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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
111

Strategies for building polymers from renewable sources : Using prepolymers from steam treatment of wood and monomers from fermentation of agricultural products

Söderqvist Lindblad, Margaretha January 2003 (has links)
<p>A strategic research area today is development of polymericproducts made from renewable sources. The ways of utilizingrenewable sources studied in this thesis are using 1)prepolymers obtained by steam treatment of wood and 2) monomersobtainable by fermentation of agricultural products.</p><p>Novel hemicellulose-based hydrogels were prepared by usingprepolymers obtained from steam treatment of spruce.Hemicellulose was first modified with well-defined amounts ofmethacrylic functions. Hydrogels were then prepared by radicalpolymerization with 2-hydroxyethyl methacrylate orpoly(ethylene glycol) dimethacrylate to form hydrogels. Theradical polymerization reaction was carried out in water usinga redox initiator system. The hydrogels were in generalelastic, soft and easily swollen in water. Frequency sweeptests indicated that the hydrogel system displayed prevailingsolid-like behavior. Comparison of the hemicellulose-basedhydrogels with pure poly(2-hydroxyethyl methacrylate)-basedhydrogels showed that it was possible to preparehemicellulose-based hydrogels with properties similar to thoseof pure poly(2-hydroxyethyl methacrylate)-based hydrogels.</p><p>Polyester-based materials were prepared by using themonomers 1,3- propanediol and succinic acid obtainable byfermentation. α,ω-Dihydroxyterminatedoligomeric polyesters produced by the thermal polycondensationof 1,3-propanediol and succinic acid were chain-extended toobtain sufficiently high molecular weight. Depending on thechain-extension technology adopted, poly(ester carbonate)s orpoly(ester urethane)s were obtained. In the case of poly(estercarbonate)s, the chain-extended products ofα,ω-dihydroxyterminated oligomeric copolyesters werealso produced using 1,3-propanediol/1,4-cyclohexanedimethanol/succinic acid mixtures toimprove thermal and mechanical properties. Segmented poly(esterether carbonate)s fromα,ω-dihydroxyterminated oligo(propylenesuccinate)s and poly(ethylene glycol) were also synthesized toincrease the hydrophilicity.</p><p>Molecular weights and polydispersity were analyzed by SECfor all materials. Their structures were also identified by NMRspectroscopy (1H NMR and 13C NMR). All characterizations werein agreement with the proposed structures. Thermal parameterswere characterized by DSC. Tensile testing anddynamic-mechanical tests were performed and in additionpreliminary processing trials were carried out in some cases.The results demonstrate the feasibility of using monomersderived from renewable sources to build up new polymericstructures endowed with a variety of physical and mechanicalproperties.</p>
112

Rôle des anomalies de transmission des contraintes dans la pathogénèse des maladies fémoro-acétabulaires / Key role of strains' transmission abnormality as an origin of femoro-acetabular diseases

Ollivier, Matthieu 07 December 2016 (has links)
Dans le cadre de ce travail de thèse nous nous sommes intéressés à deux pathologies fémoro-acétabulaires dont la pathogénie semble liée aux « conditions biomécaniques » locales. La première partie de cette thèse était consacrée à l’analyse de l’influence de l’anatomie osseuse sur l’apparition de l’ostéonécrose aseptique de la tête fémorale. Nous avons réalisé des analyses analytique de l’anatomie des patients souffrant d’ONA (notre hypothèse était que nous retrouverions un profil anatomique particulier chez les patients souffrant d’ONA par rapport à la population générale.Nos résultats démontrent que les patients souffrant d’ONA présentent fréquemment une anatomie particulière. Notre modèle en éléments finis de la hanche de dix patients souffrant d’ONAi, a permis de valider notre hypothèse puisqu’il existe un recouvrement quasi-parfait, entre la zone de nécrose osseuse et celle supportant les contraintes fémoro-acétabulaires. L’hypothèse selon laquelle une pathogénie mécanique puisse être responsable du développement l’ostéonécrose aseptique de la tête fémorale est vérifiée par nos travaux.Dans la seconde partie de cette thèse nous avons décrit le rôle mécanique du LA par une évaluation multimodale combinant analyse cinématique,de contraintes fémoro-labrales et enfin analyse en éléments finis. Les résultats de ces études ont permis de constater que le LA se déforme lors du mouvement reflétant une transmission de contraintes fémoro-labrales lors du mouvement d’abduction. Ces contraintes ont pu être enregistrées à l’aide de capteurs piezo-resistifs, elles augmentent lors du mouvement d’abduction. Ces éléments ont été confirmés par notre modèle en éléments finis. / As parts of this thesis we focused on two femoro-acetabular diseases whose pathogenesis appears to be related to "biomechanical local conditions". The first part of this thesis was devoted to analyze the influence of bony anatomy on the development of aseptic osteonecrosis of the femoral head. We thus aimed to analyze ONA patients’ anatomy in a matched-controlled fashioned study. Our results demonstrate that patients with ONA often present a particular anatomy. A finite element model of ten iONA hips validated our hypothesis since we found an overlap between bone necrosis area and femoro-acetabular strains bearing area. The assumption that a mechanical pathogenesis may be responsible for ONA development has been confirmed by our results.If the relationship between bony anatomy and bone disease is quite intuitive, acetabular labrum involvement (AL) in the regulation of femoro-acetabular mechanical conditions is unclear. The mechanical role of the AL is widely controversial, though some authors attributed, AL, a key role in hip joint’s mechanics, others advocated its complete resection in case of painful traumatic tears. We tried to demonstrate AL’s mechanical role in a multimodal analysis combining kinematic, strains and finite element analysis. The AL deforms during abduction movement reflecting femoro-labral strains’ transmission. Those strains have been recorded using piezo-resistive sensors, they increase during adduction to abduction movement. These elements were confirmed by our finite element model: labral resection changed the Femoro-acetabular strains to the detriment of cartilage surfaces.
113

Evolution microstructurale et comportement mécanique des composites à base de MgH₂ au cours des cycles d'hydruration / Microstructural evolution and mechanical behavior of MgH₂ based composites during hydorgenation cycles

Nachev, Simeon 05 October 2015 (has links)
Lors de la dernière décennie, l’hydrure de magnésium est apparu comme le candidat le plus intéressant pour le stockage solide de l’hydrogène à grande échelle. La présente étude s’est intéressée au gonflement irréversible de composites à base d’hydrure de magnésium durant les cycles d’hydruration/déshydruration ainsi qu’à l’évolution de leurs propriétés mécaniques.Les expériences de dilatométrie in-situ et les caractérisations microstructurales (MEB,granulométrie), menées sur des échantillons de MgH₂co-broyés avec des additifs devanadium ou Ti-V-Cr ont montré que la coalescence des particules nanométriques favorise la formation de larges agglomérats qui induisent une augmentation de la porosité et qui expliquent le gonflement irréversible des composites.Les tests de nano-indentation ont montré une augmentation du module de Young de plus de 30 % après 10 cycles d’hydruration/déshydruration. Les mesures de la dureté Vickers sur des pastilles de MgH2 sans additif ont permis d’estimer sa dureté en fonction de la densité relative. Ainsi la dureté d’une pastille qui aurait une densité proche de la densitéthéorique (95 %) a été extrapolée à 0.58 GPa. / The last decade the magnesium hydride stood out as the most attractive candidatefor solid storage of hydrogen at large scale. The main subject of this study is thephenomenon of irreversible swelling of the composites based on magnesium hydride, duringthe hydriding/dehydriding cycles as well as the evolution of their mechanical properties.In-situ dilatometry measurements and the microstructural characterizations (SEM,granulometry) were performed on magnesium hydride samples co-milled with vanadium orTi-V-Cr additive. The results reveal that the coalescence of nanometric particles tends tocreate large agglomerates, which induce an increase in porosity, and explain the progressiveswelling of composites.The nanoindentation tests performed on compacted pellets show an enhancement ofabout 30 % of the Young modulus after 10 cycles. From the Vickers hardness measured oncompacted powders, the hardness of a highly densified magnesium hydride wasextrapolated to 0.58 GPa, which shows that the magnesium hydride is harder thanmagnesium.
114

Determinação de parâmetros mecânicos para dimensionamento de pavimentos com resíduos de construção e demolição / Determination of mechanical parameters for pavement design with construction and demolition waste

Delongui, Lucas January 2016 (has links)
Os processos de reciclagem e produção de agregados reciclados provenientes de resíduos de construção e demolição (RCD) estão se consolidando no Brasil, mas o seu emprego não ocorre na mesma proporção. A utilização desses em pavimentação, principalmente em camadas de base e sub-base, é considerada mais conveniente que em outras áreas, visto que não necessita de procedimentos avançados de reciclagem e utiliza os mesmos processos construtivos que agregados já consagrados, como britas graduadas. Entretanto, as recomendações normativas existentes remetem à caracterização dos agregados, sendo que as alusões ao seu comportamento mecânico são idênticas às impostas para britas graduadas. Além disso, a literatura existente é limitada frente a outros materiais alternativos, o que implica restrições ao seu emprego. Buscando atenuar essas incertezas, essa pesquisa tem como objetivo analisar o comportamento mecânico de agregados reciclados provenientes de RCD, de modo a identificar suas principais características e fornecer parâmetros de anteprojeto para o dimensionamento de pavimentos que utilizam esse material como camadas de suporte. Para isso, a primeira etapa comportou uma análise dos processos de beneficiamento dos agregados reciclados, de modo a identificar como influem nas suas características, o que foi alcançado concomitantemente a segunda etapa, que consistiu na análise dos agregados por meio de ensaios específicos de caracterização física e química. A terceira e principal etapa baseou-se na análise do comportamento mecânico, que além da determinação em equipamentos convencionais, também utilizou um equipamento triaxial de grande porte que comporta corpos de prova de 25 x 50 cm, permitindo a utilização da distribuição a ser empregada em campo. Essa etapa iniciou pela análise da compactação, realizada com curvas granulométricas e modos de umedecimento distintos, onde os mais promissores foram escolhidos para verificar a influência do método de compactação, sendo ele dinâmico ou vibratório. Após essas determinações, a análise concentrou-se no módulo de resiliência, na resistência ao cisalhamento e na deformação permanente, sendo que as evoluções da deformação permanente foram classificadas segundo a teoria do Shakedown. Os resultados demonstraram que a compactação causa a quebra de agregados, porém essa é menor quando utilizada compactação dinâmica. Os RCD apresentaram bom comportamento em relação deformações elásticas, com módulo de resiliência semelhantes aos apresentados por britas. Dado a diminuição de partículas lamelares causada pela quebra durante o processo de compactação, os valores mais representativos do ângulo de atrito e do intercepto coesivo foram 41° e 60 kPa, respectivamente. As análises das deformações realizadas em multiestágios demonstraram que, se utilizados em pavimentos com baixo de volume de tráfego, para razões de tensões σd / σ3 < 2 e tensões desvio σd ≤ 210 kPa, bases compostas de RCD não vão desenvolver deformações plásticas iniciais excessivas e o material vai responder elasticamente. Além disso, essas bases estão seguras contra falhas de cisalhamento. Em suma, as análises indicam que os RCD podem ser utilizados como materiais para bases e sub-bases de pavimentos de baixo volume de tráfego, dando um destino nobre a uma matéria-prima renovável e facilmente encontrada, que na maioria das vezes é desperdiçada e cuja geração aumenta constantemente. / Construction and Demolition Waste (CDW) recycling processes are consolidating in Brazil, but their use does not occur in the same proportion. The application of such in pavement, especially in base and sub-base layers, it is considered more convenient than in other areas because it does not require advanced recycling procedures and using the same constructive processes which aggregates already established, as graded gravel. However, existing normative recommendations refer to the characterization of the aggregates, and the allusions to their mechanical behavior are identical to those imposed on graded gravel. Moreover, the existing literature is limited compared to other alternative materials, implying restrictions on its use. Seeking to mitigate these uncertainties, this research aims to analyze the mechanical behavior of recycled aggregates from CDW, in order to identify its main characteristics and provide parameters for draft design of pavements that using this material as a support layer. For this, the first step involved an analysis of the aggregates recycling procedures, in order to identify the influence of this process in their characteristics, which were concomitantly reached the second stage consisting in the analysis of aggregate by specific tests of physical and chemistry characterization. The third and main step was based on the analysis of mechanical behavior, which besides determining in conventional equipment also utilized a large triaxial device that carries specimens of 25 x 50 cm, allowing the use of the distribution to be employed in field. This step began by analyzing the compaction performed with gradation curves and distinct modes of moistening, where the most promising were chosen to investigate the influence of compaction method, either dynamic or vibration. After these determinations, the analysis focused on the resilient modulus, shear strength and permanent strain, and the evolution of permanent strain were classified according to the theory of Shakedown. The results showed that compaction causes the aggregates break, but this is less when used dynamic compaction. The CDW had good behavior relative elastic strains, with resilient modulus similar to those presented by gravel. Since the decrease of lamellar particles caused by breakage during the compaction process, the most representative values of the friction angle and cohesive intercept were 41° and 60 kPa, respectively. The analysis of the permanent strain carried out in multistage demonstrated that if used in pavements with low traffic volume, for reasons of stress σd / σ3 < 2 and deviator stress σd ≤ 210 kPa, compound bases CDW will not develop excessive initial plastic strain and the material will respond elastically. In addition, these bases are secure against shear failure. In essence, the analysis indicates that the CDW can be used as materials for bases and sub-bases of low volume traffic floors, giving a noble destiny to a renewable raw material and easily found that most of the time is wasted and whose generation is constantly increasing.
115

Compréhension des relations entre l'état mécanique et le fonctionnement d'une pile à combustible de type PEMFC à l'aide d'une approche duale expérimentale et prédictive / Optimisation of PEM fuel cell operation through a double approach experimental and predictive

Carral, Christophe 08 December 2014 (has links)
Dans le cadre du projet collaboratif FUI "HyPlate", cette étude apporte une contribution originale dans la compréhension des mécanismes impliqués lors de l'assemblage d'une pile à combustible de type PEMFC, à l'aide de la mesure ou de la prédiction des déformations et des contraintes mécaniques dans le cœur de pile ou MEA. Basée sur une analyse multi-échelle, une approche duale expérimentale et prédictive a été menée, comprenant le développement non seulement de nouvelles méthodes de mesures expérimentales mais également un modèle numérique 3D, basé sur la méthode des éléments finis. Le couplage des différents résultats expérimentaux et simulés a permis de déterminer, dans un premier temps, le niveau de contraintes (ou de déformations) dans les différents composants du stack en fonction des conditions d'assemblage, et d'analyser, dans un second temps, l'influence de différents paramètres, tels que les propriétés des matériaux des plaques bipolaires, le nombre de cellules et leur position. Il a notamment été montré que la distribution des déformations dans le cœur de pile diminuait avec le nombre de cellules et au centre du stack. Des modifications sur le système de serrage de la pile ont alors été proposées afin d'améliorer l'homogénéité de l'état mécanique global. Des mesures de force in-situ ont alors permis de valider certaines propositions et d'analyser l'influence de deux modes de serrage, en contrainte ou déformation imposée, sur la performance électrochimique de la pile. / Within the context of the FUI project "HyPlate", this thesis bring an original contribution in the understanding of the mechanisms implied during the assembly of a Proton Exchange Membrane Fuel Cell (PEMFC), through the measurements and the predictions of the mechanical stresses and strains in the fuel cell core, also known as the MEA. Based on a multi-scale analysis, a double approach experimental and predictive was followed, including not only the development of new experimental measurement methods but also a 3D numerical model, based on the finite element method. The results gathered from these two studies allowed us to determine, in a first step, the stress (or strain) level within the different stack components according to the assembly conditions, and to analyze, in a second step, the influence of different parameters such as the bipolar plate mechanical properties, the number of cells and their position. It was notably shown that the MEA strain distribution decreased with the number of cells and at the center of the stack. Some modifications of the clamping system were proposed in order to enhance the global mechanical state homogeneity. In situ measurements of the clamping force allowed us to validate some propositions made and to analyze the influence of two clamping modes, implying a constant stress or strain, on the electrochemical performance of the fuel cell.
116

Comportamento numérico e vida em fadiga de elastômeros clorados em função da temperatura

Krützmann, Moisés Henrique January 2015 (has links)
O conhecimento do comportamento mecânico do material é vital para a previsão da durabilidade e atendimento aos requisitos iniciais de projeto. Por meio de ensaios experimentais é possível mensurar esse comportamento e utilizar como parâmetro de entrada em simulações numéricas. Nesse ponto a temperatura altera significativamente as propriedades mecânicas estáticas e dinâmicas do material. Testes de fadiga devem ser considerados na caracterização do material mesmo que um alto custo e tempo sejam necessários. Assim o objetivo deste trabalho é avaliar o comportamento termo-mecânico do policloropreno em tração e fadiga. Este estudo se fez necessário para prever a durabilidade em diversas temperaturas em mancais de rolamento de cardans que exigem rigidez e durabilidade. A abordagem proposta consiste em formular equações constitutivas que considerem as constantes dependentes da temperatura para a situação estática (ensaio de tração) e dinâmica (ensaio de fadiga). Foram estudados 4 modelos constitutivos já consagrados na literatura. Corpos de prova normatizados foram utilizados para a avaliação experimental do material tanto em tração quanto em fadiga. Pode-se concluir que esta abordagem conseguiu modelar adequadamente o comportamento mecânico em ambas as situações estudadas. / Mechanical behavior of materials is vital for predicting durability and compliance with initial requirements of the project. Through experimental tests can measure this behavior and use as an input parameter in numerical simulations. At this point temperature significantly changes static and dynamic mechanical properties of the material. Fatigue tests should be considered in material characterization even if a high-cost and time are required. So the aim of this study is evaluate the thermo-mechanical behavior of polychloroprene in tension and fatigue. This study was necessary to predict durability in various temperatures in driveshafts of rolling bearings that requires rigidity and durability. The proposed approach is formulating constitutive equations to consider the dependent constant temperature for static situation (tensile test) and dynamic (fatigue test). Four constitutive models already established in literature were studied. Standardized test specimens were used for the experimental evaluation of the material both in tension and in fatigue. It can be concluded that this approach could adequately model the mechanical behavior in both cases studied.
117

Chaotic electron transport in semiconductor devices

Scannell, William Christian, 1970- 06 1900 (has links)
xix, 171 p. : ill. (some col.) A print copy of this thesis is available through the UO Libraries. Search the library catalog for the location and call number. / The field of quantum chaos investigates the quantum mechanical behavior of classically chaotic systems. This dissertation begins by describing an experiment conducted on an apparatus constructed to represent a three dimensional analog of a classically chaotic system. Patterns of reflected light are shown to produce fractals, and the behavior of the fractal dimension D F is shown to depend on the light's ability to escape the apparatus. The classically chaotic system is then used to investigate the conductance properties of semiconductor heterostructures engineered to produce a conducting plane relatively free of impurities and defects. Introducing walls that inhibit conduction to partition off sections considerably smaller than the mean distance between impurities defines devices called 'billiards'. Cooling to low temperatures enables the electrons traveling through the billiard to maintain quantum mechanical phase. Exposure to a changing electric or magnetic field alters the electron's phase, leading to fluctuations in the conductance through the billiard. Magnetoconductance fluctuations in billiards have previously been shown to be fractal. This behavior has been charted using an empirical parameter, Q , that is a measure of the resolution of the energy levels within the billiard. The relationship with Q is shown to extend beyond the ballistic regime into the 'quasi-ballistic' and 'diffusive' regimes, characterized by having defects within the conduction plane. A model analogous to the classically chaotic system is proposed as the origin of the fractal conductance fluctuations. This model is shown to be consistent with experiment and to account for changes of fine scale features in MCF known to occur when a billiard is brought to room temperature between low temperature measurements. An experiment is conducted in which fractal conductance fluctuations (FCF) are produced by exposing a billiard to a changing electric field. Comparison of D F values of FCF produced by electric fields is made to FCF produced by magnetic fields. FCF with high D F values are shown to de-correlate at smaller increments of field than the FCF with lower D F values. This indicates that FCF may be used as a novel sensor of external fields, so the response of FCF to high bias voltages is investigated. / Adviser: Stephen Kevan, Chairperson, Physics; Richard Taylor, Advisor, Physics; Robert Zimmerman, Member, Physics; Stephen Gregory, Member, Physics; David Johnson, Outside Member, Chemistry
118

Les bétons bas pH : comportements initial et différé sous contraintes externes / Low pH concretes : instantaneous and delayed behaviors under external stress

Leung Pah Hang, Thierry 22 May 2015 (has links)
Dans le cadre du stockage des déchets radioactifs en couches géologiques profondes (argilite du Callovo-Oxfordien), des bétons à faible alcalinité et à faible chaleur d'hydratation référencés "bas pH " ont été élaborés. L'utilisation de ces types de béton permet de limiter la dégradation des propriétés confinantes du matériau argileux type bentonite. Deux bétons bas pH à base de liants ternaires ont étudiés : un composé de ciment, fumée de silice et cendres volantes (TCV) et l'autre composé de ciment, fumée de silice et laitier moulu de haut fourneau (TL). L'objectif de l'étude est d'analyser le comportement de ces matériaux pour s'assurer : d'une mise en œuvre correcte à l'échelle industrielle, d'une bonne tenue chimique et mécanique dans le temps et d'un confinement performant. Le programme expérimental comprend la caractérisation physico-chimique et mécanique de ces matériaux à forte teneur en additions et est couplé à de la modélisation dans le but, in fine, de disposer d'outils permettant de prédire leur comportement au sein de l'ouvrage. Les résultats montrent qu'un cobroyage des constituants du liant permet d'améliorer la réactivité du liant et de s'assurer d'une bonne robustesse des formules de béton. La condition essentielle de l'obtention d'un pH de leur solution interstitielle de 11 est assurée dès 28 jours. Les bétons peuvent être considérés à faible chaleur d'hydratation du fait des échauffements rencontrés à court terme. A long terme, de hautes performances mécaniques, de faibles coefficients de perméabilité et de diffusion sont obtenus sur ces matériaux. Les modélisations de l'hydratation, de l'évolution de propriétés mécaniques, de l'endommagement, des déformations différées et des transferts hydriques ont été abordées. Le modèle d'hydratation utilisé a été adapté aux liants ternaires en prenant en compte les phénomènes de nucléation des additions sur l'hydratation du ciment. Pour les autres modèles, l'acquisition des mesures expérimentales a permis de fournir les données d'entrée pour leur utilisation et de vérifier leur validité sur des liants fortement dilués. Tous ces travaux permettent au final d'envisager sereinement la modélisation et la prédiction du comportement des structures réalisées en béton bas pH. / In the context of the radioactive wastes disposal in deep geological repository of clay, low-alkalinity and low heat of hydration concretes referenced "low pH " were designed. The degradation of the properties of the clay can be limited by using these types of concrete. Two types of low pH binder were chosen for this research: the first one is comprised of cement, silica fume and fly ash (TCV) and the other one is comprised of cement, silica fume and slag (TL). The objective of this research is to comprehend the behavior of these concrete in order to ensure the well-placing of the fresh concrete at an industrial scale and good mechanical performances, chemical stability and confining properties. The experimental program focuses on a physico-chemical and mechanical characterization of these recent materials with high pozzolanic addition content. The experimental data are then modeled for the purpose of having a tool that, in the end, is able to predict the behavior of the low pH concretes within the structure. The results show that grinding altogether the three constituents improves the reactivity of the binder and allows a good reproducibility of the low pH design. The most important criterion which is a pH of the interstitial solution below 11 is met at 28 days. The heat measurements at early age show that the low pH concretes are low heat of hydration concretes as well. In the long run, high mechanical performances, low permeabilities and diffusivities were obtained on these materials. The modeling of the hydration, evolution of mechanical properties, damage, creep and hydric transfers is also covered in this thesis. The model of hydration was adjusted to match the hydration of ternary binders by taking into account the effects of the additions such as the heterogeneous nucleation, on the hydration of the cement. As for the other models, the experimental results were used as data input to validate the models on binders with high replacement rates. Ultimately, this work allows us to contemplate serenely the modeling and the prediction of the behavior of structure made of low pH concretes.
119

Relations procédé-microstructure-comportement de composites à matrice vitrocéramique mis en œuvre par voie liquide / Glass-ceramic matrix composites : liquid molding and mechanical behavior

Farrugia, Anaïs 09 December 2013 (has links)
L'objectif du projet COMPTINN (COMPosites Tièdes INNovants) est d'obtenir des matériaux composites pouvant être utilisés sur de longues durées, à des températures comprises entre 150°C et 400°C, pour des applications structurales de l'aéronautique civile. Les travaux de thèse s'inscrivent dans un objectif de développement de matériaux thermostructuraux mis au point par un procédé industrialisable pour la production de pièces en série, respectueux de l'environnement et économiquement viable. Les procédés d'élaboration choisis sont ceux utilisés pour la mise en œuvre des CMO (Composites à Matrice Organique) thermodurcissables en moule fermé et par voie liquide. Les procédés les plus conventionnels ont été sélectionnés : l'injection par transfert de résine (RTM : Resin Transfer Molding) et l'infusion de résine sous vide (LRI : Liquid Resin Infusion). Les constituants des composites sont d'une part une matrice vitrocéramique, issue d'une résine dérivée d'un système géopolymérique, et d'autre part des renforts 2D et 3D en fibres de carbone. La viscosité d'une résine est la propriété principale qui conditionne sa mise en œuvre par les procédés d'élaboration par la voie liquide. La résine utilisée étant une suspension dont la viscosité est relativement élevée, la faisabilité de l'élaboration de composites par RTM ou LRI est a priori délicate. Une attention particulière a donc été portée à la rhéologie de la résine. Les résultats de cette étude ont permis d'optimiser d'importants paramètres procédés. L'étude s'est ensuite dirigée vers l'élaboration et la caractérisation des composites. L'impact du procédé de mise en œuvre sur la microstructure et sur les propriétés thermomécaniques des composites a été évalué. L'influence d'autres paramètres procédés, tels que le taux de dilution de la résine, la direction d'imprégnation du renfort et le différentiel de pression, a été étudiée. / This research work is part of the collaborative project COMPTINN (Innovative composite materials for intermediate temperature applications). This project aims at enabling the manufacturing of competitive structural composites able to bear up continuous thermal exposure, such as in aircraft parts located close to engines. A new class of glass-ceramic matrices for structural composites was developed to reach this goal. These new matrices come from an inorganic thermosetting polymer derived from a geopolymeric system. Prepreg process is currently used to manufacture composites but these composites would be more competitive if they are produced by an easy and cost effective process technology. Liquid molding (LRI or RTM) seems to be a convenient solution. Two kinds of reinforcements were considered: a layup of several two-dimensional woven fabric plies and a three-dimensional preform.The rheological behaviour of the considered inorganic polymer was firstly investigated. The best conditions were identified to obtain the lowest viscosity of the resin in order to help the production of structural composite parts by liquid molding.Then, the research work investigates how changes in the manufacturing process impact the mechanical properties of the composites. A microstructural characterization helps to link the mechanical behavior to the processing route. The effects of varying several processing parameters have been studied such as the dilution rate of the resin, the impregnation direction or the pressure differential.
120

Stratégies et scénarii de valorisation de déchets phénoplastes au sein de matrices thermoplastiques / Development of mechanical recycling methods for phenolic resin based thermoset waste

Bernardeau, Fabien 12 October 2017 (has links)
Cette thèse, réalisée en partenariat avec deux industriels, a pour objectif de mettre au point une voie de valorisation matière des résines phénoplastes (bakélite) issues de gisement de déchets plastiques. En effet, ce type de résine (thermodurcissable) n’est pour l’instant pas valorisé en fin de vie et finit en enfouissement. Pour répondre aux attentes législatives (directive DEEE, mais aussi VHU dans l’automobile), qui imposent un quota de recyclage (réutilisation et valorisation matière) et de valorisation énergétique minimum pour les déchets en fin de vie, il parait important de développer des procédés de régénération de ces plastiques ainsi que de trouver des domaines d’application pour leur utilisation en tant que matière première secondaire.Enedis, dans le cadre du déploiement de ces nouveaux compteurs électriques, collecte les anciens compteurs et équipements installés et cherche une solution de recyclage adaptée. Une partie de ce gisement important de déchets est constituée de plastiques de tous types en mélange, et en particulier de bakélite. Le travail de cette thèse s’est concentré sur le traitement et la régénération de ce gisement.Dans un premier temps, un schéma de démantèlement et de tri de ce gisement varié a été mis en place. Il est basé sur une étude des matières présentes dans le gisement, en particulier plastiques. La présence d’additifs est également évaluée, en particulier celle de substances contrôlées comme les retardateurs de flamme halogénés, le cadmium, etc. L’objectif était d’optimiser le procédé de séparation des matières en vue d’obtenir des gisements de matières régénérées de pureté suffisante pour le réemploi, tout en limitant la présence d’additifs contrôlés pour respecter les concentrations maximales légales.Pour valoriser les résines phénoplastes issues de ce gisement, la voie envisagée consiste à réutiliser cette matière sous forme de charges incorporées au sein de matrices thermoplastiques (éventuellement régénérées). Pour ce faire, une étude de la transformation de la bakélite par broyage pour obtenir un produit de granulométrie très fine (micronisation) a été réalisée. La distribution granulométrique, la morphologie et son état physico-chimique de surface ont été évaluées en fonction des paramètres du procédé. Après incorporation à différents taux de charge dans des matrices thermoplastiques, les propriétés mécaniques en quasi-statique et dynamique des composites ont été évaluées. La fonctionnalisation des charges/matrices et l’incorporation d’agents compatibilisants ont permis d’améliorer la cohésion des interfaces. Une modélisation par homogénéisation a été réalisée pour rendre compte de l’influence des différentes variables sur la tenue mécanique des composites.Le comportement au feu des composites formulés a également été étudié. Du fait de la stabilité thermique élevée de la bakélite et du taux de char important formé lors de sa combustion, il est envisagé d’utiliser les charges phénoplastes comme donneur de carbone dans la formulation d’un système retardateur de flamme intumescent. Des additifs appropriés, comme une source d’acide et un agent gonflant, seront évalués pour la formulation du système. / The main goal of this PhD project, born from a partnership between EMA, APR2 and Enedis, was to develop a material recycling solution for phenolic molding compound (PMC, or Bakelite). Indeed, these types of thermoset material are hardly valorized and end up in landfill, mostly because of the lack of technically and economically viable solutions for recycling.Phenolic molding compound material are present in large amount in End of Life (EOL) electrical meter waste stream. Therefore, Enedis committed to find a valorisation scheme for these materials. This PhD work is aimed to develop a recycling process for PMC issued from this waste stream.Firstly, a dismantlement and sorting scheme was designed. It is based on the study of the waste stream material composition – in particular the plastic stream. The presence of regulated substances (such as halogenated flame retardant, etc.) in plastic formulations was assessed. The objective was to optimize the separation process to recover materials with a high degree of purity.The proposed recycling solution consists in using the PMC as a functional filler in a thermoplastic matrix. To do so, a comminution scheme was developed to reduce the size of the PMC part. The particle size distribution, morphology and surface chemistry of the obtained products were characterized. Quasi-static and dynamic mechanical properties of composite materials incorporating micronized PMC were determined. Various coupling schemes were studied in order to increase the adhesion between filler and matrix. The mechanical behaviour of the composite materials was also modelized using finite element methods.The fire behaviour of the composite material incorporating PMC filler was also studied. Because of the high thermal stability and high char yield of phenolic molding compound, its potential use as a carbon donor in intumescent flame retardant formulations was finally assessed.

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