Les composites à matrice céramique, constitués à la fois d’une matrice et d’un renfort fibreux en carbure de silicium, ont été choisi pour le développement des réacteurs d’avion. Bien que de nombreux travaux se soient intéressés à la synthèse de la matrice ou de l’interphase, peu ont traité directement du renfort, élément clé dans le comportement des composites, dans de telles conditions d’application. Ce mémoire porte donc sur ces matériaux appartenant à la première génération (contenant une grande proportion d’oxygène) et se scinde en deux parties. Tout d’abord, la réactivité chimique des fibres vis-à-vis de l’air, de la vapeur d’acide phosphorique ou du dichlore est étudiée via l’énergie d’activation apparente de l’attaque, et des corrélations avec les propriétés physicochimiques ou microstructurales des fibres en sont tirées. Ces résultats montrent l’influence notable qu’ont des éléments métalliques (titane, zirconium), pourtant présents en faibles quantités (<1% at.) Ensuite, la rupture prématurée de fils Si-C-O est étudiée et prédite aux températures intermédiaires (400-900°C). Ces résultats, une fois corrélés aux propriétés des fibres et à leur réactivité chimique, permettent de proposer deux mécanismes d’endommagement pouvant entrainer la rupture des fils selon les conditions d’essais : la fissuration sous-critique ou l’oxydation sans contrainte. Pour pallier l’instabilité de certaine de ces fibres un traitement de phosphatation, précédé ou non d’une chloration, transforme la surface en une barrière environnementale multicouche, sans dégradation des propriétés mécaniques, ce qui a pour effet de ralentir le mécanisme d’endommagement induit par l’oxydation et se répercute par une nette augmentation de leur durée de vie. / Ceramic Matrix Composites (CMC) are technical materials, made of a matrix reinforced by continuous fibers, considered for civil aircraft jet engine. Although the matrix and the interphase were extensively studied in past decades, reinforcement did not gain much attention however it pilots the ultimate failure of the composite. This work is dedicated to the first generation SiC fibers containing a large amount of oxygen and is divided in two parts. Firstly, chemical reactivity of Si-C-O fibers is studied against chloride, oxidant of phosphating gases. Apparent activation energies appear as an intrinsic property and are correlated with physicochemical or microstructural properties. Among observations, we show that the nature of the metallic element, such as titanium or zirconium, greatly influence the chemical stability of the fibers, however their proportion is low (1at. %). Thereafter, delayed failure of Si-C-O tows has been studied in order to predict it at intermediate temperatures (400-900°C). A statistical approach of tows’ lifetime allows us to define the survival probability at given condition, key point for the composite certification. Results were correlated to fibers properties and their chemical reactivity suggesting two damaging phenomena leading to the tows failure: slow crack growth or static oxidation. To overcome the instability of some fibers (doped with titanium), phosphating treatment was used to transform the surface of each fiber in multilayer silicophosphate coating acting as an environmental barrier. Obviously, mechanical properties of the fibers core were not affected by this etching reaction. A clear oxidation resistance and lifetime enhancement of the tows was reached by this route.

É elaborada uma proposta de procedimentos de projetos de comboios fluviais adaptados às condições existentes das vias navegáveis, a partir de uma visão ampliada da necessidade de obtenção de menores custos de transporte, com níveis adequados de segurança e de respeito ao meio ambiente. Uma análise das inter-relações técnicas entre hidrovias e embarcações, assim como dos condicionantes e implicações do conceito de embarcações adaptadas às vias navegáveis, orientou a elaboração do modelo. Este foi estruturado em módulos, com o objetivo de reproduzir, um a um, os fatores mais importantes que influenciam a eficiência, a segurança e o nível de interferência ambiental do transporte de cargas por comboios. Um programa computacional foi desenvolvido como instrumento de aplicação do modelo, consolidando os procedimentos propostos para a escolha das melhores alternativas de projeto e de operação de comboios. Resultados experimentais com comboios em escala real e com modelos em tanques de provas, foram utilizados para validação dos procedimentos adotados. Dados de acidentes com comboios em várias hidrovias do mundo foram utilizados como bases para avaliações de risco. O modelo foi aplicado aos casos de transportes de soja pela hidrovia Tietê-Paraná e pelo rio Araguaia, exemplificando as formas de análise e de escolha das alternativas de soluções de projeto. Ao final, os resultados obtidos comprovaram a utilidade da adoção de um enfoque mais abrangente do processo de projeto de comboios fluviais. / It is proposed a procedure model for design of barges push-tow adapted to waterway actual conditions, with the purpose of minimize transportation costs but always making verifications of navigation safety and ambient interferences levels. An analysis of inter-relations on inland waterways and cargo ships and, also, detailed conditionings and implications of waterway adapted ships concept, was used for model elaboration. It was structured in blocks to reproduce, one to one, the most important factors that modify efficiency, safety and environmental interference levels of barges push-tow cargo transportation. A computational program was developed to consolidate the proposed model and to apply procedures to choose best design and operational alternatives. Results of full scale and towing tank tests with push-tows were used to verify the mathematical and semi-empirical models. Barges push-tows accidents data from waterways of the world was used as risk model basis. To evaluate its effectiveness, the model was applied to bulk grain transportation cases by Tietê-Paraná waterway and by Araguaia river. The results shows that the special emphasis on three factors (efficiency, safety and ambient) improves the quality of barges push-tow design process.

Résumé confidentiel / Résumé confidentiel

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Cette thèse s’intéresse à la déformabilité des renforts à bases de fibres de lin lors de leur mise en forme, au cours du procédé RTM (Resin Tranfer Molding), notamment lorsque les formes considérées sont complexes. La compréhension des défauts et mécanismes de déformations de ces renforts est alors nécessaire. S’appuyant sur un banc d’essai d’emboutissage spécifique, une caractérisation globale (défauts de mise en forme) et locale (déformations des mèches par méthode optique) des préformes a été réalisée, pour différents paramètres procédés (pressions serre-flan et orientation du renfort) et matériaux (architecture). De cette étude, un défaut spécifique lors de la mise en forme a été mis en évidence : le bouclage, sous la forme de flambement hors plan des mèches. Afin de contribuer à sa compréhension, peu décrite dans la littérature, un banc de caractérisation, indépendamment du procédé, a été conçu pour reproduire le phénomène dans le plan et identifier les différents mécanismes à l’origine de ce défaut. Une méthode interférométrique pour quantifier ce phénomène est proposée et une étude paramétrique est réalisée (tensions appliquées, angle de courbure, orientation, architecture du renfort). Au sein du renfort, le comportement des mèches présente de fortes non-linéarités en tension. Un modèle macroscopique par éléments finis est proposé afin de mettre en avant l’importance de ces non-linéarités sur les résultats numérique issus de l’opération de formage. Une étude de sensibilité sous différentes conditions procédés de ces non-linéarités est également apportée. / This study concerns the manufacturing process of composite material from woven flax reinforcement and specifically the preforming stage of the RTM (Resin Transfer Molding) process, with complex geometries. During the process several deformation modes take place and several defects may appear and it is therefore important to understand the mechanisms controlling their appearance. A specific sheet forming bench has been used to characterise the formed shapes at the macroscopic scale (global defects) as well as at the mesoscopic scale (tow strains). Various process parameters (blank holder pressures and reinforcement orientation) and the local tensile strains were measured using an optical method. From the observed defects, the tow buckling, out of plane bending of tows, was particularly investigated as this one is not very much described in the litterature. An experimental setup independent of the forming process was designed to specifically study this defect and to quantify the key parameters controlling its appearance. An interferometric method was proposed to measure the size of the buckles with accuracy and a parametric study (applied tensions, bending angles, orientation and architecture of the reinforcement) has been completed. Within the reinforcement, the tensile behaviour of tows presents strong non-linearities. A finite elements model at the macroscopic scale is proposed to highlight the impact of these non-linearities on the forming modeling results. A sensitivity study under several process conditions has been realized.

É elaborada uma proposta de procedimentos de projetos de comboios fluviais adaptados às condições existentes das vias navegáveis, a partir de uma visão ampliada da necessidade de obtenção de menores custos de transporte, com níveis adequados de segurança e de respeito ao meio ambiente. Uma análise das inter-relações técnicas entre hidrovias e embarcações, assim como dos condicionantes e implicações do conceito de embarcações adaptadas às vias navegáveis, orientou a elaboração do modelo. Este foi estruturado em módulos, com o objetivo de reproduzir, um a um, os fatores mais importantes que influenciam a eficiência, a segurança e o nível de interferência ambiental do transporte de cargas por comboios. Um programa computacional foi desenvolvido como instrumento de aplicação do modelo, consolidando os procedimentos propostos para a escolha das melhores alternativas de projeto e de operação de comboios. Resultados experimentais com comboios em escala real e com modelos em tanques de provas, foram utilizados para validação dos procedimentos adotados. Dados de acidentes com comboios em várias hidrovias do mundo foram utilizados como bases para avaliações de risco. O modelo foi aplicado aos casos de transportes de soja pela hidrovia Tietê-Paraná e pelo rio Araguaia, exemplificando as formas de análise e de escolha das alternativas de soluções de projeto. Ao final, os resultados obtidos comprovaram a utilidade da adoção de um enfoque mais abrangente do processo de projeto de comboios fluviais. / It is proposed a procedure model for design of barges push-tow adapted to waterway actual conditions, with the purpose of minimize transportation costs but always making verifications of navigation safety and ambient interferences levels. An analysis of inter-relations on inland waterways and cargo ships and, also, detailed conditionings and implications of waterway adapted ships concept, was used for model elaboration. It was structured in blocks to reproduce, one to one, the most important factors that modify efficiency, safety and environmental interference levels of barges push-tow cargo transportation. A computational program was developed to consolidate the proposed model and to apply procedures to choose best design and operational alternatives. Results of full scale and towing tank tests with push-tows were used to verify the mathematical and semi-empirical models. Barges push-tows accidents data from waterways of the world was used as risk model basis. To evaluate its effectiveness, the model was applied to bulk grain transportation cases by Tietê-Paraná waterway and by Araguaia river. The results shows that the special emphasis on three factors (efficiency, safety and ambient) improves the quality of barges push-tow design process.

This thesis primarily focused on the development of novel composite tubes by braiding. The objective was to use hierarchical scale technique, i.e., micro, meso and macro scales, with the transfer of information from one scale to another to develop novel braided composite tubes. This research was conducted and reported in three journal papers. The aim of the first paper was to predict plane elastic properties for E-glass/epoxy braided composite structures at different braid orientations, by analytical and finite element techniques. The lenticular shape has been used to describe the geometry of the tow. Modified lenticular geometric model was developed to improve an existing geometric model, in terms of tow parameters, thereafter, plane elastic properties from Chamis micromechanical model for E-glass fibre and epoxy matrix without any knockdown effects were used as benchmark to develop predictive models, namely; Lekhnitskii's methodology and braided unit cell meso-scale finite element model to account for the effects of tow geometry, undulations/crimp, cross-over and braid orientations on the plane elastic properties of E-glass/epoxy composite. The results showed agreement in trend between the predictive models, Chamis micromechanical model, and a similar existing model. However, the plane elastic properties were knocked down in predictive models by 30% in the E11 direction and 32% in the E22 direction, when compared with Chamis micro-mechanical model for largest ±65° braid angle, among the braid angles, considered. The aim of the second paper was to manufacture E-glass/epoxy braided tubes at different braid orientations by vacuum bag infusion technique, conduct internal pressure tests, and determine the hoop and axial moduli of the infused tubes. Lekhnitskii's methodology was also used to develop plane elastic moduli by experiment using microscopy results, and by calculation. The experimental elastic moduli of the infused tubes and the experimental elastic moduli from Lekhnitskii's methodology were used to compare the predictive elastic moduli for E-glass/epoxy braided structures by Chamis micro-mechanical model, and the braided unit cell meso-scale finite element model. The two were from another paper. Results showed a perfect agreement in trend between the experimental results and the predictive results. However, the values of the experimental results were close but lower than the predicted results. Optical microscopy was performed on braided tube cross-section to evaluate the level of crimp or undulation. This was done by the determination of tow centreline crimp angle and aspect ratio. Results show that when compared with the predicted crimp, there was an agreement in trend, although the experimental results were lower than the predicted. Also, the knockdown factor was evaluated and used to quantify the reduction in experimental elastic moduli when compared with the predicted. Results showed that the absences of crimp in the Chamis model caused a tremendous difference between it, other predicted models and the experiment results. The elastic moduli of Chamis were by far higher than all others, including other predictive models. The purpose of the third paper was to manufacture E-glass/epoxy braided tube at ±31°, ±45°, ±55°, ±65° braid orientations using vacuum bagging and resin infusion technique, to design and manufacture a rig for tube internal pressures experiment, to determine the hoop and axial stress performances of the tubes by internal pressure experiment, to compare experimental results with laminate analysis predictions to evaluate the effect of crimp on the internal pressure performance of the braided tubes. To use E-glass braided tow meso-scale unit cell finite element model to predict the tow critical stresses, and the optimum braided tube architecture, using tube hoop and axial failure stresses or strains. The tubes were manufactured and subjected to internal pressure test (2:1), to failure. Failure mode was by weeping and bursting. Hoop stress was twice the axial stress. The highest value of hoop stress was at the ±65° braid angle, higher than the hoop stresses at the ±31°, ±45°, and ±55 ° braid angles by 50%, 39%, and 28% respectively. Hoop stress increased with increase in braid angle. The experimental results were validated by laminate analysis predictions by Chamis micro-mechanical model and Lekhnitskii's methodology, and the trend of the laminate analysis prediction matched that of the experimental results. However, the predicted values were higher than the experimental results by 21%, 14%, 11%, 10% for the ±31°, ±45°, ±55°, ±65° braid angles for the Chamis micro-mechanical model and 5%, 7%, 7%, 5% for the ±31°, ±45°, ±55°, ±65 braid angles respectively for the Lekhnitskii's model, showing the severe effect of crimp in the experimental tube, mostly when compared with Chamis micro-mechanical model. Braided tow unit cell finite element model prediction, showed that tow axial stresses increased with increase in braid angle, while the tow transverse stresses decreased with increase in braid angle. The predictions showed that the tow critical stresses and the tube optimum braided architecture lie between the ±65° and 90° braid angles. The tow critical stresses are the stresses at which the tow decreasing transverse stress and the tow increasing axial stress causes the tube to fail.

L'industrie oléicole joue un rôle socio-économique important pour les pays méditerranéens. Cependant, ce secteur pose également de sérieux problèmes environnementaux dus à la production de grandes quantités de sous-produits pendant de courtes périodes : les grignons d'olive, les margines (effluents liquide) et les margions. En effet, les margines représentent un défi environnemental majeur. Face à cette situation, plusieurs techniques physico-chimique et biologique ont été développées pour répondre à cette problématique. Malgré leur efficacité, ces techniques présentent l’inconvénient d’être chères. L'objectif de ce travail est de contribuer à la gestion et la valorisation à grande échelle des sous-produits oléicoles à travers l’optimisation des paramètres de démarrage du processus, le compostage et le lombricompostage et de mettre au point une méthode simple et efficace de suivi de l’évolution chimique et biologique des composts. Notre étude a porté sur le lombricompostage et le compostage d’un mélange de grignons d’olive, de fumier de cheval et de paille de blé, imbibé avec un ajout de margines à différentes concentrations. Le compost et le vermicompost ont été caractérisés par des paramètres physico-chimiques et biologiques qui ont mis en évidence la minéralisation, l’humification et la stabilisation de la matière organique. Le lombricompostage, combiné au compostage, peut être une technique adaptée et moins couteuse pour le traitement et la valorisation des sous-produits oléicoles comme amendement organique à grande échelle. / The olive industry plays an important socio-economic role for the Mediterranean countries. However, this sector also caused serious environmental problems due to the production of large quantities of by-products for short periods: olive pomace, olive mille wastewater (OMWW) and tow phase olive waste. Indeed, OMWW represent a major environmental challenge because of their chemical composition. Faced with this situation, several physicochemical and biological techniques have been developed to respond to this problem. Despite their effectiveness, these techniques have the disadvantage of being expensive. The objective of this study is to contribute to the management and the large-scale valorization of olive oil by-products through the optimization of the starting parameters of the process; composting and vermicomposting and to develop a simple and effective method for monitoring the chemical and biological evolution of composts. Our study focused on vermicomposting and composting a mixture of olive pomace, horse manure and wheat straw, soaked with the addition of OMWW at different concentrations. Compost and vermicompost were characterized by physicochemical parameters and biological parameters which showed the mineralization, humification and stabilization of organic matter.Vermicomposting, combined with composting, may be a suitable and less expensive technique for the processing and valorization of olive oil by-products as a large-scale organic amendment.

Cette étude a été motivée par la nécessité de pouvoir décrire la variabilité biogéochimique avec la même résolution que les paramètres physiques. Des profileurs optiques ont permis de mesurer à haute fréquence les propriétés optiques inhérentes dans la colonne d'eau. Par comparaison avec des données discrètes acquises simultanément à nos mesures, les coefficients optiques à des longueurs d'onde précises ont été convertis en grandeurs biogéochimiques quantitatives. Nous avons estimé la concentration en chlorophylle a et en carbone particulaire total ainsi que la répartition verticale de la matière organique dissoute colorée (CDOM). La nature qualitative du matériel particulaire et dissous a été abordée en combinant différents coefficients optiques ainsi qu'en analysant leur dépendance spectrale. En préalable aux campagnes dans l'Atlantique nord (campagnes POMME), une expérience en milieu contrôlé a été menée sur une population d'organismes phytoplanctoniques calcifiants (Emiliania huxleyi) afin de caractériser ses propriétés biooptiques ainsi que leurs modifications consécutives à une augmentation de la pCO2 atmosphérique du niveau actuel (360 ppm) au niveau prévu pour la fin du siècle (700 ppm). Lors des campagnes entre le Portugal continental et les Açores nous avons effectué le suivi biooptique de la variabilité à méso-échelle à trois périodes clés de l'année : fin de l'hiver, printemps et fin de l'été. L'observation à haute résolution de la colonne d'eau a permis de mettre en évidence certaines relations entre les caractéristiques hydrologiques et biogéochimiques. Le déploiement de nos instruments le long de radiales avec un système tracté autorisant une résolution de 2 milles (Tow-Yo) a conduit à préciser l'influence des structures tourbillonnaires de moyenne échelle.

La rupture différée des fibres SiC de type Hi-Nicalon à l’échelle multifilamentaire, des minicomposites de type Hi-Nicalon/PyC/SiC et Hi-Nicalon/type PyC/B4C a été étudiée à l’aide de moyens d’essais spécifiques et innovants. Des essais de fatigue statique sous air aux très hautes températures (900°C-1300°C) avec mesure des déformations ont ainsi pu être réalisés sur ces différents matériaux. Les résultats expérimentaux obtenus (durée de vie, déformation, lois de comportement en traction) ont permis de comprendre et de modéliser les mécanismes responsables de la rupture différée aux différentes échelles : - Les fils Hi-Nicalon rompent par mécanisme de fissuration lente activé par l’oxydation du carbone libre des fibres. Le mécanisme de fissuration est perturbé par la formation rapide d’oxyde SiO2 à partir de 1000°C : pour les faibles contraintes, la cinétique de fissuration lente est ralentie par formation d’oxyde protecteur empêchant l’accès de l’oxygène aux fissures ; pour les fortes contraintes, la rupture des fils est prématurée à cause de collages inter-fibres (fibre-oxyde-fibre). A 1200°C, le mécanisme de fluage semble être à l’origine de la rupture quasi-instantanée du matériau pour des contraintes supérieures à 200 MPa. - Les minicomposites Hi-Nicalon/type PyC/SiC rompent par mécanisme de fissuration lente ralenti par la présence de matrice SiC et par la formation d’oxyde SiO2 limitant l’accès de l’oxygène aux fibres. le mécanisme de fluage est observé à partir de 1200°C mais il n’a jamais été responsable de la rupture du matériau. - Les minicomposites Hi-Nicalon/type PyC/B4C rompent par mécanisme de fissuration lente ralenti par formation d’oxyde B2O3 à 900°C pour les fortes contraintes. Pour les autres températures et pour les faibles contraintes à 900°C le mécanisme de rupture est la diminution rapide du diamètre des fibres à cause de l’augmentation de la cinétique d’oxydation des fibres par l’oxyde B2O3. Des modèles analytiques basés sur ces différents mécanismes permettent de prévoir la durée de vie du matériau en prenant en compte les incertitudes de mesure et la variabilité des résultats de durée de vie. / Delayed failure of SiC Hi-Nicalon multifilament tows (500 fibers), minicomposites Hi-Nicalon/type PyC/SiC and Hi-Nicalon/type PyC/B4C was investigated in static fatigue, in air, at high temperatures (900°C – 1300°C) using specific and innovative devices. Static fatigue tests with measure of strain were performed on these materials. The experimental results (lifetime, strain, tensile behavior) have helped to understand and model the mechanisms responsible for the delayed failure at the different scales: - Hi-Nicalon tows rupture is caused by subcritical crack growth mechanism activated by oxidation of free carbon in the fibres. This phenomenon is disrupted by fast oxide SiO2 formation over 900°C: subcritical crack growth kinetic slows down for low stresses because of protective oxide formation which prevents the cracks from oxygen; For high stresses, the lifetime of Hi-Nicalon tows is weaker because of fibers interactions (fiber-oxide-fiber). At last, creep seems to cause the rupture of the tows for stresses over 200 MPa at 1200°C. - Hi-Nicalon/type PyC/SiC minicomposites break by subcritical crack growth slowed down by the SiC matrix and by the SiO2 formation which limit the access of the oxygen to the fibers. Creep occurs at 1200°C but it isn’t responsible of the rupture. - Hi-Nicalon/type PyC/B4C minicomposites break by subcritical crack growth slowed down by the formation of B2O3 oxide at 900°C for high stresses. The rupture is caused by the fast decrease of the diameter of the fibers at the other temperatures and for low stresses at 900°C. The oxidation kinetic of the fibers increases because of the dissolution of silica coating by B2O3 oxide. Analytical modeling was performed to schedule the lifetime of these materials and the variability of the experimental results is studied.