spectroscopy, Alkyl
Abstract

The influence of the cation chemical structure, namely its side chain, on the thermal properties of imidazolium-based protic ionic liquids (PILs) with different perfluorinated anions (trifluoromethanesulfonimide (TFSI), trifluoromethanesulfonic (TFS), and trifluoroacetic (TFA) acids) was studied. With that purpose, twenty-one PILs with various alkyl (methyl-, ethyl-, butyl- and vinyl-) and fluorinated (-CH2CF3, -CH2CHF2, and -CH2CH2F) side chains were successfully synthesized. Special attention was paid to an optimization of their synthesis conditions. The structure of synthesized fluorinated and alkyl-substituted PILs was confirmed by means of nuclear magnetic resonance (NMR) analysis (1D: 1H, 19F, 13C and 2D: 1H – 19F HOESY experiments) and Fourier transform infrared (FTIR) spectroscopy, while PILs thermal behavior was determined by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) in dynamic and isothermal modes. The correlation between the PILs chemical structure and their thermal stability was established. It has been found that an increase of the length of alkyl side chain (methyl

Published
2022
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13. New ionic liquid-based polyoxadiazole electrolytes for hydrogen middle- and high-temperature fuel cells

Author

Ye.V. Lobko, Yu.V. Yakovlev, Ya. L. Kobzar, T. Hrbek, Stéphane Marais, and Kateryna Fatyeyeva

Subjects
chemistry.chemical_classification, Materials science, Polyvinylpyrrolidone, Hydrogen, chemistry.chemical_element, Filtration and Separation, Polymer, Electrolyte, Atmospheric temperature range, Biochemistry, chemistry.chemical_compound, Membrane, chemistry, Chemical engineering, Ionic liquid, medicine, General Materials Science, Thermal stability, Physical and Theoretical Chemistry, medicine.drug
Abstract

New polyoxadiazole-based supported ionic liquid membranes were designed and elaborated for the first time to be used as a middle- and high-temperature polymer electrolyte membrane for fuel cell application. The proposed membrane molecular design combined hydroxyl-functionalized sulfonated polyoxadiazole, hydrophilic polyvinylpyrrolidone and specific protic ionic liquid, thus allowing elaboration of membranes with remarkable physical-chemical characteristics. It is found that the fine tuning of the membranes properties is possible by varying the ratio of polyoxadiazole and polyvinylpyrrolidone. The obtained membranes reveal high thermal stability in dynamic and static modes (up to 350 °C), good oxidative stability, sufficient mechanical properties (Young's modulus of 0.3–21.4 MPa and elongation at break from of 6 to 174%), high degree of ionic liquid impregnation (up to 297%), stable and relatively high conductivity (up to 1.3 mS∙cm−1) in a wide temperature range (from 40 to 120 °С) and under dry conditions. All these properties make the elaborated membranes very attractive for middle- and high-temperature fuel cell application.

Published
2021
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14. Physicochemical properties and pervaporation performance of dense membranes based on cellulose acetate propionate (CAP) and containing polymerizable ionic liquid (PIL)

Author

Stéphane Marais, Edyta Rynkowska, Andrzej Wolan, Antoine Lancien, Krzysztof Dzieszkowski, Kateryna Fatyeyeva, Anthony Szymczyk, Joanna Kujawa, Wojciech Kujawski, Stanisław Koter, Nicolaus Copernicus University [Toruń], Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Institut des Sciences Chimiques de Rennes (ISCR), Université de Rennes 1 (UR1), Université de Rennes (UNIV-RENNES)-Université de Rennes (UNIV-RENNES)-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)-Ecole Nationale Supérieure de Chimie de Rennes (ENSCR)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), DEC-2015/18/M/ST5/00635, NCN, Narodowe Centrum Nauki, Université de Rouen Normandie (UNIROUEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Université de Rennes (UR)-Institut National des Sciences Appliquées - Rennes (INSA Rennes), and 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)

Subjects
Filtration and Separation, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Biochemistry, Cellulose acetate propionate, chemistry.chemical_compound, medicine, [CHIM]Chemical Sciences, Organic chemistry, General Materials Science, Physical and Theoretical Chemistry, Plasticization, Plasticizer, Polymerizable ionic liquids, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Hildebrand solubility parameter, Monomer, Membrane, Hydrophilic pervaporation, chemistry, Chemical engineering, Ionic liquid, Pervaporation, Swelling, medicine.symptom, 0210 nano-technology, Hybrid material, Hansen's solubility parameters
Abstract

International audience; The new type of efficient pervaporative separation hybrid materials based on cellulose acetate propionate (CAP) and doped with 1-methyl-3-(4-vinylbenzyl)-1H-imidazol-3-ium chloride polymerizable ionic liquid (PIL) monomers (12.3–44.4 wt%) were elaborated for dehydration of propan-2-ol. Broad material and physicochemical characterization of membranes was performed including assessment of physicochemical, equilibrium, transport, and separation properties. Incorporation of PIL results in the plasticization of CAP based membranes. Additionally, with increasing loading of PIL from 12.3 to 44.4 wt% values of thickness-normalized Pervaporation Separation Index (PSIN) increase 1.6–2.4 times comparing to unloaded membrane (pure CAP). The distance parameters calculated on the base of the Hansen's solubility parameters were additionally employed to interpret swelling and pervaporative properties of membranes as well as to discuss interactions between solvents and prepared membranes. Lower value of distance parameter between pristine CAP and ethanol corresponds to the highest molar swelling degree of CAP based membranes. Swelling of CAP-PIL membranes in contact with water, ethanol, and propan-2-ol increased with of the increasing PIL content due to the hydrophilic character of ionic liquid. The gathered data provided insight into the potential applicability of the novel hybrid separation materials for pervaporative separation of liquid-liquid mixtures. © 2017 Elsevier B.V.

Published
2017
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15. How the chemical structure of the plasma-deposited SiOx film modifies its stability and barrier properties: FTIR study

Author

Thanh Hien Tran, Fabienne Poncin-Epaillard, Stéphane Marais, Dominique Debarnot, D.B. Au, Bassidi Diawara, J. Ortiz, Kateryna Fatyeyeva, Institut des Molécules et Matériaux du Mans (IMMM), Le Mans Université (UM)-Centre National de la Recherche Scientifique (CNRS), Le Mans Université (UM)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), and Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)

Subjects
Materials science, General Chemical Engineering, PECVD, 02 engineering and technology, Substrate (electronics), engineering.material, 010402 general chemistry, 01 natural sciences, Coating, X-ray photoelectron spectroscopy, Materials Chemistry, inorganic silicon, [CHIM]Chemical Sciences, Fourier transform infrared spectroscopy, Thin film, Polycarbonate, ComputingMilieux_MISCELLANEOUS, density, Organic Chemistry, [CHIM.MATE]Chemical Sciences/Material chemistry, Permeation, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Surfaces, Coatings and Films, [CHIM.POLY]Chemical Sciences/Polymers, Chemical engineering, visual_art, engineering, visual_art.visual_art_medium, permeation, Wetting, 0210 nano-technology, fluorinated silicon
Abstract

Organosilicon thin films issued from the gas mixture of oxygen and hexamethyledisiloxane (HMDSO), 2,4,6,8-tetramethylcyclotetrasiloxane (TMCTS), or fluorotriethoxysilane (FTEOS) deposited on polycarbonate (PC) substrate were obtained thanks to a RF plasma source. The chemical structure of the two types of inorganic SiOx (HMDSO/O2, TMCTS/O2) and fluorinated SiOxCyFz (FTEOS/O2, FTEOS/O2/TMCTS) coatings have been investigated by FTIR and XPS spectroscopies, and wettability measurement. Network structure and density of SiOx and SiOxCyFz thin films were discussed as a function of the νSiOSi band shifting observed in their respective FTIR spectra. The influence of various plasma parameters (such as discharge power, precursor/O2 ratio and, duration) on the film properties was studied in order to optimize the growth of both inorganic and fluorinated thin films. The ageing of such layers either at ambient atmosphere or even at reduced pressure showed a chemical alteration of the thin films surface and bulk, which stabilized after 15 days of storage. Such phenomenon is explained by the hydrophobicity recovery that may induce the observed network alteration. Water and oxygen permeation and transport properties of treated PC films were correlated with the coating structure and composition; then TMCTS was identified as the most efficient precursor for enhancing water barrier property. Furthermore, the permeation properties of these deposits seem to be more controlled by the material density than by their chemistry.

Published
2019
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16. Evolution of mechanical and barrier properties of thermally aged polycarbonate films

Author

Bassidi Diawara, José Ortiz, Corinne Chappey, Kateryna Fatyeyeva, Laurent Colasse, Stéphane Marais, Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), and Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Filtration and Separation, 02 engineering and technology, Thermal treatment, 010402 general chemistry, 01 natural sciences, Biochemistry, Contact angle, Ultimate tensile strength, General Materials Science, Physical and Theoretical Chemistry, Composite material, Polycarbonate, ComputingMilieux_MISCELLANEOUS, Relaxation (NMR), [CHIM.MATE]Chemical Sciences/Material chemistry, Permeation, 021001 nanoscience & nanotechnology, 0104 chemical sciences, [CHIM.THEO]Chemical Sciences/Theoretical and/or physical chemistry, [CHIM.POLY]Chemical Sciences/Polymers, Volume (thermodynamics), visual_art, visual_art.visual_art_medium, 0210 nano-technology, Glass transition
Abstract

Polycarbonate (PC) films of two different grades (Macrolon® LED 2245 and Macrolon® AL 2447) were elaborated and thermally aged at 100, 120 and 140 °C during intermediate and long times of aging. The physical aging effect on the film properties was analyzed by infrared spectroscopy, water contact angle, thermal and tensile tests, and water and gas permeation and sorption measurements. The effect of thermal treatment on PC properties was revealed, especially for the film aged at 120 °C. Aging caused a continual increase of PC glass transition temperature and relaxation enthalpy, an increase in Young's modulus and yield strength values and a decrease in the elongation at break. These results were attributed to the reduction of the free volume because of the PC conformational changes. The film barrier properties using liquid water and gas (N2, O2 and CO2) molecules as probes were studied in order to highlight the free volume evolution. It was shown that physical aging caused a reduction of water and gas permeability. This fact was mainly explained by the decrease of the solubility coefficient with the aging time increase.

Published
2019
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17. Chemically and Thermally Crosslinked PVA-Based Membranes: Effect on Swelling and Transport Behavior

Author

Wojciech Kujawski, Joanna Kujawa, Stéphane Marais, Kateryna Fatyeyeva, and Edyta Rynkowska

Subjects
Vinyl alcohol, Polymers and Plastics, Synthetic membrane, Alcohol, macromolecular substances, Thermal treatment, contact angle measurements, Article, lcsh:QD241-441, chemistry.chemical_compound, lcsh:Organic chemistry, medicine, Dehydration, sulfosuccinic acid, technology, industry, and agriculture, General Chemistry, medicine.disease, water permeation, poly(vinyl alcohol), Membrane, Chemical engineering, chemistry, Methanol, Swelling, medicine.symptom, chemical and thermal crosslinking
Abstract

The novel poly(vinyl alcohol) (PVA)-based membranes were prepared using the two-step crosslinking approach: the chemical crosslinking of PVA using sulfosuccinic acid (SSA) (0&ndash, 50 wt.%) and the thermal treatment (120&ndash, 160 &deg, C). The membrane composition and crosslinking temperature were optimized in terms of the mechanical and transport properties. The FTIR-ATR analysis revealed that the increase of the SSA concentration and crosslinking temperature resulted in the rise of the ester bond bands intensity due to the esterification reaction between PVA and SSA. As a consequence, the PVA-based membrane with 50 wt % SSA and crosslinked at 140 &deg, C showed the reduced Young&rsquo, s modulus (from 1266.2 MPa to 1.4 MPa) and elongation at break (from 316% to 66%) in comparison with the pure PVA membrane. The studied swelling behavior of the obtained membranes revealed significantly higher water sorption than that in methanol and propal-2-ol whatever the crosslinking temperature. The performed studies provide a new way of tailoring the membrane physicochemical properties, in particular, the surface hydrophilicity. In addition, the obtained results are crucial for the design and elaboration of the polymer membranes for the pervaporative separation of the liquid-liquid mixtures, in particular, for the alcohol dehydration.

Published
2019
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18. Water molecular state in 1-hexylpyridinium hexafluorophosphate: Water mean cluster size as a function of water concentration

Author

Dominique Langevin, Stéphane Marais, Kateryna Fatyeyeva, Corinne Chappey, Abdellatif Dahi, Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), and Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Tetrafluoroborate, Water activity, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, chemistry.chemical_compound, Hexafluorophosphate, Materials Chemistry, Physical and Theoretical Chemistry, Spectroscopy, ComputingMilieux_MISCELLANEOUS, Hydrogen bond, Sorption, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Condensed Matter Physics, 6. Clean water, Atomic and Molecular Physics, and Optics, 0104 chemical sciences, Electronic, Optical and Magnetic Materials, [CHIM.POLY]Chemical Sciences/Polymers, chemistry, Ionic liquid, Gravimetric analysis, Physical chemistry, Pyridinium, 0210 nano-technology
Abstract

The water sorption behavior of representative pyridinium-based ionic liquid (IL), 1-hexylpyridinium hexafluorophosphate ([C6Py][PF6]), was studied over the whole range of the water activity a using a continuous gravimetric method. The analysis of the water sorption isotherm using the combination of a two-mode sorption (i.e. Henry-clustering) allowed to better understand [C6Py][PF6]-water interactions. At low and intermediate activity (a ≤ 0.8), the water molecules revealed a very low affinity to [C6Py][PF6] and, consequently, the water uptake was rather low. On the contrary, at high water activity (a > 0.8), the water uptake increased exponentially and the water clustering easily occurred. The constant of the Henry-clustering equation as well as the water clustering mechanism in [C6Py][PF6] were discussed and compared to those of imidazolium-based ILs: 1-hexyl-3-methylimidazolium hexafluorophosphate [C6C1im][PF6] (water-immiscible IL) and 1-butyl-3-methylimidazolium tetrafluoroborate [C4C1im][BF4] (water-miscible IL). It is shown that the sorption of water molecules by pyridinium-based ILs is controlled not only by the anion's nature, but also by the cation's nature. Moreover, the Zimm-Lundberg theory was used to determine the water mean cluster size (MCS) in [C6Py][PF6], [C6C1im][PF6] and [C4C1im][BF4]. The MCS results confirmed the strong capacity of water molecules to be aggregated in [C6Py][PF6]. In order to have a deeper insight into the water molecular state, infrared spectroscopy measurements were carried out as a function of the relative humidity value and the obtained results were correlated with the results of water sorption isotherms. It is found that at high water activity (a > 0.8), sorbed water molecules are strongly linked with ILs by hydrogen bonds and, therefore, are easily aggregated.

Published
2019
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19. Polymer inclusion membranes based on CTA/PBAT blend containing Aliquat 336 as extractant for removal of Cr(VI): Efficiency, stability and selectivity

Author

Stéphane Marais, Ferhat Sellami, Nicolas Couvrat, Kateryna Fatyeyeva, Ounissa Kebiche-Senhadji, Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Laboratoire de procédés membranaires et de technique de séparation et de récupération (LPMSTR), Université A. Mira de Bejaia, Targa Ouzemmour 06000, Bejaia, Algeria, Sciences et Méthodes Séparatives (SMS), Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Normandie Université (NU), and Collaboration

Subjects
Polymers and Plastics, General Chemical Engineering, 02 engineering and technology, Aliquat 336, 010402 general chemistry, 01 natural sciences, Biochemistry, Chloride, Contact angle, chemistry.chemical_compound, Materials Chemistry, medicine, Environmental Chemistry, ComputingMilieux_MISCELLANEOUS, chemistry.chemical_classification, Chemistry, General Chemistry, Polymer, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Cellulose triacetate, Membrane, [CHIM.POLY]Chemical Sciences/Polymers, Ionic liquid, 0210 nano-technology, Selectivity, Nuclear chemistry, medicine.drug
Abstract

Cellulose triacetate (CTA) and poly(butylene adipate-co-terephthalate) (PBAT)-based polymer inclusion membranes (PIMs) containing ionic liquid (tricaprylmethylammonium chloride (Aliquat 336)) as the carrier extractant were obtained for the facilitated and selective transport of Cr(VI) ions. The composition of PIMs was optimized in terms of the CTA/PBAT ratio. The obtained membranes were investigated using different techniques in order to show the influence of the membrane composition and the ionic liquid presence on the PIM resulting properties. The infrared analysis confirmed the presence of the intermolecular interactions of the hydroxyl groups of CTA with the carboxyl groups of PBAT and of the negatively charged carboxyl groups of CTA with the positively charged ammonium groups of Aliquat 336. The water contact angle measurements highlighted that the Aliquat 336 and PBAT presence modified the membrane hydrophobic/hydrophilic character. Moreover, it was shown that PIM containing the equivalent content of CTA and PBAT (35/35 wt%/wt%) with 30 wt% of Aliquat 336 revealed the optimized composition and was used for the Cr(VI) ions transport measurements. It was found that this PIM transported >99% of Cr(VI) in only 6 h and accumulated 120 h).

Published
2019
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20. Impact of water and thermal induced crystallizations in a PC/MXD6 multilayer film on barrier properties

Author

Cyrille Sollogoub, Valerie Gaucher, Nicolas Delpouve, Nadège Follain, Guillaume Miquelard-Garnier, Tiphaine Messin, Corinne Chappey, Stéphane Marais, Alain Guinault, Polymères Biopolymères Surfaces (PBS), Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), Isolement, structure, transformations et synthèse de substances naturelles (ISTSSN), Université de Reims Champagne-Ardenne (URCA)-Centre National de la Recherche Scientifique (CNRS), Procédés et Ingénierie en Mécanique et Matériaux [Paris] (PIMM), Conservatoire National des Arts et Métiers [CNAM] (CNAM)-École Nationale Supérieure d'Arts et Métiers (ENSAM), Arts et Métiers Sciences et Technologies, HESAM Université (HESAM)-HESAM Université (HESAM)-Arts et Métiers Sciences et Technologies, HESAM Université (HESAM)-HESAM Université (HESAM)-Centre National de la Recherche Scientifique (CNRS), Groupe de physique des matériaux (GPM), Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU), Unité Matériaux et Transformations - UMR 8207 (UMET), Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut National de la Recherche Agronomique (INRA), École Nationale Supérieure d'Arts et Métiers (ENSAM), HESAM Université (HESAM)-HESAM Université (HESAM)-Centre National de la Recherche Scientifique (CNRS)-Conservatoire National des Arts et Métiers [CNAM] (CNAM), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-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), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche sur les Matériaux Avancés (IRMA), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Rouen Normandie (UNIROUEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Conservatoire National des Arts et Métiers [CNAM] (CNAM)-Arts et Métiers Sciences et Technologies, HESAM Université (HESAM)-HESAM Université (HESAM), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), and Institut de Chimie du CNRS (INC)-Institut National de la Recherche Agronomique (INRA)-Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)

Subjects
Materials science, Polymers and Plastics, General Physics and Astronomy, chemistry.chemical_element, 02 engineering and technology, Adipamide, Sciences de l'ingénieur, 010402 general chemistry, 01 natural sciences, Oxygen, law.invention, Crystallinity, chemistry.chemical_compound, [SPI]Engineering Sciences [physics], law, Thermal, Materials Chemistry, Crystallization, Composite material, Polycarbonate, Organic Chemistry, 021001 nanoscience & nanotechnology, Nitrogen, 0104 chemical sciences, chemistry, 13. Climate action, visual_art, visual_art.visual_art_medium, Water of crystallization, 0210 nano-technology
Abstract

International audience; A multilayer film composed of alternating layers of polycarbonate (PC) and poly(m-xylene adipamide) (MXD6) was elaborated by using an innovative multilayer coextrusion process. Quasi-continuous thin MXD6 layers (nanolayers) alternating with PC layers were successfully obtained. The PC/MXD6 multilayer film showed a confining effect of MXD6 exerted by PC layers leading to an improvement of barrier properties despite a low degree of crystallinity (X c < 10 wt%). In order to further improve the barrier performances, crystallization treatments induced by water and by heating were then applied on the multilayer film and allowed reaching around 30 wt% of crystallinity in MXD6 layers. To decouple crystallization and geometrical constraint effects on the barrier properties in the multilayer films, the two treatments were also applied on MXD6 films. Surprisingly, despite an increase of the degree of crystallinity from 6 to 26%, water crystallization did not permit to improve gas barrier performances of the MXD6 film nor into the PC/MXD6 multilayer film. On the other hand, thermal crystallization of MXD6 in the multilayer film seems to be a more efficient route to strongly decrease the gas and moisture permeability, up to 75% for nitrogen, 58% for oxygen, 84% for carbon dioxide and 43% for water.

Published
2019
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21. Dimethylketene-based aliphatic polyketones: Copolymers and star-shaped polymers potentially useful in food packaging

Author

Fabrice Burel, Stéphane Marais, Hanbin Wang, Nadège Follain, Nicolas Desilles, Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), and Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)

Subjects
chemistry.chemical_classification, Materials science, Polymers and Plastics, Organic Chemistry, Cationic polymerization, General Physics and Astronomy, 02 engineering and technology, Polymer, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, Food packaging, Oxygen permeability, [CHIM.POLY]Chemical Sciences/Polymers, chemistry, Polyketone, Polymer chemistry, Materials Chemistry, Copolymer, Degradation (geology), Fourier transform infrared spectroscopy, 0210 nano-technology, ComputingMilieux_MISCELLANEOUS
Abstract

This paper aims to design new aliphatic polyketones based on dimethylketene, by cationic polymerization. Previous works showed that the polyketone type of polydimethylketene presents excellent oxygen barrier properties even in the presence of humidity, enabling this material to compete with the polymers currently used in the food packaging industry. However, PDMK has a degradation temperature close to its melting temperature which may make processability uneasy. PDMK structure is thus modified to broaden the gap between these two temperatures: for the first time, a dimethylketene/ethylketene random copolymer and a star-shaped polydimethylketene are targeted by cationic polymerization. The obtained polymers are studied by 1H and 13C NMR, FTIR, and capillary viscosimetry, the thermal properties are more particularly analyzed by TGA and DSC, and the oxygen permeability is measured.

Published
2016
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22. Effect of the polar–nonpolar liquid mixtures on pervaporative behavior of perfluorinated sulfonic membranes in lithium form

Author

Edyta Rynkowska, Wojciech Kujawski, Joanna Kujawa, Anne-Marie Kelterer, Larisa Karpenko-Jereb, Kateryna Fatyeyeva, Stéphane Marais, Corinne Chappey, Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Nicolaus Copernicus University, Faculty of Chemistry, Nicolaus Copernicus University [Toruń], and Graz University of Technology [Graz] (TU Graz)

Subjects
Methyl acetate, Analytical chemistry, Solvation, Filtration and Separation, [CHIM.MATE]Chemical Sciences/Material chemistry, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Biochemistry, Dissociation (chemistry), 0104 chemical sciences, chemistry.chemical_compound, [CHIM.POLY]Chemical Sciences/Polymers, Membrane, chemistry, Nafion, Organic chemistry, General Materials Science, Pervaporation, Methanol, Physical and Theoretical Chemistry, Dimethyl carbonate, 0210 nano-technology, ComputingMilieux_MISCELLANEOUS
Abstract

Two ion-exchange membranes possessing perfluorinated backbone and sulfonic groups (i.e. Nafion ® 120 and IonClad™ R4010) with lithium(I) counter-ions were investigated. The interactions between solvents of different polarity and the ion-exchange membranes with various morphologies were taken into account in order to better understand solvation and dissociation phenomena of the ion-pairs. Pervaporation of polar (i.e. water, methanol)–nonpolar (i.e. methyl acetate, dimethyl carbonate) liquid mixtures was carried out. It was revealed that the increase of the polar component concentration above 2 wt% in the feed mixture leads to dissociation of ion-pairs in Nafion membrane, which is reflected by the rapid increase of the polar component partial flux. In the case of IonClad membrane the dissociation of the ion-pairs during pervaporation was observed only when water was a polar feed component. The dissociation of ion-pairs was also evidenced in infrared study by observing the shift of symmetric stretching vibrations (ν s ) bands of sulfonic groups to the lower wavenumbers, compared to the membrane in the dry state. The symmetric stretching vibrations (ν s ) bands of the dry Nafion membrane and membrane solvated with water and methanol were equal to 1071 cm −1 , 1058 cm −1 , and 1054 cm −1 , respectively. In the case of IonClad membrane the symmetric stretching vibration (ν s ) bands changed in contact with water from 1047 cm −1 (dry membrane) to 1037 cm −1 . The dissociation of the ion-pairs did not occur in IonClad membrane equilibrated with methanol, which is also consistent with the result obtained during pervaporation.

Published
2016
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23. Enhanced removal of Cr(VI) by polymer inclusion membrane based on poly(vinylidene fluoride) and Aliquat 336

Author

Ferhat Sellami, Laurent Colasse, Stéphane Marais, Ounissa Kebiche-Senhadji, Kateryna Fatyeyeva, Université Abderrahmane Mira [Béjaïa], Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), and Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)

Subjects
chemistry.chemical_classification, Facilitated diffusion, Metal ions in aqueous solution, Inorganic chemistry, Plasticizer, Filtration and Separation, 02 engineering and technology, Polymer, Aliquat 336, 021001 nanoscience & nanotechnology, Acceptor, Analytical Chemistry, chemistry.chemical_compound, Membrane, 020401 chemical engineering, chemistry, [CHIM]Chemical Sciences, 0204 chemical engineering, 0210 nano-technology, Fluoride
Abstract

New polymer inclusion membranes (PIMs) based on poly(vinylidene fluoride) (PVDF) (polymer matrix), tricaprylmethylammonium chloride (Aliquat 336) (ion carrier) and 2-nitrophenyloctylether (2NPOE) (plasticizer) were successfully elaborated by casting evaporation method and used in selectively facilitated transport of Cr(VI) ions in an acidic aqueous medium. Obtained PIMs are dense and homogeneous and are characterized by intermolecular interactions of the membrane components (i.e. polymer matrix, ion carrier and plasticizer). The presence of ion carrier and plasticizer enhances the membrane flexibility and its hydrophilic character. The decrease of the PVDF melting point is ascribed to the strong electrostatic interactions between liquid compounds (i.e. ion carrier and plasticizer) and polymer chains. PVDF-based PIM with only 20 wt% of Aliquat 336 ensures almost complete transport of Cr(VI) ions from the donor to acceptor phase. Moreover, the addition of 5 wt% of plasticizer significantly increases the transport flux. Also, Cr(VI) ions are selectively recovered (~97%) from a mixture containing other heavy metal ions (Cd(II), Pb(II), Fe(III), Zn(II), Cu(II), Ni(II), Co(II)) with such PIM. Elaborated PVDF-based PIMs reveal improved transport properties compared to other polymer-based PIMs, exhibiting high stability (more than 190 h) and lifetime durability and so they are suitable for long term application.

Published
2020
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24. Biodegradable PLA/PBS multinanolayer membrane with enhanced barrier performances

Author

Nadège Follain, Nicolas Delpouve, Valerie Gaucher, Cyrille Sollogoub, Tiphaine Messin, Stéphane Marais, Alain Guinault, Polymères Biopolymères Surfaces (PBS), Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-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), Unité Matériaux et Transformations - UMR 8207 (UMET), Centrale Lille-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), Groupe de physique des matériaux (GPM), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche sur les Matériaux Avancés (IRMA), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Rouen Normandie (UNIROUEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Conservatoire National des Arts et Métiers [CNAM] (CNAM)-Arts et Métiers Sciences et Technologies, HESAM Université (HESAM)-HESAM Université (HESAM), Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE)-Centrale Lille Institut (CLIL), Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU), Normandie Université (NU)-Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), Procédés et Ingénierie en Mécanique et Matériaux [Paris] (PIMM), Conservatoire National des Arts et Métiers [CNAM] (CNAM)-École Nationale Supérieure d'Arts et Métiers (ENSAM), Arts et Métiers Sciences et Technologies, HESAM Université (HESAM)-HESAM Université (HESAM)-Arts et Métiers Sciences et Technologies, HESAM Université (HESAM)-HESAM Université (HESAM)-Centre National de la Recherche Scientifique (CNRS), Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de Recherche pour l’Agriculture, l’Alimentation et l’Environnement (INRAE), and Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université de Rouen Normandie (UNIROUEN)

Subjects
Matériaux [Sciences de l'ingénieur], Materials science, Diffusion, Filtration and Separation, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Biochemistry, [SPI.MAT]Engineering Sciences [physics]/Materials, Crystallinity, Coextrusion, poly(butylene succinate), General Materials Science, Physical and Theoretical Chemistry, ComputingMilieux_MISCELLANEOUS, chemistry.chemical_classification, Barrier properties, Thin layers, [CHIM.MATE]Chemical Sciences/Material chemistry, Polymer, Multilayer film, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Polybutylene succinate, Polyester, Membrane, chemistry, Chemical engineering, Barrier properties - Coextrusion - Multilayer film - poly(butylene succinate) - poly(lactic acid), Extrusion, poly(lactic acid), 0210 nano-technology
Abstract

International audience; Polyester multilayer membranes with more than 2000 alternating layers of poly(lactic acid) (PLA) and poly(butylene succinate) (PBS) were successfully prepared via a nanolayer coextrusion process equipped with a multiplying-element device. This process allows to make films consisting of very thin layers of polymers and in which a confinement effect of the semicrystalline polymer can be induced at point to significantly improve its physical properties. In this work, a homogeneous multinanolayer film of PLA/PBS was obtained without defaults or delamination, while the two polymers are immiscible. Continuous and homogeneous ultrathin layers of PBS (~45 nm) were obtained and the resulting confined structure of PBS led to an improvement of its barrier performances until 30% for oxygen, 40% for water and 70% for carbon dioxide. This improvement was explained by a decrease of the solubility coefficient and surprisingly not by the diffusion coefficient. This result was attributed to a slight orientation of the crystals in the extrusion direction and to the probable presence of an interphase between the layers of PLA and PBS.

Published
2020
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25. Tunable gas barrier properties of filled-PCL film by forming percolating cellulose network

Author

Julien Bras, Alain Dufresne, Sabrina Belbekhouche, Stéphane Marais, Corinne Chappey, Nadège Follain, Gilberto Siqueira, Polymères Biopolymères Surfaces (PBS), Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie et des Matériaux Paris-Est (ICMPE), Institut de Chimie du CNRS (INC)-Université Paris-Est Créteil Val-de-Marne - Paris 12 (UPEC UP12)-Centre National de la Recherche Scientifique (CNRS), Laboratoire Génie des procédés papetiers (LGP2 ), Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP )-Institut National Polytechnique de Grenoble (INPG)-Centre National de la Recherche Scientifique (CNRS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), and Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Gas permeation, Nanoparticle, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Nanocellulose, Nanocomposites, Percolating network, [SPI.MAT]Engineering Sciences [physics]/Materials, chemistry.chemical_compound, Crystallinity, [SPI]Engineering Sciences [physics], Colloid and Surface Chemistry, Phase (matter), [CHIM]Chemical Sciences, Cellulose, Nanocomposite, Gas diffusion, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, [CHIM.POLY]Chemical Sciences/Polymers, Chemical engineering, chemistry, Nanocrystal, 0210 nano-technology, Caprolactone
Abstract

International audience; Herein, a three-dimensional percolating cellulose nanocrystal network has been successfully entangled into a poly(caprolactone) (PCL) film to prepare fully biodegradable bio-nanocomposites. To strongly assembly the reinforcing dense cellulose phase and PCL chains and limit the incompatibility effect, the cellulose surface was chemically modified using a long-chain isocyanate as grafting agent. Structural effects are highlighted through gas transport examination using several diffusing probes. A peculiar and unexpected behavior is evidenced: both permeability and diffusivity increased, whereas solubility is reduced, compared to the unfilled PCL film. One can suspect that the formation of the reinforcing cellulose network and its anchoring to PCL chains are the cause of structural defects facilitating the gas transfer localized in interfacial regions. The resulting structure of the film plays a main role on gas barrier performances compared to the change in crystallinity and tortuosity effect induced by rod-like nanoparticles.

Published
2018
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26. Improvement of barrier properties of bio-based polyester nanocomposite membranes by water-assisted extrusion

Author

Jérémie Soulestin, Nadège Follain, Sébastien Charlon, Eric Dargent, Michel Sclavons, Stéphane Marais, Corinne Chappey, Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Laboratoire d’Etude et de Caractérisation des Amorphes et des Polymères (AMME-LECAP EA 4528 International Laboratory), Université de Rouen Normandie (UNIROUEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA), 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, and Université Catholique de Louvain = Catholic University of Louvain (UCL)

Subjects
Materials science, Plastics extrusion, Filtration and Separation, 02 engineering and technology, 010402 general chemistry, 01 natural sciences, Biochemistry, Polymer chemistry, General Materials Science, Thermal stability, Physical and Theoretical Chemistry, ComputingMilieux_MISCELLANEOUS, chemistry.chemical_classification, Nanocomposite, [CHIM.MATE]Chemical Sciences/Material chemistry, Polymer, 021001 nanoscience & nanotechnology, Exfoliation joint, 0104 chemical sciences, [CHIM.POLY]Chemical Sciences/Polymers, Membrane, Chemical engineering, chemistry, Extrusion, 0210 nano-technology, Dispersion (chemistry)
Abstract

Hybrid membranes made of a biopolymer matrix poly(butylene succinate) (PBS) or poly(butylene succinate-co-butylene adipate) (PBSA) loaded with 5 wt% of native (CNa) or organo-modified (C30B) montmorillonites were successfully extruded using new extrusion conditions where liquid water was introduced into the extruder barrel to improve the nanofiller dispersion and exfoliation levels. The C30B incorporation in both matrices leads to the degradation of polymer chains and the reduction of the thermal stability while the CNa introduction combined with the water injection presents no effect on the polymer molecular weight and the thermal stability. The water-assisted extrusion process enables the increase in CNa dispersion and exfoliation levels in both matrices, which improves barrier properties to gases and water by tortuosity effects. In the case of C30B, the positive effect of dispersion induced by water injection was much less pronounced since C30B particles were already well dispersed and exfoliated in both matrices. The use of the water injection at high pressure during the extrusion process was found really efficient for native montmorillonite and so appears as a promising process for dispersing hydrophilic particles in polymers having a low hydrophilic character, without preliminary chemical modification of the fillers.

Published
2015
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27. Multifunctional hydrolyzed EVA membranes with tunable microstructure and water barrier properties

Author

Eric Dargent, Kateryna Fatyeyeva, Stéphane Marais, Jorge Arturo Soto Puente, Polymères Biopolymères Surfaces (PBS), Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), Groupe de physique des matériaux (GPM), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche sur les Matériaux Avancés (IRMA), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Rouen Normandie (UNIROUEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), and Normandie Université (NU)

Subjects
Vinyl alcohol, Water transport, Materials science, Filtration and Separation, Sorption, [CHIM.MATE]Chemical Sciences/Material chemistry, Microstructure, Biochemistry, [SPI]Engineering Sciences [physics], chemistry.chemical_compound, Crystallinity, [CHIM.POLY]Chemical Sciences/Polymers, Membrane, chemistry, Chemical engineering, 13. Climate action, Desorption, Polymer chemistry, Vinyl acetate, [CHIM]Chemical Sciences, General Materials Science, Physical and Theoretical Chemistry, ComputingMilieux_MISCELLANEOUS
Abstract

A new functional membrane based on poly(ethylene- co -vinyl acetate) (EVA) and poly(ethylene- co -vinyl alcohol) (EVOH) was obtained by hydrolysis reaction on both surfaces of an EVA film, and as a result a three-layered structure (EVOH/EVA/EVOH) was formed. The chemical modification of the film and the thickness of hydrolyzed layer were controlled by FTIR and fluorescent microscopy measurements, respectively. The influence of the hydrolysis time ( t h ) on the thermal properties and membrane microstructure, studied by thermal analysis and X-ray diffraction measurements, indicated the evolution from the amorphous state to the semicrystalline one. The impact of the microstructure modification on the water transport properties was evaluated by permeability and sorption measurements. The plasticization effect of the three-layered membrane was found to be 2 times higher than that in the case of the completely hydrolyzed membrane ( t h >72 h). Such behavior was related to the amorphous/crystalline state of EVOH in the membrane. The results of water sorption measurements indicated that the water desorption is delayed at the highest temperatures in the case of the three-layered membranes. A strong correlation between the water properties of the hydrolyzed EVA membranes and the EVOH structure was observed. In addition, to providing details on structural characteristics of the three-layered multifunctional membrane with tunable water barrier properties, some possible applications where controlled moisture is necessary (such as food packaging or proton exchange fuel cell membrane) were discussed.

Published
2015
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28. Sulfonic Membrane Sorption and Permeation Properties: Complementary Approaches to Select a Membrane for Pervaporation

Author

Wojciech Kujawski, Larisa Karpenko-Jereb, Anne-Marie Kelterer, Edyta Rynkowska, Stéphane Marais, Corinne Chappey, Kateryna Fatyeyeva, Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Nicolaus Copernicus University, Faculty of Chemistry, Nicolaus Copernicus University [Toruń], and Graz University of Technology [Graz] (TU Graz)

Subjects
Chemistry, Inorganic chemistry, Membrane structure, Sorption, [CHIM.MATE]Chemical Sciences/Material chemistry, 02 engineering and technology, Permeation, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Dissociation (chemistry), 0104 chemical sciences, Surfaces, Coatings and Films, chemistry.chemical_compound, [CHIM.POLY]Chemical Sciences/Polymers, Membrane, Materials Chemistry, Semipermeable membrane, Pervaporation, Methanol, Physical and Theoretical Chemistry, 0210 nano-technology, ComputingMilieux_MISCELLANEOUS
Abstract

In this contribution, the physical and chemical properties of the dense sulfonic membrane IonClad R4010 in the lithium form were studied to evaluate its potential application in pervaporation. To develop new membrane materials, it is necessary to know the influence of the membrane structure on the membrane equilibrium and transport properties. For this purpose, the sorption and permeation measurements of water and methanol in the liquid and vapor states were performed and correlated to the ion pairs/solvent interactions analyzed by the infrared spectroscopy. The IonClad R4010 equilibrium and transport properties were found to be quite different depending on the permeant nature. The sorption and diffusion behavior of water and methanol was well described by means of the type II sorption model (BET theory). The swelling capacity of the IonClad R4010 membrane in methanol was found to be much lower than that in liquid water. In contrast to methanol, the total dissociation of the ion pairs in the IonClad R4010 membrane was obtained in the presence of water but only at high activity (∼0.8). Besides, the dispersion of the water molecules in the membrane was found to be homogeneous. The infrared spectroscopy results revealed that the methanol molecules had weaker interactions with the sulfonic groups of IonClad R4010 in agreement with the sorption data. The permeation properties were investigated by means of the sweeping gas and gravimetric methods in order to evaluate the membrane performance for pervaporation. The permeation results are in accordance with those obtained by sorption, thus confirming the complementariness of the two approaches.

Published
2017
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29. Confinement effect in PC/MXD6 multilayer films: Impact of the microlayered structure on water and gas barrier properties

Author

Nadège Follain, Guillaume Miquelard-Garnier, Stéphane Marais, Alain Guinault, Cyrille Sollogoub, Valerie Gaucher, Nicolas Delpouve, Tiphaine Messin, Polymères Biopolymères Surfaces (PBS), Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), Procédés et Ingénierie en Mécanique et Matériaux [Paris] (PIMM), Conservatoire National des Arts et Métiers [CNAM] (CNAM)-École Nationale Supérieure d'Arts et Métiers (ENSAM), Arts et Métiers Sciences et Technologies, HESAM Université (HESAM)-HESAM Université (HESAM)-Arts et Métiers Sciences et Technologies, HESAM Université (HESAM)-HESAM Université (HESAM)-Centre National de la Recherche Scientifique (CNRS), Normandie Université (NU), Unité Matériaux et Transformations - UMR 8207 (UMET), Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut National de la Recherche Agronomique (INRA), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Laboratoire Procédés et Ingénierie en Mécanique et Matériaux (PIMM), Conservatoire National des Arts et Métiers [CNAM] (CNAM)-Arts et Métiers Sciences et Technologies, HESAM Université (HESAM)-HESAM Université (HESAM), Institut de Chimie du CNRS (INC)-Institut National de la Recherche Agronomique (INRA)-Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Ecole Nationale Supérieure de Chimie de Lille (ENSCL), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), 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, and HESAM Université - Communauté d'universités et d'établissements Hautes écoles Sorbonne Arts et métiers université (HESAM)

Subjects
Confined structure, Matériaux [Sciences de l'ingénieur], Chemical substance, Filtration and Separation, 02 engineering and technology, 010402 general chemistry, poly(m-xylene adipamide), 01 natural sciences, Biochemistry, Permeability, [SPI.MAT]Engineering Sciences [physics]/Materials, Crystallinity, Multilayer, General Materials Science, Physical and Theoretical Chemistry, Polycarbonate, Barrier properties, Mécanique [Sciences de l'ingénieur], Chemistry, Permeation, [SPI.MECA]Engineering Sciences [physics]/Mechanics [physics.med-ph], 021001 nanoscience & nanotechnology, 0104 chemical sciences, Amorphous solid, Polycarbonate, poly(m-xylene adipamide), Membrane, Chemical engineering, Permeability (electromagnetism), visual_art, visual_art.visual_art_medium, 0210 nano-technology, Science, technology and society
Abstract

Films of PC and MXD6 were prepared via multilayer coextrusion. Films presenting stretched nodules/lamellas of MXD6 in the PC matrix, and films with quasi-continuous thin MXD6 layers alternating with PC layers were obtained. The transport properties were specifically investigated from water and gas permeation kinetics, and the corresponding permeation parameters were determined. The confinement effect of MXD6 in the multilayer structure was highlighted by comparing the permeability predicted from the series model equation with the experimental data. Although the MXD6 layers were not homogeneous and continuous for all membranes, water and gas permeabilities of the PC/MXD6 multilayer film were largely reduced. Such improvement of barrier properties was related to the change of the MXD6 structure, considering that the confinement of the MXD6 layers induced by PC layers allowed to bring chain orientation and to reduce the chain segment mobility in the MXD6 amorphous constrained zones. In addition, in the case of a PC/MXD6 multilayer structure well defined with continuous layers and relatively homogeneous thicknesses, the degree of crystallinity was slightly increased.

Published
2017
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30. Structure and Barrier Properties of Multinanolayered Biodegradable PLA/PBSA Films: Confinement Effect via Forced Assembly Coextrusion

Author

Nicolas Delpouve, Cyrille Sollogoub, Valerie Gaucher, Stéphane Marais, Alain Guinault, Nadège Follain, Tiphaine Messin, Polymères Biopolymères Surfaces (PBS), Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), Procédés et Ingénierie en Mécanique et Matériaux [Paris] (PIMM), Conservatoire National des Arts et Métiers [CNAM] (CNAM)-École Nationale Supérieure d'Arts et Métiers (ENSAM), Arts et Métiers Sciences et Technologies, HESAM Université (HESAM)-HESAM Université (HESAM)-Arts et Métiers Sciences et Technologies, HESAM Université (HESAM)-HESAM Université (HESAM)-Centre National de la Recherche Scientifique (CNRS), Unité Matériaux et Transformations - UMR 8207 (UMET), Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut National de la Recherche Agronomique (INRA), Groupe de physique des matériaux (GPM), Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-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), Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Institut de Recherche sur les Matériaux Avancés (IRMA), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Rouen Normandie (UNIROUEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Centre National de la Recherche Scientifique (CNRS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Conservatoire National des Arts et Métiers [CNAM] (CNAM)-Arts et Métiers Sciences et Technologies, HESAM Université (HESAM)-HESAM Université (HESAM), Institut de Chimie du CNRS (INC)-Institut National de la Recherche Agronomique (INRA)-Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Ecole Nationale Supérieure de Chimie de Lille (ENSCL), and Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN)

Subjects
Matériaux [Sciences de l'ingénieur], Materials science, multilayer polymer film, Diffusion, barrier properties, 02 engineering and technology, coextrusion, 010402 general chemistry, 01 natural sciences, [SPI.MAT]Engineering Sciences [physics]/Materials, Crystallinity, General Materials Science, poly(butylene succinate-co-butylene adipate), Composite material, chemistry.chemical_classification, Mécanique [Sciences de l'ingénieur], confined crystallization, Polymer, Permeation, [SPI.MECA]Engineering Sciences [physics]/Mechanics [physics.med-ph], 021001 nanoscience & nanotechnology, Microstructure, 0104 chemical sciences, Amorphous solid, Polyester, chemistry, multilayer polymer film, coextrusion, confined crystallization, permeability, poly(lactic acid), poly(butylene succinate-co-butylene adipate), barrier properties, poly(lactic acid), permeability, 0210 nano-technology, Layer (electronics)
Abstract

International audience; Multilayer coextrusion processing was applied to produce 2049-layer film of poly(butylene succinate-co-butylene adipate) (PBSA) confined against poly(lactic acid) (PLA) using forced assembly, where the PBSA layer thickness was about 60 nm. This unique technology allowed to process semicrystalline PBSA as confined polymer and amorphous PLA as confining polymer in a continuous manner. The continuity of PBSA layers within the 80/20 wt % PLA/PBSA layered films was clearly evidenced by atomic force microscopy (AFM). Similar thermal events to the reference films were revealed by thermal studies; indicating no diffusion of polymers during the melt-processing. Mechanical properties were measured for the multilayer film and the obtained results were those expected considering the fraction of each polymer, revealing the absence of delamination in the PLA/PBSA multinanolayer film. The confinement effect induced by PLA led to a slight orientation of the crystals, an increase of the rigid amorphous fraction (RAF) in PBSA with a densification of this fraction without changing film crystallinity. These structural changes allowed to strongly improve the water vapor and gas barrier properties of the PBSA layer into the multilayer film up to two decades in the case of CO2 gas. By confining the PBSA structure in very thin and continuous layers, it was then possible to improve the barrier performances of a biodegradable system and the resulting barrier properties were successfully correlated to the effect of confinement on the microstructure and the chain segment mobility of the amorphous phase. Such investigation on these multinanolayers of PLA/PBSA with the aim of evidencing relationships between microstructure implying RAF and barrier performances has never been performed yet. Besides, gas and water permeation results have shown that the barrier improvement obtained from the multilayer was mainly due to the reduction of solubility linked to the reduction of the free volume while the tortuosity effect, as usually expected, was not really observed. This work brings new insights in the field of physicochemical behaviors of new multilayer films made of biodegradable polyesters but also in interfacial processes due to the confinement effect induced in these multinanolayer structures obtained by the forced assembly coextrusion. This original coextrusion process was a very advantageous technique to produce eco-friendly materials with functional properties without the help of tie layer, additives, solvents, surface treatments, or inorganic fillers.

Published
2017
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31. Supported ionic liquid membranes for water and volatile organic compounds separation: Sorption and permeation properties

Author

Dominique Langevin, Stéphane Marais, Oksana Tarasyuk, Abdellatif Dahi, Kateryna Fatyeyeva, Corinne Chappey, Sergiy Rogalsky, and Amel Benamor

Subjects
Materials science, Cyclohexane, Filtration and Separation, Sorption, Permeation, Biochemistry, chemistry.chemical_compound, Membrane, chemistry, Chemical engineering, Phase (matter), Ionic liquid, Organic chemistry, General Materials Science, Bubble point, Physical and Theoretical Chemistry, Phase inversion
Abstract

Supported ionic liquid membranes (SILMs) were prepared by immobilizing the room temperature ionic liquids (RTILs) ([C4C1im][BF4] and [CnC1im][PF6] (n=4 and 6)) in a porous Matrimid membrane. The Matrimid membrane was prepared by water vapor-induced phase inversion, and its porous structure was characterized by SEM. After immersion of the porous Matrimid membrane in RTILs, the prepared SILMs were composed of 60% of RTIL phase. From the bubble point test, the SILMs displayed an excellent retention of their RTIL phase, and thus showed a good stability in the face of increased pressure on one of their faces. The feasibility of the prepared SILMs for the separation of water and volatile organic compounds (VOCs) such as ethanol and cyclohexane by vapor permeation was investigated. For this purpose, a preliminary study of water and VOC vapor sorption in RTILs was necessary to determine the affinity between each solute and RTILs. Only [C4C1im][BF4] showed both the best sorption capacities and the good sorption selectivities. The vapor permeation measurements were therefore carried out only through the SILMs impregnated with [C4C1im][BF4]. The SILM permeability was found to increase in the same sorption affinity order as for [C4C1im][BF4], i.e. cyclohexane

Published
2014
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32. Effect of cold plasma treatment on surface properties and gas permeability of polyimide films

Author

Corinne Chappey, Stéphane Marais, Dominique Langevin, Abdellatif Dahi, Jean-Marc Valleton, Kateryna Fatyeyeva, and Fabienne Poncin-Epaillard

Subjects
chemistry.chemical_classification, Materials science, General Chemical Engineering, Analytical chemistry, General Chemistry, Surface finish, Plasma, Polymer, Permeation, Contact angle, X-ray photoelectron spectroscopy, chemistry, Surface modification, Polyimide
Abstract

The surface functionalization of polyimide (Matrimid® 5218) films was carried out by cold plasma treatment with CF4, N2 and O2 gases using a radio frequency discharge and the optimum plasma conditions were evaluated by water contact angle measurements. The surface hydrophobicity of polyimide films was obtained after CF4 plasma treatment, while O2 and N2 plasma treatments contributed to the hydrophilic surface functionalization. X-ray photoelectron spectroscopy (XPS) results revealed the presence of CFx, amino or oxygen-containing groups attached to the polyimide film surface depending on the treatment gas. A strong influence of the used plasma gas on the film roughness was determined by atomic force microscopy (AFM) measurements. The influence of the surface modification on CO2, N2 and O2 gas permeation through the plasma treated films was evaluated. The permeation behaviour was characterized in terms of transport parameters, namely, coefficients of permeability, diffusion and solubility. The permeability coefficient of all plasma treated polyimide films for the studied gases (CO2, N2 and O2) was found to decrease following the order of increasing the kinetic molecular diameter of the penetrant gas. Besides, the selectivity coefficient was found to be significantly increased after the plasma treatments – αCO2/N2 was increased up to 36% and 98% for O2 and N2 plasma treated Matrimid® 5218 films, respectively. The relationship between the gas permeation behaviour and the surface modification of polymer film by cold plasma was discussed.

Published
2014
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33. Water sorption in Nafion® membranes analyzed with an improved dual-mode sorption model—Structure/property relationships

Author

Dominique Langevin, Yongli Li, Marc Legras, Stéphane Marais, Quang Trong Nguyen, and Camille Lixon Buquet

Subjects
Membrane structure, Ionic bonding, Filtration and Separation, Sorption, complex mixtures, Biochemistry, chemistry.chemical_compound, Membrane, Solvation shell, Chemical engineering, chemistry, Nafion, Organic chemistry, General Materials Science, Physical and Theoretical Chemistry, Ionomer, Water vapor
Abstract

Sigmoid-shaped isotherms for water vapor sorption in fuel cell membranes were analyzed with Feng's new dual-mode model for two series of ionomer systems, Nafion ® 117 membranes with different counter-ions and protonated Nafion ® membranes aged under different degrees of humidity. Feng's model appeared to be an excellent sorption model for these sigmoid isotherms and the values of its parameters were used for an analysis of the membrane structure/property relationships. The first model parameter, Cp , corresponds to the number of water molecules strongly sorbed in the first hydration shell of the membrane sulfonic sites. The upward curvature in the isotherms at high water activities, reflected by the A ′ parameter, appeared to be mainly due to the clustering of new water molecules on those of the first hydration shell. The number of water molecules per ionic site hydration depends on several structural parameters. The counter-ion of high electrostatic power attracts more water molecules per ion site, both in the first hydration shell and in subsequent sorption layers. The qualitative relationships between the membrane structure and its sorption properties obtained by analyzing the New Dual Mode Sorption (NDMS) model parameters make possible different interpretations of several data sets reported in the literature, such as the data on the sorption of different alcohols and the water sorption in Nafion ® membranes during ageing.

Published
2013
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34. Water Transport Properties of Poly(butylene succinate) and Poly[(butylene succinate)- co -(butylene adipate)] Nanocomposite Films: Influence of the Water-Assisted Extrusion Process

Author

Jérémie Soulestin, Sébastien Charlon, Stéphane Marais, Michel Sclavons, Nadège Follain, 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, Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Université Catholique de Louvain = Catholic University of Louvain (UCL), and UCL - SST/IMCN/BSMA - Bio and soft matter

Subjects
Water transport, Nanocomposite, Materials science, Sorption, 02 engineering and technology, [CHIM.MATE]Chemical Sciences/Material chemistry, Permeation, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, Exfoliation joint, 0104 chemical sciences, Surfaces, Coatings and Films, Electronic, Optical and Magnetic Materials, Polybutylene succinate, Crystallinity, General Energy, [CHIM.POLY]Chemical Sciences/Polymers, Chemical engineering, Adipate, Polymer chemistry, Physical and Theoretical Chemistry, 0210 nano-technology, ComputingMilieux_MISCELLANEOUS
Abstract

Poly(butylene succinate) (PBS) and poly-[(butylene succinate)-co-(butylene adipate)] (PBSA)-based composite films loaded with 5 wt % of fillers (native or organomodified montmorillonites) were extruded using a standard protocol or assisted by water injection. In the resulting composite films, the filler morphology was altered, as evidenced by TEM images. The CNa aggregates were broken with the help of water injection, and the exfoliation/dispersion levels of C30B were dependent on the matrix. By considering the degree of crystallinity of the polymer matrix, the nature of the fillers, and also the processing conditions, the film (micro)structure was successfully correlated to the water (liquid and vapor) behavior of the PBSand PBSA-based films, studied by means of sorption and permeation measurements. The water permeability and diffusivity were significantly reduced even with an increased water sorption, depending on the matrix and the clay morphology or nature. Specifically, concomitant effects such as tortuosity and trapping but also preferential diffusion pathways as well as free volumes in matrix strikingly were responsible for the barrier performances evolution.

Published
2016
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35. Barrier properties of polyamide 12/montmorillonite nanocomposites: Effect of clay structure and mixing conditions

Author

Laurent Colasse, Pascal Médéric, Nadège Follain, Stéphane Marais, B. Alexandre, Corinne Chappey, Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Laboratoire d'Ingénierie des Matériaux de Bretagne (LIMATB), Université de Bretagne Sud (UBS)-Université de Brest (UBO)-Institut Brestois du Numérique et des Mathématiques (IBNM), Université de Brest (UBO)-Université de Brest (UBO), and SOS Mal de Seine

Subjects
Materials science, Water activity, 02 engineering and technology, 010402 general chemistry, Thermal diffusivity, 01 natural sciences, Tortuosity, chemistry.chemical_compound, [SPI]Engineering Sciences [physics], medicine, [CHIM]Chemical Sciences, Composite material, ComputingMilieux_MISCELLANEOUS, Aqueous solution, Nanocomposite, General Engineering, Sorption, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Water retention, Montmorillonite, [CHIM.POLY]Chemical Sciences/Polymers, chemistry, Ceramics and Composites, medicine.symptom, 0210 nano-technology
Abstract

Hybrid films, composed of a PA12 polyamide matrix filled with 5 wt% of clays were melt processed under different mixing conditions to classically obtain montmorillonite-filled microcomposites and organo-modified montmorillonite-filled nanocomposites. The change in mixing shear rates allowed to notably modulating the fragmentation level for montmorillonite and the exfoliation level for modified montmorillonite. Barrier properties to nitrogen and water were altered with a reduction in PA12 chain mobility by confinement effect and geometrical constraints. Tortuosity effects induced by fillers were also highlighted. The water permeability and diffusivity were significantly decreased with exfoliated clays, while an increase was measured with an increased water solubility in presence of clay aggregates, both counterbalanced tortuosity effects. This trend was amplified when using low shear rates. According to filler used and mixing conditions, water sorption measurement has successfully demonstrated an increase in water solubility, due to filler affinity, which was surprisingly inconsistent with the change of water permeability. The occurrence of water plasticization phenomenon was also pointed out through the non-constant diffusivity, reflecting an increased free volume with water activity. Again, a decrease in water diffusivity was unexpectedly obtained, explained by tortuosity effects and ascribed to local water retention at the vicinity of clays, which creates water aggregates in films. These findings were also confirmed by a mathematical modeling approach of sorption process, discussing about the sorbed water access.

Published
2016
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36. Influence of Crystallinity on the Dielectric Relaxations of Poly(Butylene Succinate) and Poly[(Butylene Succinate)- Co -(Butylene Adipate)]

Author

Nadège Follain, Stéphane Marais, Laurent Delbreilh, Eric Dargent, Sébastien Charlon, Jérémie Soulestin, Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Laboratoire d’Etude et de Caractérisation des Amorphes et des Polymères (AMME-LECAP EA 4528 International Laboratory), Université de Rouen Normandie (UNIROUEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA), 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), and Ecole nationale supérieure Mines-Télécom Lille Douai (IMT Lille Douai)

Subjects
Materials science, Polymers and Plastics, General Physics and Astronomy, 02 engineering and technology, Dielectric, 010402 general chemistry, 01 natural sciences, Crystallinity, Differential scanning calorimetry, Adipate, Polymer chemistry, Materials Chemistry, [PHYS.COND]Physics [physics]/Condensed Matter [cond-mat], ComputingMilieux_MISCELLANEOUS, chemistry.chemical_classification, Organic Chemistry, Polymer, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Microstructure, 0104 chemical sciences, Amorphous solid, Polybutylene succinate, [CHIM.POLY]Chemical Sciences/Polymers, chemistry, Chemical engineering, 0210 nano-technology
Abstract

Amorphous and semi-crystalline poly(butylene succinate) (PBS) and poly[(butylene succinate)-co-(butylene adipate)] (PBSA) are studied with Differential Scanning Calorimetry and Broadband Dielectric Spectroscopy (BDS). It was shown that 21 mol% of butylene adipate group decreases drastically the degree of crystallinity and the size of the crystal lamellae of the PBSA. For the two semi-crystalline polymers, the microstructure is well described by a three-phase model including a small degree of rigid amorphous fraction. Fragility indexes of the main dielectric relaxation are identical for each sample which shows similar segmental dynamics of their amorphous phase. BDS allows detecting complex secondary relaxations in semi-crystalline PBS and PBSA. Local motions are impacted by the microstructure and a new relaxation occurs in more constrained amorphous environments. Correlations between molecular mobility and barrier properties are proposed.

Published
2016
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37. Ab initio study of cationic polymeric membranes in water and methanol

Author

Kateryna Fatyeyeva, Sarah Lunghammer, Stéphane Marais, Larisa Karpenko-Jereb, Corinne Chappey, Anne-Marie Kelterer, Edyta Rynkowska, Wojciech Kujawski, Joanna Kujawa, Graz University of Technology [Graz] (TU Graz), Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Nicolaus Copernicus University, Faculty of Chemistry, and Nicolaus Copernicus University [Toruń]

Subjects
General Chemical Engineering, Inorganic chemistry, Ab initio, General Physics and Astronomy, 02 engineering and technology, Physics and Astronomy(all), 010402 general chemistry, 01 natural sciences, Dissociation (chemistry), chemistry.chemical_compound, Materials Science(all), Nafion, Polymer chemistry, Side chain, General Materials Science, Engineering(all), ComputingMilieux_MISCELLANEOUS, Chemistry, General Engineering, Cationic polymerization, Solvation, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Membrane, [CHIM.POLY]Chemical Sciences/Polymers, Ionic strength, Chemical Engineering(all), 0210 nano-technology
Abstract

The work is devoted to a computational study of three types of cationic polymeric membranes in Li+-ionic form, in water and methanol environments, at various solvation levels. The studied membranes Nafion, IonClad, and M3 possess the perfluorinated backbone; however, various side chains were terminated with the functional groups of distinctly different ionic strength. The paper discusses the structural features of the membrane-solvent clusters as well as an influence of the side chain nature on the dissociation of the functional groups and the binding energy of the solvent molecules. Additionally, the paper compares the obtained results for Li+-Nafion membrane in water with the results published earlier for H+ and Na+ forms.

Published
2016
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38. Composite membranes based on Nafion® and plasma treated clay charges: Elaboration and water sorption investigations

Author

Fabienne Poncin-Epaillard, Kateryna Fatyeyeva, Stéphane Marais, Jean-Marc Valleton, Corinne Chappey, and Dominique Langevin

Subjects
chemistry.chemical_classification, Water activity, Plasma activation, Filtration and Separation, Sorption, Polymer, Biochemistry, chemistry.chemical_compound, Membrane, Adsorption, chemistry, Chemical engineering, Nafion, Polymer chemistry, Particle, General Materials Science, Physical and Theoretical Chemistry
Abstract

Composite polymer membranes were prepared by incorporation of modified layered inorganic clay (Laponite) into Nafion® membranes. The modification of Laponite particles was performed by the plasma activation process and the chemical grafting of sulfonic groups as well as by the direct plasma sulfonation. The modified Laponite particles incorporated into a polymer film contribute to an increase of the proton conductivity of composite membranes at high temperatures (85 °C). For the first time the water vapor sorption properties of the modified clay and the composite membranes were investigated varying water activity conditions (from 0.1 to 0.95) by means of microgravimetry. The BET adsorption model as well as models of Park and Feng were applied to the experimental data. The parameter values (concentration of the adsorbed water, specific capacity and different aggregation constants) were found to agree well with the measured ones.

Published
2011
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39. Alfa fibres for unsaturated polyester composites reinforcement: Effects of chemical treatments on mechanical and permeation properties

Author

Laurent Lebrun, Nadège Follain, A. Bessadok, S. Roudesli, Stéphane Marais, Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Laboratoire Polymères, Biopolymères, Matériaux Organiques [Monastir] (LPBMO), and Université de Monastir - University of Monastir (UM)

Subjects
Materials science, Composite number, Maleic anhydride, [CHIM.MATE]Chemical Sciences/Material chemistry, 02 engineering and technology, Permeation, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, Styrene, [SPI]Engineering Sciences [physics], chemistry.chemical_compound, Acetic anhydride, [CHIM.POLY]Chemical Sciences/Polymers, chemistry, Mechanics of Materials, Permeability (electromagnetism), Ceramics and Composites, [CHIM]Chemical Sciences, Composite material, 0210 nano-technology, Reinforcement, ComputingMilieux_MISCELLANEOUS, Acrylic acid
Abstract

In this study, composite materials were prepared using unsaturated polyester resins reinforced by Alfa fibres. The fibres were previously modified by chemical treatments, maleic anhydride (MA), styrene (S), acrylic acid (AA) and acetic anhydride (Ac). The Ac and the S treatments allowed an increase in the moisture resistance and the mechanical properties of the fibres. The preliminary S or MA treatment of the fibres allowed a decrease of the water permeability of the composite. A slight increase of the stiffness of the composite was observed due to the presence of the fibres (treated or not), whereas the resistance (breaking strength and strain) was not improved. The mechanical behaviour of the composites appeared similar whatever the treatment of the fibres except with S treatment which seemed to improve the breaking strength.

Published
2009
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40. Influence of chemical modifications on water-sorption and mechanical properties of Agave fibres

Author

C. Lixon, A. Bessadok, Michel Metayer, S. Roudesli, and Stéphane Marais

Subjects
Langmuir, Materials science, Maleic anhydride, Young's modulus, Sorption, Acetic anhydride, chemistry.chemical_compound, symbols.namesake, chemistry, Mechanics of Materials, Ultimate tensile strength, Ceramics and Composites, symbols, Gravimetric analysis, Composite material, Acrylic acid
Abstract

Because of their good mechanical properties and low density, natural fibres are more and more considered as reinforcement in composite materials. In this work, to improve the adhesion between a polyester matrix (unsaturated polyester resin) and Agave (Agave Americana L .) fibres and to increase their moisture resistance, chemical surface treatments have been performed on the fibres. These different treatments were performed with acetic anhydride (Ac), styrene (S), acrylic acid (AA) and maleic anhydride (MA). The modified Agave fibres were characterized by means of infrared spectroscopy, surface energy, and microscopic analysis. The effect of these treatments on water sorption was investigated by using a gravimetric static equilibrium method. Water sorption isotherms have been deduced from kinetic data. The Park model based on the three sorption modes: Langmuir, Henry’s law, and clustering, was successfully used to simulate the experimental sorption data. It was found that the chemical treatments used reduced the overall water uptake of the Agave fibres. In particular, the acetylation treatment allows to significantly increase the moisture resistance of these fibres. The mechanical properties of the treated fibres were analyzed from tensile tests. The tensile modulus, the breaking strength and the breaking strain depend on the chemical treatment used.

Published
2008
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41. Kinetics of water sorption in flax and PET fibers

Author

A. Bessadok, F. Gouanvé, Michel Metayer, Stéphane Marais, and Dominique Langevin

Subjects
Absorption of water, Materials science, Polymers and Plastics, Water activity, Organic Chemistry, General Physics and Astronomy, Sorption, Thermal diffusivity, Synthetic fiber, Materials Chemistry, Fiber, Composite material, Water vapor, Natural fiber
Abstract

Composite materials are usually reinforced by synthetic fibers as carbon, glass etc…. Because of their good mechanical properties and low density, natural fibers are being considered more preferentially as reinforcement. The application of natural fibers as reinforcements in composite materials requires a strong adhesion between the fiber and the matrix. The poor resistance towards water absorption is one of the drawbacks of natural fibers which makes it more important to understand the dynamic properties of penetration of water molecules through these heterogeneous materials. Water vapour sorption kinetics in natural flax fibers have been performed at 25 °C by using an electronic microbalance (IGA, Hiden). By using the Fickian model for a complete cylinder water diffusion coefficients have been determined and calculated at short times (first half-sorption) and long times (second half-sorption) of kinetic curve and for different water activities. The values obtained for D1 and D2 are rather similar on the all range of water activity. Generally, water diffusivity increases and then decreases with water activity. The increase of diffusivity at low water activities may be explained on the basis of the dual mode sorption (Langmuir and Henry sorption’s combination) whereas the decrease for the higher activities can be attributed to the immobilization of sorbed water molecules due to the water clustering.

Published
2007
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42. Preparation and characterization of flax biocomposites made of seed mucilage reinforced by fibers

Author

Nadège Follain, Laurent Bizet, Davy Duriatti, Laurent Colasse, Florence Paynel, Stéphane Marais, Claudine Morvan, Iain Allan, Christophe Rihouey, Andrey Pavlov, Laurent Lebrun, Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), N.I. Vavilov Research Institute of Plant Industry (VIR (BИP)), Laboratoire Ondes et Milieux Complexes (LOMC), Centre National de la Recherche Scientifique (CNRS)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Normandie Université (NU), and University of Brighton

Subjects
Materials science, Scanning electron microscope, Composite number, Modulus, Compression molding, [CHIM.MATE]Chemical Sciences/Material chemistry, Compression (physics), [CHIM.POLY]Chemical Sciences/Polymers, Mucilage, Mechanics of Materials, Ribbon, Ceramics and Composites, [CHIM]Chemical Sciences, [SDV.BV]Life Sciences [q-bio]/Vegetal Biology, Fiber, Composite material, ComputingMilieux_MISCELLANEOUS
Abstract

Natural biocomposites were prepared from flax fibers and mucilage polysaccharides extracted from flax seeds, as a matrix, in two steps: impregnation and compression molding. The ribbons were preimpregnated with water plasticized mucilage. Solid mucilage (30%, w/w) was added to the ribbon impregnated with 20% mucilage, and the composite was compression molded. The solidified mucilage was homogeneous and rigid (2 GPa) with an elastic deformation of approximately 1%. The mechanical properties of the composites were in the ranges of 7–10 GPa, 300–400 MPa and 4–5% for the modulus, maximal strength and strain, respectively. The two latter parameters were larger than the ones for the fiber. The experimental values of the modulus and strength were in accordance with the values computed using the rule of mixture, which indicated a good interface between the fibers and the matrix. This was confirmed visually with scanning electron microscopy. The water sorption behavior of the composites was intermediate between the mucilage and the fiber alone.

Published
2015
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43. Water sorption properties of room-temperature ionic liquids over the whole range of water activity and molecular states of water in these media

Author

Sergiy Rogalsky, Oksana Tarasyuk, Stéphane Marais, Dominique Langevin, Corinne Chappey, Abdellatif Dahi, Kateryna Fatyeyeva, Polymères Biopolymères Surfaces (PBS), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Institute of Bioorganic Chemistry and Petrochemistry, and National Academy of Sciences of Ukraine (NASU)

Subjects
Water activity, Hydrogen bond, Chemistry, General Chemical Engineering, Inorganic chemistry, Sorption, 02 engineering and technology, General Chemistry, [CHIM.MATE]Chemical Sciences/Material chemistry, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 6. Clean water, 0104 chemical sciences, chemistry.chemical_compound, [CHIM.POLY]Chemical Sciences/Polymers, Ionic liquid, Non-random two-liquid model, Gravimetric analysis, Molecule, 0210 nano-technology, Water content, ComputingMilieux_MISCELLANEOUS
Abstract

The water sorption behavior for various RTILs ([C4C1im][BF4], [C4C1im][PF6], [C6C1im][PF6], [C4im][DBP], [C4im][BEHP] and [Et3HN][CF3SO3]) was studied over the whole range of water activity using a continuous gravimetric method. Analysis of the water sorption isotherms using the non-random two-liquid model (NRTL) and the combination of a dual-mode sorption (Henry-clustering) allowed a better understanding of the RTIL-water interactions. It is noticed that the sorption of water by RTILs is mainly controlled by the anion's nature. Anions interact with water molecules by hydrogen bonds that promotes the formation of a hydrogen bond network between the water molecules. The water uptake by RTILs increases in the following order (up to 0.8 in the water activity a): [C6C1im][PF6] ≤ [C4C1im][PF6] 0.8), water molecules are aggregated only in water-miscible RTILs (case of [C4im][DBP] and [Et3HN][CF3SO3]) because of their stronger anion basicity. To complete the sorption study, the molecular state of water dissolved in RTILs was studied by the infrared spectroscopy. The water molecules dissolved in water-immiscible RTIL such as [C4C1im][PF6] are not self-associated independently of the water content and, thus, can be defined as “free” water molecules interacting via H-bonding with the anions in the symmetric complex: anion⋯HOH⋯anion. On the contrary, the water molecules sorbed in water-miscible RTILs such as [C4im][DBP] or [Et3HN][CF3SO3] are strongly associated by H-bonds and also with the anions even at low water activity, and are easily aggregated when the water content reaches the critical concentration at high activity.

Published
2015
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44. Study of the α-relaxation of PVC, EVA and 50/50 EVA70/PVC blend

Author

C. Cabot, Jean-Marc Saiter, E. Bureau, and Stéphane Marais

Subjects
chemistry.chemical_classification, Materials science, Polymers and Plastics, Organic Chemistry, General Physics and Astronomy, Polymer, Amorphous solid, Polyvinyl chloride, chemistry.chemical_compound, Fragility, Differential scanning calorimetry, chemistry, Materials Chemistry, Relaxation (physics), Polymer blend, Composite material, Glass transition
Abstract

The dipole dynamics and α-relaxation behaviour of polyvinyl chloride PVC, poly(ethylene-co-vinyl-acetate) EVA70 and blend of them EVA70/PVC have been investigated by differential scanning calorimetry (DSC) and dielectric relaxation spectroscopy (DRS). The differential scanning calorimetry (DSC) thermograms measured on samples show a single glass transition in the analysed temperature range. These three polymers are wholly amorphous and pure PVC and pure EVA70 are miscible in the ratio 1:1. The glass transition temperature Tg decreases significantly with presence of EVA70. Furthermore, the values of apparent activation energies for molecular motions at the α-relaxation and the values of fragility index have also been determined for each sample using Moynihan expression for DSC results and Vogel–Fulcher–Tammann–Hesse (VFTH) form for DRS results. It is shown a large dependence of all the values of these parameters with the content of EVA70. Comparing these three polymers, we found that the more fragile glass forming liquid is the PVC. Fragility decreases drastically with EVA70 content. EVA70 and EVA70/PVC blend exhibit practically the same behaviour. The effect of inter- and intra-molecular interactions on fragility is discussed to explain these variations.

Published
2005
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45. Study of transport of small molecules through ethylene-co-vinyl acetate copolymers films. Part B: CO2 and O2 gases

Author

Michel Metayer, C. Devallencourt, Jean-Marc Saiter, Stéphane Marais, and Q.T Nguyen

Subjects
Materials science, Polymers and Plastics, Diffusion, Organic Chemistry, Analytical chemistry, chemistry.chemical_element, Permeation, Oxygen, chemistry.chemical_compound, Low-density polyethylene, chemistry, Polymer chemistry, Vinyl acetate, Gaseous diffusion, Semipermeable membrane, Solubility
Abstract

The transport of gases (pure oxygen and carbon dioxide) through poly(ethylene-co-vinyl acetate) (EVA) of different VA contents, was studied by permeation measurements. Permeabilities, diffusivities, and solubilities were determined for EVA films containing 19, 33, 50 and 70% (w/w) VA. A low density polyethylene LDPE (used as reference with 0% VA) was also studied. The diffusion of oxygen was determined from transient permeation fluxes and the diffusion of carbon dioxide from time-lag permeation. In the case of gas permeation, whatever the VA content of the polymer used, the experimental transient fluxes are characterized by a constant diffusion coefficient for both O2 and CO2. In terms of gas permeability, compared with water permeability (Part A), these copolymers are characterized by very low coefficients, especially for oxygen. Assuming that D is constant, the O2 and CO2 solubility coefficient was then deduced and its value is shown to increase proportionally with the VA content in these rubbery copolymers (whose quantity of crystalline phases decreases and become nil for 70% VA). The H2O/CO2 and H2O/O2 ideal selectivity α increases with the VA content, in agreement with the increase in average polarity of the copolymer.

Published
2002
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46. Microstructure and barrier properties of PHBV/organoclays bionanocomposites

Author

Jérémie Soulestin, Eric Dargent, Stéphane Marais, Serge Bourbigot, Nadège Follain, Raphaël Crétois, Laurent Lebrun, Polymères Biopolymères Surfaces (PBS), Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), Laboratoire d’Etude et de Caractérisation des Amorphes et des Polymères (AMME-LECAP EA 4528 International Laboratory), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), IMT Lille Douai, Ecole nationale supérieure Mines-Télécom Lille Douai (IMT Lille Douai), Institut Mines-Télécom [Paris] (IMT)-Institut Mines-Télécom [Paris] (IMT), Ingénierie des Systèmes Polymères, Unité Matériaux et Transformations - UMR 8207 (UMET), Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut National de la Recherche Agronomique (INRA)-Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut National de la Recherche Agronomique (INRA), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA), Institut Mines-Télécom [Paris] (IMT), Institut de Chimie du CNRS (INC)-Institut National de la Recherche Agronomique (INRA)-Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut de Chimie du CNRS (INC)-Institut National de la Recherche Agronomique (INRA)-Centre National de la Recherche Scientifique (CNRS)-Université de Lille-Ecole Nationale Supérieure de Chimie de Lille (ENSCL), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Centre National de la Recherche Scientifique (CNRS), and Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)-Institut National de la Recherche Agronomique (INRA)-Ecole Nationale Supérieure de Chimie de Lille (ENSCL)-Institut de Chimie du CNRS (INC)-Université de Lille-Centre National de la Recherche Scientifique (CNRS)

Subjects
Materials science, Nanocomposite, PHBV, Barrier properties, Intercalation (chemistry), Filtration and Separation, Permeation, Microstructure, Biochemistry, chemistry.chemical_compound, Bionanocomposite, Montmorillonite, [CHIM.POLY]Chemical Sciences/Polymers, Chemical engineering, chemistry, 13. Climate action, Phase (matter), Polymer chemistry, Copolymer, Sorption, [CHIM]Chemical Sciences, General Materials Science, Physical and Theoretical Chemistry, Dispersion (chemistry)
Abstract

International audience; The impact of organomodified montmorillonite on morphology, thermal and barrier properties of PHBV-based nanocomposites prepared by melt intercalation was investigated. XRD analyses and TEM observations have shown the presence of aggregated and intercalated structures with individual nanoclay platelets and a significant orientation of nanoclays into the nanocomposites. No nucleating effect induced by nanoclays was detected in DSC measurements, which indicates that the crystalline phase of the PHBV copolymer was not impacted. The improvement of barrier properties to gas and water was found to be dependent not only on the dispersion and orientation of nanoclays but also the nature of permeated molecules, the quality of the matrix/nanoclays interface and degradation effects induced during melting process. A competition between kinetic and thermodynamic contributions of the permeation process was highlighted. A dependence of the water diffusion coefficient with water concentration was observed as a result of water plasticization effect.

Published
2014
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47. Effect of molecular structure of sulphonated polyimide membranes on water sorption

Author

Camille Lixon Buquet, Quang Trong Nguyen, Stéphane Marais, and Yongli Li

Subjects
Models, Molecular, Materials science, Molecular Conformation, Ionic bonding, Imides, chemistry.chemical_compound, Nafion, Polymer chemistry, Computer Simulation, Electrical and Electronic Engineering, chemistry.chemical_classification, Water, Sorption, Membranes, Artificial, Polymer, Electronic, Optical and Magnetic Materials, Membrane, chemistry, Chemical engineering, Models, Chemical, Polymer blend, Adsorption, Counterion, Sulfonic Acids, Hydration energy, Hydrophobic and Hydrophilic Interactions, Biotechnology
Abstract

Water sorption in sulphonated polyimides with or without ionic block structure was analysed with Feng's new dual mode model. The effect of their molecular structure that determines the chain organisation in the solid materials was analysed by using the model parameters. The model parameters C p and A ' correspond to the sorbed water molecules on the first layer close to the ionic groups and on the subsequent layers, respectively. Based on these fitted physical parameters, the water sorption on the membranes with different counterions was studied and the hydration energy was proved to have much influence on the C p values. The effect of the structure of the block and the random copolymers on the C p and A ' values was discussed and compared with that for the well-known Nafion ® membranes. The large amount of sorbed water at high activities may induce a sufficiently large mobility of the polymer segments in the hydrophilic domains for material inflation, which leads to high A ' values.

Published
2014

48. The behaviour of wine aroma compounds related to structure and barrier properties of virgin, recycle and active PET membranes

Author

Clara Dombre, Camille Lixon-Buquet, Corinne Chappey, Pascale Chalier, Stéphane Marais, Ingénierie des Agro-polymères et Technologies Émergentes (UMR IATE), Centre de Coopération Internationale en Recherche Agronomique pour le Développement (Cirad)-Institut National de la Recherche Agronomique (INRA)-Université Montpellier 2 - Sciences et Techniques (UM2)-Centre international d'études supérieures en sciences agronomiques (Montpellier SupAgro)-Université de Montpellier (UM)-Institut national d’études supérieures agronomiques de Montpellier (Montpellier SupAgro), Polymères Biopolymères Surfaces (PBS), Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), Institut national d’études supérieures agronomiques de Montpellier (Montpellier SupAgro)-Centre de Coopération Internationale en Recherche Agronomique pour le Développement (Cirad)-Centre international d'études supérieures en sciences agronomiques (Montpellier SupAgro)-Université Montpellier 2 - Sciences et Techniques (UM2)-Université de Montpellier (UM)-Institut National de la Recherche Agronomique (INRA), Institut national d’études supérieures agronomiques de Montpellier (Montpellier SupAgro), Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Institut national d'enseignement supérieur pour l'agriculture, l'alimentation et l'environnement (Institut Agro)-Centre de Coopération Internationale en Recherche Agronomique pour le Développement (Cirad)-Centre international d'études supérieures en sciences agronomiques (Montpellier SupAgro)-Université Montpellier 2 - Sciences et Techniques (UM2)-Université de Montpellier (UM)-Institut National de la Recherche Agronomique (INRA), Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Institut Normand de Chimie Moléculaire Médicinale et Macromoléculaire (INC3M), Institut de Chimie du CNRS (INC)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut national des sciences appliquées Rouen Normandie (INSA Rouen Normandie), Institut National des Sciences Appliquées (INSA)-Normandie Université (NU)-Institut National des Sciences Appliquées (INSA)-Université Le Havre Normandie (ULH), Normandie Université (NU)-Université de Rouen Normandie (UNIROUEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)-Université de Caen Normandie (UNICAEN), Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Université Le Havre Normandie (ULH), and Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS)

Subjects
oxidation, [SDV]Life Sciences [q-bio], Aroma of wine, chemistry.chemical_element, Filtration and Separation, Biochemistry, Oxygen, Oxygen permeability, chemistry.chemical_compound, Crystallinity, polymère, pet, vin, Organic chemistry, Aroma compound, General Materials Science, Recycling, Physical and Theoretical Chemistry, wine, Aroma, Barrier properties, biology, food and beverages, oxydation, Sorption, biology.organism_classification, arôme, chemistry, 13. Climate action, Packaging, Oxygen scavenger, Nuclear chemistry
Abstract

Virgin PET, 100% recycled PET and PET containing an oxygen scavenger have been compared for their thermal properties and gas and aroma compound permeability. Thermal properties were slightly different between virgin and recycled PET, which exhibited the same degree of crystallinity but also strong heterogeneity in dispersion and size of crystals. However, glass transition was higher in the presence of oxygen scavenger because of its nature. Similar oxygen and carbon dioxide permeability were measured for virgin, recycled and PET with 1% of oxygen scavenger, whereas with 3% of oxygen scavenger gas barrier properties increased. Water barrier properties of PET were not influenced either by recycling or by the presence of oxygen scavenger and a plasticization effect was evidenced for all films. Concerning volatile organic compounds such as ethanol and aroma compounds, virgin PET was the best barrier. Permeability was strongly affected by the affinity of the compound for the material. Sorption of pure or diluted solution of ethanol induced changes in thermal properties with a slight decrease in Tg and a marked decrease of crystallinity. In contrast, the oxygen permeability after contact with the diluted solution of ethanol was increased, suggesting a reduction of free volume by sorption. Finally, the impact of film barrier properties on three aroma compounds of wine was evaluated and confirmed the inertness of PET concerning aroma compounds and the positive effect of active packaging.

Published
2014
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49. Fragility of unsaturated polyester resins cured with styrene: influence of the styrene concentration

Author

Michel Metayer, Stéphane Marais, Jean-Marc Saiter, F. Dreux, C. Cabot, E. Bureau, and K. Chebli

Subjects
Materials science, Polymers and Plastics, Organic Chemistry, Analytical chemistry, General Physics and Astronomy, Activation energy, Calorimetry, Heat capacity, Styrene, chemistry.chemical_compound, Fragility, Brittleness, chemistry, Polymer chemistry, Materials Chemistry, Glass transition, Stoichiometry
Abstract

Unsaturated polyester resins cured with varying styrene content (20–50% (w/w)) has been studied by calorimetry (DSC). We have evaluated the values of the heat capacity at the glass transition ΔCp=[Cp,l−Cp,g]T=Tg, the values of apparent activation energy Δh*, and the values of the fragility index m for each sample. It is found a constant value of ΔC p =0.29 J g −1 K−1 for all the samples while Δh* and m increase with the styrene content. These results discussed in regard with the strong fragile glass-formers concept indicate a character becoming more fragile when the amount of styrene increases. Introducing the “bead concept” proposed by Wunderlich, we show that the average elementary energy barrier that the molecular species (or relaxing units) must overstep during their relaxation process is unchanged whatever the content of styrene. The origin of the variations with the styrene content of the fragility behavior is understood by the increase of the bead number.

Published
2001
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50. Diffusion and permeation of water through unsaturated polyester resins—influence of resin curing

Author

Stéphane Marais, Trong Q. Nguyen, Jean Marc Saiter, Michel Metayer, and M. Labbé

Subjects
Polyester resin, chemistry.chemical_classification, Materials science, Polymers and Plastics, Organic Chemistry, technology, industry, and agriculture, General Physics and Astronomy, Permeation, Copolyester, Styrene, Polyester, chemistry.chemical_compound, chemistry, Polymerization, Materials Chemistry, Composite material, Glass transition, Curing (chemistry)
Abstract

The diffusion and permeation properties of liquid water through an isophthalic-maleic acid-propanediol-based copolyester resin were studied with a highly sensitive permeameter. The value of the parameters of the exponential dependence of the diffusion coefficient on the water concentration decreases with the curing extent, except that of the plasticization coefficient, which decreases after a post-curing at 120°C. Infrared-spectrophotometric and calorimetric data show that the curing involves mainly a polymerization of styrene during the curing at 25°C, and a crosslinking by the opening of the double bonds on the polyester chains in the subsequent curing step at 80°C. The water sorption by the resin results in a 20°C-decrease in the glass transition temperature of the water saturated resin, leading to the diffusivity enhancement by the plasticization effect.

Published
2000
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