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Automated evaluation of three dimensional ultrasonic datasetsOsman, Ahmad 14 June 2013 (has links) (PDF)
Non-destructive testing has become necessary to ensure the quality of materials and components either in-service or at the production stage. This requires the use of a rapid, robust and reliable testing technique. As a main testing technique, the ultrasound technology has unique abilities to assess the discontinuity location, size and shape. Such information play a vital role in the acceptance criteria which are based on safety and quality requirements of manufactured components. Consequently, an extensive usage of the ultrasound technique is perceived especially in the inspection of large scale composites manufactured in the aerospace industry. Significant technical advances have contributed into optimizing the ultrasound acquisition techniques such as the sampling phased array technique. However, acquisition systems need to be complemented with an automated data analysis procedure to avoid the time consuming manual interpretation of all produced data. Such a complement would accelerate the inspection process and improve its reliability. The objective of this thesis is to propose an analysis chain dedicated to automatically process the 3D ultrasound volumes obtained using the sampling phased array technique. First, a detailed study of the speckle noise affecting the ultrasound data was conducted, as speckle reduces the quality of ultrasound data. Afterward, an analysis chain was developed, composed of a segmentation procedure followed by a classification procedure. The proposed segmentation methodology is adapted for ultrasound 3D data and has the objective to detect all potential defects inside the input volume. While the detection of defects is vital, one main difficulty is the high amount of false alarms which are detected by the segmentation procedure. The correct distinction of false alarms is necessary to reduce the rejection ratio of safe parts. This has to be done without risking missing true defects. Therefore, there is a need for a powerful classifier which can efficiently distinguish true defects from false alarms. This is achieved using a specific classification approach based on data fusion theory. The chain was tested on several ultrasound volumetric measures of Carbon Fiber Reinforced Polymers components. Experimental results of the chain revealed high accuracy, reliability in detecting, characterizing and classifying defects.
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Mechanical Behavior Study of Microporous Assemblies of Carbon Nanotube and GrapheneReddy, Siva Kumar C January 2015 (has links) (PDF)
Carbon nanotubes (CNT) and graphene have been one of the noticeable research areas in science and technology. In recent years, the assembly of these carbon nanostructures is one of the most interesting topic to the scientific world due to its variety of applications from nano to macroscale. These bulk nanostructures to be applicable in shock absorbers, batteries, sensors, photodetectors, actuators, solar cells, fuel cells etc.
The present work is motivated to study the detailed compressive behavior of three dimensional cellular assemblies of CNT and graphene. The CNT foams are synthesized by chemical vapor deposition method. It is interesting to study the compressive behavior of CNT foam in the presence external magnetic field applied perpendicular to CNT axis. The peak stress and energy absorption capability of CNT foam enhances by four and nearly two times in the presence of magnetic field as compared to the absence of the magnetic field. In the absence of magnetic field the deformation of CNT foam is obtained elastic, plateau and densification regions. Further CNT foam is loaded with iron oxide nanoparticles of diameter is ~ 40nm on the surface and detailed study of the compressive behavior of the foam by varying iron nanoparticles concentration. The peak stress and energy absorption capability of CNT foam initially decreases with increasing the intensity of the magnetic field, further increases the intensity of the magnetic field the maximum stress and energy absorption capability increases which is due to magnetic CNT and particles align in the direction of the magnetic field.
CNT surfaces were further modified by fluid of different viscosities. The mechanical behavior of CNT foam filled with fluids of varying viscosities like 100%, 95% and 90% glycerol and silicone oil are 612, 237, 109 and 279 mPa-s respectively. The mechanical behavior of CNT foam depends on both the intensity of magnetic field and fluid viscosity. The non linear relation between peak stress of CNT and magnetic field intensity is σp(B, η) = σ0 ± α(B-B0) where σ0 is the peak stress at B = B0 , η is the fluid viscosity, parameter α depends on properties of the MR fluid and B0 is an optimum magnetic field for which peak stress is maximum or minimum depending on the fluid viscosity.
Graphene is assembled into a three dimensional structure called graphene foam. The graphene foam is infiltrated with polymer and study the detailed compressive behavior of graphene foam and graphene foam/PDMS at different strains of 20, 40, 60 and 70%. The maximum stress and energy absorption capability of graphene foam/PDMS is six times higher than the graphene foam. Also the graphene foam/PDMS is highly stable and reversible for 100 cycles at strains of 30 and 50%. The mechanical behavior of CNT, graphene foam, CNT/PDMS and graphene foam/PDMS is compared. Among all the foams, graphene foam/PDMS has shown the highest elastic modulus as compared to other foams. This behavior can be attributed to the wrinkles formation during the growth of graphene and a coupling between PDMS and interfacial interactions of graphene foam. Therefore it suggests potential applications for dampers, cushions and electronic packaging.
Furthermore, the interaction between nanoparticles and polymer in a novel architecture composed of PDMS and iron oxide nanoparticles is studied. The load bearing capacity of uniform composites enhanced by addition of nanoparticles, reaching to a maximum to 1.5 times of the PDMS upon addition of 5wt.% of nanoparticles, and then gradually decreased to 1/6th of PDMS upon addition of 20wt.% of nanoparticles. On the other hand, the load bearing capacity of architectured composites at high strains (≥40%) monotonically increased with addition of nanoparticles in the pillars.
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Desenvolvimento de blendas de poliestireno/composto de resíduo de borracha da indústria calçadista.SILVA, Divânia Ferreira da. 25 June 2018 (has links)
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Previous issue date: 2018-06-25 / Capes / O objetivo deste trabalho foi desenvolver blendas de poliestireno/composto de
resíduo de borracha de estireno-co-butadieno (PS/SBRr) da indústria calçadista
visando tenacificar o PS e reaproveitar o SBRr. As blendas foram preparadas nas
composições (70/30; 60/40 e 50/50%) em massa e com 5% do compatibilizante
estireno-butadieno-estireno (SBS). A fim de se estudar o efeito da sequência de
mistura, escolheu-se a composição 50/50% que apresentou o melhor resultado de
resistência ao impacto. As sequências realizadas foram: PS/SBRr/SBS
47,5/47,5/5%; PS/SBRr + SBS 47,5/47,5 + 5% e PS/SBS + SBRr 47,5/5 + 47,5%
em massa. As blendas foram preparadas por extrusão seguida de injeção e
caracterizadas por reometria de torque, tração, impacto, flexão, temperatura de
deflexão térmica (HDT), análise térmica dinâmico-mecânica (DMTA), calorimetria
exploratória diferencial (DSC), microscopia eletrônica de varredura (MEV) e
microscopia eletrônica de transmissão (MET). Observou-se nos resultados dos
ensaios mecânicos redução no módulo de elasticidade e na resistência à tração e
um aumento significativo na resistência ao impacto quando comparados ao PS
para todas as composições. A HDT das misturas reduziu pouco em relação ao
PS. A sequência de mistura proporcionou bons resultados das propriedades
mecânicas, principalmente na composição PS/SBS + SBRr 47,5/5 + 47,5% em
massa. Por MEV e MET, pôde-se observar que as blendas compatibilizadas
obtiveram uma melhor distribuição das partículas de borracha com uma
morfologia mais estável que as não compatibilizadas. Estes resultados foram
confirmados por meio dos maiores valores de resistência ao impacto, o que indica
a ação do compatibilizante melhorando a adesão entre os componentes desta
blenda. Por DMTA constatou-se que estas blendas são imiscíveis. Portanto, fica
evidenciada a importância da reutilização dos resíduos de borracha tanto para a
tenacificação do PS como também para a redução dos problemas causados ao
meio ambiente, quando estes são descartados de forma indevida. / The aim of this study was to develop blends of polystyrene/compound of rubber
waste (PS/SBRr) of the shoes industry aiming to tough the PS and to reuse the
SBRr. The blends were prepared in the compositions (70/30; 60/40 and 50/50
wt.%) and with 5 wt.% of styrene-butadiene-styrene compatibilizer (SBS). In order
to study the effect of mixing sequence, the 50/50 wt.% composition, which
presented the best result in impact strength, was selected. The sequences were
PS/SBRr/SBS 47.5/47.5/5%; PS/SBRr + SBS 47.5/47.5 + 5% and PS/SBS + SBRr
47.5/5 + 47.5 wt.%. The blends were prepared by co-rotational twin screw extruder
and molded by injection and characterized by torque rheometer, mechanical
properties, heat deflection temperature (HDT), dynamic mechanical thermal
analysis (DMTA), differential scanning calorimetry (DSC), scanning electron
microscopy (SEM) and transmission electron microscopy (TEM). From the
mechanical tests, a reduction in elastic modulus and tensile strength and a
significant increase in impact strength were observed in relation to PS. The HDT
for all blends was reduced compared to the PS. The mixing sequence showed
good results in mechanical properties, especially in composition PS/SBS + SBRr
47.5/ 5 + 47.5 wt.%. By SEM and TEM it can be seen that the compatibilized
blends presented a better distribution of the rubber particles with a morphology
that was more stable than the one that was not compatibilized. These results were
confirmed by the highest impact strength values, indicating the compatibiliz er
action that improves adhesion among the components of the blend. By DMTA it
was possible to state that these blends are immiscible. Hence, the importance of
the reusing of rubber wastes is evidenced both for toughening of the PS and for
the reduction of problems caused to the environment, when they are discharged
improperly.
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Influência da mercerização e irradiação por feixe de elétrons na aderência da fibra do ouriço da castanha do Brasil em matriz de polietileno de alta densidade / Influency of mercerization and electron beam irradiation on the adhesion between fibre from Brazil nut pod and a high density polyethilene matrixRejane Daniela de Campos 18 September 2015 (has links)
O interesse na utilização de fibras naturais com matrizes poliméricas para a preparação de compósitos espalhou-se rapidamente ao longo dos últimos anos. No entanto, a adesão interfacial entre a fibra e a matriz tem ainda de ser aperfeiçoada. Para melhorar a adesão entre os constituintes e, consequentemente as propriedades mecânicas e térmicas dos materiais, duas abordagens foram investigadas: a irradiação por feixe de elétrons e a mercerização. Este trabalho descreve a fabricação e caracterização de biocompósitos de polietileno de alta densidade e fibra do ouriço da castanha do Brasil que foram preparadas por duas metodologias diferentes: a primeira foi irradiar o compósito com 150 kGy e a segunda foi irradiar a matriz com 15 kGy e então produzir o compósito. Para ambas as metodologias foram utilizadas fibras naturais mercerizadas e não mercerizadas. O efeito dos tratamentos estudados para melhorar a adesão entre a fibra e a matriz polimérica foi avaliado através de caracterizações mecânica, química, térmica e morfológica. Com base neste estudo, observou-se que a fibra do ouriço da castanha do Brasil é um material tecnicamente viável para uso como reforço em compósitos poliméricos. Observou-se que o processo de irradiação da matriz seguida da produção dos compósitos é um método eficaz para melhorar as propriedades térmicas e mecânicas dos compósitos biopoliméricos e que, quando comparado com o processo de mercerização, esse método pode ser considerado mais ambientalmente correto (sem produtos químicos e sem geração de resíduo), mais barato e mais simples. / The interest in the use of natural fibres with polymeric matrix for the preparation of composite spread rapidly over the last years. However, the interfacial adhesion between the fiber and the matrix has to be improved. To improve the adhesion between the constituents and consequently the mechanical and thermal properties of materials, two approaches were investigated: electron beam irradiation and mercerization. This paper describes the fabrication and characterization of biocomposites compounds with high density polyethylene and fibre from Brazil nut pod that were prepared by two different methods: the first irradiating the composite with 150 kGy and the second was radiating matrix with 15 kGy and then produce the composite. For both methodologies, natural fibers, mercerized and non-mercerized were used. The effect of the treatments to improve adhesion between the fiber and the polymer matrix was evaluated through mechanical, chemical, thermal and morphology charcterization. Based on this study, it was observed that fibre from Brazil nut pod is a technically viable material for use as reinforcement in polymer composites. It was observed that the process of matrix irradiation followed by the composite fabrication is an effective method for improving the thermal and mechanical properties of the composites, when compared with mercerization process, this method can be considered more environmentally friendly (no chemicals, and without generating waste), cheaper and simpler.
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Mécanismes d’endommagement du polyamide-66 renforcé par des fibres de verre courtes, soumis à un chargement monotone et en fatigue : Influence de l’humidité relative et de la microstructure induite par le moulage par injection / Damage mechanisms in short glass fiber reinforced polyamide-66 under monotic and fatigue loading : Effect of relative humidity and injection molding induced microstructureArif, Muhamad Fatikul 25 March 2014 (has links)
Le présent travail s'appuie sur une approche expérimentale étendue visant l'identification des mécanismes d'endommagement en chargement quasi-statique et en fatigue du PA66/GF30, en prenant notamment en compte l'influence de la teneur en eau et de la microstructure induite par le moulage par injection. Les essais et les observations in situ au MEB mettent en exergue le rôle déterminant de l'humidité relative sur l'initiation, le niveau et la chronologie de l'endommagement. Une analyse par micro-tomographie aux rayons X sur des échantillons ayant subi un chargement de fatigue montre que l'endommagement augmente continuellement et progressivement au cours de la fatigue, et plus significativement dans la deuxième moitié de sa durée de vie. Les résultats obtenus en quasi-statique et en fatigue révèlent des mécanismes d'endommagement similaires, notamment une décohésion des interfaces fibre/matrice. Une chronologie générale de l'endommagement est établie. Celui-ci s'initie en extrémités de fibres ou plus globalement là où les fibres sont relativement proches les unes des autres. Il s'ensuit des décohésions interfaciales se propageant le long des fibres. A une contrainte en flexion plus élevée, des microfissures de la matrice peuvent apparaître et se propager par coalescence, ce qui aboutira à la rupture. Ces résultats expérimentaux permettent d'alimenter une modélisation multi-échelles de l'endommagement à fort contenu physique. Celle-ci contribuera alors à une prédiction pertinente de l'endommagement dans les thermoplastiques renforcés pour application automobile. / The current work focuses on extensive experimental approaches to identify quasi-static and fatigue damage behavior of PA66/GF30 considering various effects such as relative humidity and injection process induced microstructure. By using in situ SEM tests, it was observed that relative humidity conditions strongly impact the damage mechanisms in terms of their initiation, level and chronology. The X-ray micro-tomography analysis on fatigue loaded samples demonstrated that the damage continuously increases during fatigue loading, but the evolution occurs more significantly in the second half of the fatigue life. From the results of damage investigation under quasi-static and fatigue loading, it was established that both loading types exhibit the same damage mechanisms, with fiber/matrix interfacial debonding as the principal damage mechanisms. General damage chronologies were proposed as the damage initiates at fiber ends and more generally at locations where fibers are relatively close to each other due to the generation of local stress concentrations. Afterwards, interfacial decohesions further propagate along the fiber/matrix interface. At high relative flexural stress, matrix microcracks can develop and propagate, leading to the damage accumulation and then the final failure. The experimental findings are important to provide a physically based damage mechanisms scenarios that can be integrated into multiscale damage models. These models will contribute towards reliable predictions of damage in reinforced thermoplastics for lightweight automotive applications.
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Three-Dimensional Graphene Foam Reinforced Epoxy CompositesEmbrey, Leslie 27 March 2017 (has links)
Three-dimensional graphene foam (3D GrF) is an interconnected, porous structure of graphene sheets with excellent mechanical, electrical and thermal properties, making it a candidate reinforcement for polymer matrices. GrF’s 3D structure eliminates nanoparticle agglomeration and provides seamless pathways for electron travel. The objective of this work is to fabricate low density GrF reinforced epoxy composites with superior mechanical and electrical properties and study the underlying deformation mechanisms. Dip coating and mold casting fabrication methods are employed in order to tailor the microstructure and properties. The composite’s microstructure revealed good interfacial interaction. By adding mere 0.63 wt.% GrF, flexural strength was improved by 56%. The addition of 2 wt.% GrF showed a surge in glass transition temperature (56oC), improvement in damping behavior (150%), and electrical conductivity 11 orders of magnitude higher than pure epoxy. Dip coated and mold casted composites showed a gauge factor of ~2.4 indicating electromechanically robust composite materials.
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Adaptation du procédé RTM (Moulage par Transfert de Résine) à la mise en œuvre de matériaux composites à matrice thermoplastique / The adaptation of the RTM (Resin Transfer Molding) process to manufacture thermoplastic-based compositesVan den Broek d'Obrenan, Ghislain 08 November 2011 (has links)
Le procédé « Resin Transfer Molding » (RTM) est très largement utilisé pour la production industrielle de matériaux composites à matrice thermodurcissable. En effet, de nombreux domaines tels que l’automobile et l’aéronautique l’emploi couramment. Dans ce travail nous avons adapté ce procédé à la mise en œuvre de matériaux composites à matrice thermoplastique afin de répondre aux critères écologiques et économiques imposés aux industries. Pour cela plusieurs étapes ont été nécessaires. La première fut la sélection d’une chimie robuste, adaptée aux exigences du procédé (faible viscosité initiale du système réactif, temps de polymérisation court, etc). La chimie choisie fut la polymérisation anionique par ouverture de cycle de l’ε-caprolactame dans le but d’obtenir du polyamide-6 (PA-6). Une étude rhéo-cinétique ainsi que les caractérisations physico-chimiques d’un PA-6 obtenu au laboratoire furent réalisé. A la suite de cette étape, des essais en conditions de procédé ont été effectué avec l’utilisation d’un équipement pilote dédié. Ces essais furent la source de modifications et d’optimisations de certains paramètres du procédé. La troisième étape, a consisté à la production de pièces composites avec un renfort de type : tissu unidirectionnel de verre. Cette production fut suivie de tests mécaniques et physico-chimiques afin d’évaluer les propriétés de ces pièces. Différents ensimages de tissu ont été étudiés avec, pour objectif, la détermination de celui offrant les meilleures propriétés. Durant cette étude nous avons observé que la nature de l’ensimage impactait peu la chimie. Pour finir, nous avons mis en place un ensimage réactif qui permettra une meilleure interaction fibre/matrice. / The "Resin Transfer Molding" (RTM) process is very largely used for the industrial production of composites materials with thermoset matrix. Indeed, it’s used by many fields such as the automotive and aeronautics. In this work we adapted this process to the manufacture of composite materials with thermoplastic matrix in order to answer the ecological and economic criteria imposed on industries. For that several steps were necessary. The first was the selection of a robust chemistry, adapted to the requirements of the process (low initial viscosity of the reactive system, polymerization time, etc). The selected chemistry, was the ring opening polymerization of ε - caprolactam to obtain polyamide-6 (PA-6). Rhéo-kinetics studies, as well as the physicochemical characterizations of a Pa-6 obtained at the laboratory were carried out. Following this step, tests in conditions of process were carried out with the use of dedicated pilot equipment. These tests were the source of modifications and optimizations of certain parameters of the process. The third step, consisted with the production of composite parts with a reinforcement of the type: unidirectional glass fabric. This production was followed mechanical and physico-chemical tests in order to evaluate the properties of these parts. Various sizing of the glass fabric were studied with, for objective, to determine which to offer the best properties. During this study we observed the low impact of the sizing on the chemistry of PA-6. To finish, we set up a reactive sizing which will allow a better interaction fibre/matrix.
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Structuration de nanocomposites à partir de copolymères à blocs : expérience et modélisation / Structuring nanocomposites from copolymers block : experience and modelingPeng, Zhen 27 February 2012 (has links)
Les copolymères à blocs sont des matériaux très intéressants en raison de leur capacité à s’auto-organiser pour former des domaines de quelques dizaines de nanomètres. Cette organisation peut être mise à profit pour obtenir des matériaux hybrides organiques/inorganiques dans lesquels la phase inorganique peut être structurée dans un des domaines plutôt que répartie de façon aléatoire. Ceci peut conférer des propriétés particulières aux copolymères hybrides. Notre travail de thèse s’inscrit dans cette problématique. Des copolymères à blocs ont été modifiés soit par greffage en solution de molécules organiques/inorganiques du type POSS réactif (polyhedral oligomeric silsesquioxane), soit par mélange en solution ou à l’état fondu de POSS non réactif. Les copolymères triblocs considérés sont du type SBS (styrène-butadiène-styrène) et SEBS-g-MA (styrène-éthylène-butène-styrène greffé anhydride maléique). L’ensemble de ces copolymères a été caractérisé expérimentalement afin de déterminer leur morphologie et leur comportement thermo-mécanique. En parallèle une approche théorique a été proposée, basée sur la modélisation moléculaire de ces copolymères à l’échelle mésoscale. La méthode sélectionnée ‘Dissipative Particle Dynamics’ a permis de modéliser la morphologie de nos copolymères avec succès ainsi que celle de nos matériaux hybrides modifiés par les POSS. Ces derniers peuvent être dispersés à l’échelle moléculaire ou au contraire former des agrégats, selon le procédé de mise en œuvre et la structure chimique des POSS. / Experimental approaches and a modeling method have been carried out in parallele. The simulation method was used firstly to confirm the experimental results, and then will be applied to more complex nanocomposites. A series of hybrid systems based on triblock copolymer of polystyrene-butadiene-polystyrene (SBS) grafted with polyhedral oligomeric silsesquioxane(POSS) molecules with a dimethylsiloxy group (DMIPOSS) were synthesized by a hydrosilation method. The characteristics on incorporation of an unreactive POSS with constituent cyclohexyl (CyPOSS) in SBS matrix have been compared with above systems. The nanocomposites obtained were analyzed by atomic force microscopy, Transmission electron microscopy, X-ray scattering and dynamic mechanical.The same strategy has been carried out on polystyrene-b-poly (ethylene-co-butylene)-b-polystyrene-g-maleic anhydride (SEBS-g-MA) with other type of POSS. Dynamic particles dissipative (DPD) simulation methods in Materials Studio (Accelrys) were employed to study morphology of SB, SBS, SEBS and hybrid system. In this mesoscopic method, the polymer is simplified as a series of connecting beads which contains one or more monomer units. And all monomer units interact with each other following Newtonian Equations of Motion.
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Study on RAFT polymerization and nano-structured hybrid system of POSS macromers / Étude sur la polymérisation RAFT et nanostructurés système hybride de macromères POSSDeng, Yuanming 08 June 2012 (has links)
Ce travail est généralement destiné à synthétiser BCPs à base d'POSS par polymérisation RAFT, à étudier leurs comportements d'auto-assemblage, à la recherche sur l'effet de POSS auto-assemblage structure sur les propriétés en vrac et à préparer nanostructuré époxy hybride par auto-assemblage de la copolymère base d’POSS. Dans le Chapitre1, Nous avons étudié la polymérisation RAFT de macromères POSS et capables de synthétiser bien définis BCPs à base d'POSS avec la fraction POSS élevé et une topologie différente tels que AB, BAB et (BA)3. Le groupe de vertex et l'effet sur la morphologie propriétés thermo-mécaniques de BCPs à base d'POSS et la relation structure-propriété ont été investigated Polymérisation RAFT dispersion dans solvant apolaire a été appliquée pour obtenir divers agrégats ayant une morphologie différente dans Chapitre2. Refroidissement de transition induite morphologie réversible a été trouvé et la sélection dans la formation des vésicules voie a été étudiée. Nano-construction de matériaux O/I époxy hybrides à base de copolymères à base d'POSS a été étudiée dans Chapitre 4. L'effet de la teneur en groupe fonctionnel sur la miscibilité de copolymère statistique base d’POSS et de l'époxy a été étudiée. Une nouvelle méthode à la technologie hybride époxy nanostructure impliquant l'auto-assemblage de BCPs à base d'POSS en résine époxy a été présenté. Homogénéité élevée et bien la taille/morphologie de contrôle de coeur-corona structure contenant coeur POSS rigide et soluble dans les réseaux corona PMMA ont été obtenus. / This work is generally aimed to synthesize POSS based BCPs via RAFT polymerization, to study their self-assembly behaviors, to research on the effect of POSS self-assembly structure on the bulk properties and to prepare nanostructured hybrid epoxy via self-assembly of POSS based copolymer. In Chapter1, We studied the RAFT polymerization of POSS macromers and capable to synthesize well defined POSS based BCPs with high POSS fraction and different topology such as AB,BAB and (BA)3. The vertex group and the morphology effect on thermo-mechanical properties of POSS based BCPs as well as the structure-property relationship was investigated. Dispersion RAFT polymerization in apolar solvent was applied and various aggregates with different morphology in Chapter2. Cooling induced reversible micelle formation and transition was found and the pathway selection in vesicle formation was investigated. Nano-construction of O/I hybrid epoxy materials based on POSS based copolymers was investigated in Chapter4. The effect of functional group content on miscibility of POSS based statistic copolymer and epoxy was investigated. A novel method to nanostructure epoxy hybrid involving self-assembly of POSS based BCPs in epoxy was presented. High homogeneity and well size/morphology control of core-corona structure containing rigid POSS core and soluble PMMA corona in networks were obtained.
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Elaboration de matériaux hybrides organiques / inorganiques par extrusion réactive : Application en pile à combustible / Synthesis of organic-inorganic hybrids via combination of sol-gel chemistry and reactive extrusion for fuel cells applicationSeck, Serigne 03 May 2013 (has links)
A l’heure actuelle, les piles à combustible à membrane échangeuse de protons (PEMFC) les plus avancées, qu’elles soient disponibles commercialement ou intégrées dans des démonstrateurs, sont réalisées avec des électrolytes polymères perfluorosulfonés de types Nafion®. En effet, ce type de polymère est celui qui présente à la fois les meilleures performances et la plus grande durée de vie sans pour autant qu’elles soient suffisantes, et ce, quelles que soient les applications (portable, stationnaire, transport). En effet ce polymère présente toutefois trois inconvénients majeurs : son prix, sa perméation au méthanol et sa perte de performance (et surtout de conductivité) dès 80-85 °C. Selon les projections avec les technologies actuelles (source DOE), le prix de vente du Nafion® serait de 80 $/m2 pour une production de 1 Mm2. Il existe un réel besoin de développer de nouveaux matériaux pour membranes échangeuses de protons présentant d’excellentes performances (propriétés mécaniques, imperméabilité maximale au méthanol et H2, conduction protonique..) sur une large gamme de températures, typiquement entre 25 et 150°C (selon l’application visée), mais présentant également un coût de fabrication réduit. Or aujourd’hui, ces différentes fonctions sont assurées par un seul polymère perfluorosulfoné ce qui est le problème principal. Ainsi, l’intérêt du projet est de combiner les avantages d’un matériau hybride obtenu par génération in situ de la phase inorganique (Sol-Gel) nanométrique avec l’utilisation d’un procédé en continu de mise en œuvre par extrusion (voie fondu), exempt de tout solvant et facilement transférable industriellement. La conduction protonique sera assurée par des fonctions sulfoniques générées grâce à l'oxydation des sites fonctionnels apportés par le précurseur fonctionnel. / Fuel cells technologies are electrochemical energy conversion devices and have a real potential to revolutionize the way to produce energy, offering cleaner, more-efficient alternatives to combustion of gasoline and other fossil fuels. In that way, the Proton Exchange Membrane Fuel Cells (PEMFC) are probably the most studied. Those fuel cells are mainly based on perfluorosulfonic acid membranes, such as Nafion®. However, Nafion® membranes, present some limitations such as dehydration at high temperatures or at low relative humidity rate leading to a decrease of proton conductivity and thus poor PEMFC performance. Consequently, PEMFC require significant improvements prior to be largely used in the automobile field. Research efforts have been oriented on the development of new materials for the PEMFC membrane as it is the main limitative component for high temperature fuel cell. In the present contribution, we wish to report the validation of a new concept of hybrid materials for the realization of proton exchange membranes. The originality of this hybrid concept is based on the contribution of both phases’ specific properties. We investigated the preparation of hybrid materials based on an inert polymer matrix (low cost) providing the mechanical stability embedding inorganic phase providing the necessary properties of proton-conduction and water retention. Hybrid nanocomposite membranes were synthesized using evaporation and recasting technique from solution containing dispersion of inorganic particles in the adequate polymer. Scanning electron microscopy (SEM) images for membrane morphology and proton conductivity results using impedance measurements from hybrid membranes will be presented. The performance of the membrane-electrode assembly (MEA) using the hybrid membrane was also evaluated by a fuel cell test. Finally, we wish to present a promising way of research based on Sol-Gel approach to generate a proton-conducting inorganic phase into the polymer matrix.
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