Actuellement, dans les plateformes aérospatiales, le nombre et le besoin d’intégration des équipements électriques et électroniques sont grandissant du fait que leurs fonctions nécessitent de plus en plus de puissance. L’objectif de minimisation des coûts et surtout la disponibilité des dispositifs électroniques forcent les concepteurs et les fabricants de ces plateformes à s’orienter vers des produits commerciaux (dits grand public). La fiabilité des boîtiers des composants de puissance doit être évaluée dans les environnements sévères des applications aérospatiales. Une dizaine de composants électroniques de puissance a été sélectionnée en fonction de leur disponibilité et l’adéquation de leurs performances électriques et thermiques aux exigences des applications aérospatiales. Ces composants intègrent différents types de semi-conducteurs tels que le silicium, le carbure de silicium et le nitrure de gallium. Tout d’abord, une étude a été menée sur les potentiels modes et mécanismes de défaillance de ces composants électroniques de puissance dans ces environnements. Elle a permis de mettre en place plusieurs procédures de vieillissement accéléré ainsi que le développement de deux bancs de tests pour suivre électriquement le vieillissement de ces composants. Ces tests ont été menés sur deux diodes Schottky SiC, commercialisées par deux fabricants, regroupant les technologies des boîtiers des composants électroniques de puissance. Les analyses de défaillance ont tout d’abord mis en évidence une immaturité de la technologie de la jonction Schottky des puces SiC de l’une des deux diodes soumis à une tension inverse. Ces défaillances sont attribuées à la destruction partielle de la structure Schottky et indique une reproductibilité non maitrisée de la fabrication des puces de ce composant. Ensuite, ces analyses ont mis en évidence plusieurs mécanismes de vieillissement lors de tests simulant des régimes « On-Off » des applications (cycles thermiques de puissance). Celui considéré comme la cause de la défaillance est la fissuration de la soudure des fils d’interconnexion avec la puce. Une loi pouvant décrire la fissuration des interconnexions a été identifiée à la suite des évolutions des cycles thermiques de puissance à l’approche de la défaillance. L’étude de ces évolutions a permis de démarrer l’élaboration d’un modèle physique de défaillance adapté aux interconnexions de la puce en vue d’estimer la durée de vie des composants commerciaux. / Currently, in the aerospace platforms, the number and the need for integration of the electric and electronic equipment are growing because their functions require more and more power. The goal of cost minimization and mostly the availability of power electronic devices push the designers and the manufacturers of these platforms moving towards commercial products (Component Off-The Shelf). The packaging reliability of power electronic components must be assessed in harsh environments of aerospace applications. A dozen of power electronic components have been selected in accordance with their availability and with the adequacy of their electrical and thermal performances according to the requirements of aerospace applications. These components integrate different types of semi-conductors such as silicon, silicon carbide and gallium nitride. Foremost, a study has been leaded on the potential failure modes and mechanisms of these power electronic components in these environments. It has permitted to put in place several procedures of accelerated ageing and the development of two test benches to electrically monitor the ageing of these components. These tests have been carried on two SiC Schottky diodes, marketed by two manufacturers, gathering the technologies of the packaging of power electronic components. The failure analyses have first highlighted an immaturity of the Schottky junction technology of the SiC die of one of the two diodes subjected to a reverse voltage. These failures are attributed to the partial destruction of the Schottky structure and indicate a not mastered reproducibility of the die manufacturing of these components. Then, these analyses have highlighted several ageing mechanisms during tests simulating « On-Off » power of applications (power thermal cycles). One considered as the failure cause is the cracking of the welding of the wire bonding with the die. A behavioral law that can describe the cracking of the interconnections has been identified according to the evolutions of the power thermal cycles when near to failure. The study of these evolutions have permitted to start the elaboration of a physical model of failure adapted to the die interconnections in order to estimate the lifetime of commercial components.

La corrosion des armatures constitue la principale cause de dégradation des ouvrages en béton armé, et occasionne des coûts élevés de maintenance/réparation. Pour prévenir ce problème sur ouvrages neufs, une solution consiste à renforcer les structures en béton par des armatures non-métalliques de type Polymère Renforcé de Fibres (PRF), généralement à base de fibres de verre, de carbone ou d'aramide. Il existe aujourd'hui plusieurs textes réglementaires consacrés aux armatures PRF, notamment aux USA, au Canada et au Japon, et de nombreux ouvrages en béton armé par barres en PRF ont d'ailleurs été construits dans ces pays. Cependant, si l'utilisation de ces nouvelles armatures semble à priori prometteuse, elle suscite encore des réserves de la part des maîtres d'ouvrages, notamment en France. Il subsiste en effet des incertitudes sur le comportement à long terme des structures renforcées par PRF, et plus particulièrement sur la durabilité en milieu alcalin des armatures à matrice vinylester ou époxy renforcée par des fibres de verre (PRFV), qui sont actuellement les plus utilisées, ou encore sur le vieillissement de l'interface PRF/béton. Dans ce contexte, la présente étude vise à développer pour la première fois en France, un ensemble de méthodologies permettant, d'une part, de caractériser les principales propriétés physiques, mécaniques et d'interface des différentes armatures en PRF disponibles sur le marché, mais également d'évaluer la durabilité d'armatures en PRFV (les plus représentatives du marché) et de l'interface PRFV/béton à travers des procédures pertinentes de vieillissements accélérés. La première partie de l'étude a donc été consacrée à la caractérisation physique et mécanique d'une sélection d'armatures du commerce, confectionnées à base de fibres de verre, de carbone ou d'aramide, et au comportement mécanique de l'interface entre ces PRF et le béton. Outre la caractérisation microstructurale des PRF par techniques de microscopie et d'analyse thermique, la mise en place de dispositifs d'essais de traction et de flexion 3 points à appuis rapprochés (Short-beam test) a permis d'accéder respectivement aux propriétés mécaniques en traction (module d'élasticité, résistance) et à la résistance au cisaillement inter-laminaire des armatures. Des essais spécifiques d'arrachement (Pull-out) ont ensuite permis d'évaluer l'influence de différents paramètres (type de fibre, diamètre et géométrie de surface des barres) sur le mécanisme de transfert d'effort à l'interface armature/béton. Une grande originalité de l'approche proposée réside dans l'instrumentation d'une partie des corps d'épreuve par des capteurs de déformation à fibre optique disposés au niveau de l'interface armature/béton ; ce dispositif de mesures réparties permet d'accéder à des informations locales comme le profil des déformations de traction de l'armature, et d'en déduire la longueur d'ancrage des différentes armatures dans le béton. En complément de l'étude expérimentale précédente, un travail de modélisation analytique et numérique a été initié en vue de simuler les essais d'arrachement et d'appréhender plus finement les mécanismes d'interface mis en jeu entre l'armature et le béton lors de ces essais. Dans cette optique, un modèle analytique d'interface a tout d'abord été proposé, puis introduit dans un modèle aux éléments finis (modèle d'endommagement de zones cohésives). Enfin, un protocole de vieillissement accéléré a été appliqué à des barres en PRFV seules ou noyées dans un milieu cimentaire. Les caractéristiques résiduelles des armatures et des interfaces ont été évaluées à différentes échéances de vieillissement (jusqu'à 240 jours). Hormis une diminution des propriétés mécaniques des barres soumises à une immersion directe en solution alcaline, cette condition pouvant être considérée comme très sévère par rapport aux conditions de service, il n'a pas été observé de dégradation des propriétés d'adhérence PRF/béton par rapport à l'état initial / Corrosion of the steel reinforcing bars (rebars) is the main process involved in the degradation of reinforced concrete (RC) structures, and has large repercussions on the maintenance/reparation expenses. To prevent such degradations on new infrastructures, the use of corrosion-free reinforcements, such as Fiber Reinforced Polymer (FRP) bars based on glass, carbon or aramid fibers, is gaining interest. Specific guidelines are already available in several countries (USA, Canada or Japan for instance), that define the design principles and good practices for this type of internal rebars; beside, many FRP RC structures have been built and are in service in these countries. Although the development of these new reinforcing bars is quite promising, infrastructures owners are still reluctant for their wide-scale use, especially in France. There are still major concerns regarding the long term behavior of FRP RC structures, and more particularly, the durability of glass fibers reinforced polymers (GFRP) when subjected to an alkaline environment, and the ageing behavior of the GFRP/concrete bonding as well. In this context, the present study aims at developing for the first time in France, a set of methodologies that allows : to characterize the main physical/mechanical properties of different types of FRP bars from the marketto assess the durability of GFRP bars (the most common type of bar) and their interface with concrete through relevant accelerated ageing procedures. The first part of this study was thus devoted to the physical/mechanical characterization of a selection of commercially available FRP rebars, based on glass, carbon or aramid fibers, and to the mechanical behavior of corresponding FRP/concrete interfaces. Beside the microstructural characterization of the various FRP materials by microscopy and thermal analysis techniques, tensile and short beam tests were developed in order to determine the tensile properties (Young's modulus and strength) and the interlaminar shear strength (ILSS) of the bars. Specific pull-out tests then made it possible to evaluate the influence of several parameters (type of fibers, diameter and surface geometry of the bars) on the mechanism of load transfer at the bar/concrete interface. A main originality of the proposed approach relied on the instrumentation of several test bodies by optical fiber strain sensors, which were installed along the bar/concrete interface. Such a distributed measurement system provided local information in the form of tensile strain profiles of the bars along the interface, and made it possible to determine the effective transfer length of the various types of FRP bars. As a complement to the previous experimental study, an analytical and numerical modeling work was initiated to simulate the pull-out tests and investigate more closely the interfacial mechanisms involved in the FRP bar/concrete bond behavior. In this line, an improved interface model was first proposed, which was then implemented in a finite element model (cohesive zone model formulated in the context of damage mechanics).Finally, an accelerated ageing protocol was developed and applied to the GFRP bars, either alone or embedded in a concrete medium. The retention properties of both bars and interfaces were determined after various periods of exposure (up to 240 days). Except a drop of tensile properties observed for GFRP bars that were directly immersed in an alkaline solution, which is considered as a very severe environment compared to actual service conditions, no significant loss of interfacial properties was detected on aged specimens compared to the initial state

Iron-tannate dyes have been used for thousands of years and on many continents to colour materials that are now part of our cultural heritage shades of black, grey, or brown. Cellulosic and proteinaceous yarns and woven textiles have been dyed with iron-tannate dyes to form objects or components of objects for domestic and ceremonial use. Unfortunately, the longevity and useful lifetime of iron-tannate dyed objects is threatened by the dye itself which accelerates the degradation of organic materials through metal-catalysed oxidation and acid-catalysed hydrolysis. The accelerated degradation causes weakening, discolouration, and embrittlement of the organic materials at a faster rate than undyed equivalents and if left unimpeded, weakens the objects to the point that they are no longer able to be exhibited without damage. In some cases the degradation is so great that the dyed areas of the objects have crumbled to dust. At present there is no suitable chemical stabilisation method available with which to inhibit this degradation. An aqueous treatment is available for successfully stabilising paper containing iron gall ink; iron gall ink is chemically similar to iron-tannate dye. However, the aqueous nature of this treatment makes it unsuitable for weakened fibres, water soluble components, and water sensitive materials which may be part of a composite material containing iron-tannate dye. Non-aqueous treatments are therefore urgently needed in order to preserve our iron-tannate dyed cultural heritage for future generations.In this project a range of non-aqueous antioxidants and a non-aqueous deacidifier (described in Chapter 8) were tested alongside existing aqueous treatment in order to establish their ability to slow down the degradation of a range of model iron-tannate dyed textiles (Chapters 9 and 10). Model textiles were developed as part of the project (Chapters 3-5) to be substitutes for historic materials in these stabilisation studies. Validation of the model textiles for this purpose (Chapter 6) involved the comparison of the model textiles with selected historic iron-tannate dyed objects within the British Museum’s collection (Chapter 6). The historic objects and the properties of the model textiles before and after accelerated ageing (Chapters 5 and 6) and before and after treatment application (Chapters 9 and 10) have been characterised using a variety of analytical techniques (Chapter 2). In order to determine which accelerated ageing conditions were the most suitable for this project various combinations of elevated temperature and either cycling or stable relative humidity were tested for their ability to produce noticeable changes in the properties of the dyed model textiles within four weeks of ageing (Chapter 7). This project is an AHRC/EPSRC funded Science and Heritage Programme PhD in which the British Museum has been a collaborative institution. Among other wider dissemination methods, research from this project has been presented to the public on numerous occasions at gallery tours and Science Day events at the British Museum.

[pt] A integridade de tubulações é um dos aspectos-chave para a operação segura e eficiente das estruturas offshore. Falhas em tubulações podem resultar em consequências econômicas e ambientais significativas, tornando a gestão da integridade de tubulações uma prioridade importante para a indústria. Uma das ferramentas mais eficazes para gerenciar tubulações em serviço é através de testes não destrutivos (NDT, na sigla em inglês). Neste estudo, inspeções de ultrassom e shearografia foram realizadas em tubulações metálicas com reparos compósitos ao longo de aproximadamente dois anos e seus resultados foram comparados. As amostras de tubos de aço com reparos compósitos foram submetidas a pouco mais de 13.500 horas de envelhecimento acelerado por névoa salina, em três diferentes temperaturas. As amostras foram removidas das câmaras de névoa salina em intervalos regulares e inspecionadas usando aparelhos de inspeção em campo. Os resultados mostraram que ambas as técnicas forneceram resultados consistentes entre cada inspeção, embora nem sempre fossem consistentes entre si. Mapas comparando as detecções e a precisão de cada técnica foram fornecidos. A viabilidade de cada técnica como ferramenta de campo para monitorar a integridade das tubulações também foi avaliada com resultados positivos. Além disso, uma metodologia de Arrhenius modificada foi proposta como um primeiro passo para prever a propagação de danos a longo prazo. / [en] Pipeline integrity is one of the key aspects for safe and efficient operation of offshore structures. Pipeline failures can result in significant economic and environmental consequences, making pipeline integrity management a top priority for the industry. One of the most effective tools for managing in-service pipelines is non-destructive testing (NDT). In this study, ultrasound and shearography inspections were performed on composite pipeline repairs over the course of approximately two years and their results were compared. The test samples evaluated were steel pipes with composite repairs and were submitted to just over 13,500 hours of salt-spray accelerated ageing, under three different temperatures. Test samples were removed from the salt-spray chambers at regular intervals and inspected by using field inspection apparatus. The results showed that both techniques provided consistent results between each inspection, although not always being consistent with each other. Maps comparing detections and accuracy of each technique were provided. The feasibility of each technique as a field tool for monitoring pipeline integrity was also evaluated with positive results. Furthermore, a modified Arrhenius methodology was proposed as a first step towards predicting long-term damage propagation.

Ce travail porte sur l'étude des comportements en flexion à court et long termes des poutres hybrides collées constituées d'un profilé pultrudé GFRP et d'une dalle en béton, assemblés par un joint de colle époxy. L'utilisation du collage dans des structures réelles se heurte encore à la réticence des concepteurs en raison du manque de garanties sur la durabilité à long terme et de l'absence d'outils de modélisation donnant la durée de vie en service des assemblages collés. La présente étude constitue donc un jalon dans cette démarche de compréhension du comportement à long terme de ces structures collées. Elle s'appuie sur analyse multi-échelles qui permet d'aborder le problème à l'échelle locale de l'interface (essai pushout) et à l'échelle globale de l'élément de structure (essai de flexion sur des poutres). Des essais de vieillissement accéléré ont tout d'abord été conduits pour étudier les effets de l'humidité et de la température sur l'adhésif seul et sur l'assemblage structural et il en ressort que l'eau, et notamment une immersion prolongée, s'avère particulièrement néfaste à la résistance au cisaillement des éprouvettes et modifie leur mode de ruine. La réponse instantanée de l'assemblage pultrudé-béton a ensuite été plus amplement étudiée. Grâce à une étude paramétrique expérimentale, une géométrie et une méthode de fabrication des éprouvettes ont été définies pour assurer la reproductibilité des résultats et limiter leur dispersion. De plus, un modèle numérique 3D a été développé dans le code d'éléments finis Cast3m et montre une distribution de contraintes, notamment de cisaillement, non uniforme le long de la surface de collage avec une concentration aux extrémités du joint. Une analyse paramétrique numérique a permis d'identifier les dimensions des dallettes et du joint de colle comme des paramètres influents sur la résistance des éprouvettes. Enfin, le comportement en fluage d'une poutre hybride est étudié. Sous l'effet d'un vieillissement naturel, seul, le joint d'adhésif ne s'avère pas impacté. Des essais de fluage en flexion 3-points ont été effectués pour étudier les réponses à long terme du profilé seul et de la poutre hybride. Ils montrent une augmentation considérable du déplacement des poutres en raison du fluage et du retrait du béton et du fluage du profilé. Des modèles 3D en variables locales, dans le cadre de la viscoélasticité linéaire, sont développés dans Cast3m et permettent de fidèlement restituer l'évolution des déplacements et des états de déformation au cours du temps pour les différentes poutres testée / This dissertation focuses on the short- and long-term responses of bonded hybrid beams consisting of a GFRP-pultruded profile bonded by an epoxy adhesive joint to a reinforced concrete-slab. The problems related to the durability and the long-term response of these structures still represent an open issue. The present study is meant to increase the knowledge and understanding of these hybrid structures in this context. Firstly, different accelerated ageing tests were carried out to evaluate the effects of some environmental agents such as water, moisture and freeze thaw cycles in the behaviour of GFRP/concrete bonded assemblies. Mechanical characterizations were carried out on control and exposed of both materials and push-out specimens to quantify the degradation and damage of the mechanical resistance of each material and of the adhesive bond properties. The water effect on the adhesion of the joints was found to be significant, especially at longer immersion times. The second part was directed at characterizing the push-out test. An experimental parametric study was performed to elaborate a methodology of fabrication of the push-out specimens that can reduce the dispersion of results and give an accurate prediction of the shear strength on a limited set of specimens. Also, a 3D finite-element model was developed using the finite-element code Cast3m. This model showed that the stress components, especially peel and shear stresses, are not constants across the bonding area and peaking near the free edges (stress concentrations). A numerical parametric study allowed to conclude that the most effective geometrical parameters influencing bond between GFRP and concrete were the bonded length and the dimensions of the concrete substrate. Last part deals with experimental and numerical investigations carried out to study the short- and long-term flexural behaviour of full-scale hybrid beams. All experiments showed considerable increase in beam deflection over time due to concrete creep and shrinkage and GFRP creep. Finally, 3D-finite-element models, realized with Cast3m, are developed based on the incremental formulation of the linear-viscoelasticity theory. The proposed models allow evaluation of the long-term deflection of the pultruded and hybrid beams. Using the proposed model, evolution with time of stresses, strains and displacements in different location of the hybrid beam are obtained

Variables for the accelerated ageing (AA) test, methods for reducing fungal contamination during the AA test, using the conductivity test as a vigour test, the effect of seed size on seed vigour and the relationship between laboratory test results and field perfonnance in selected Brassica spp were investigated. In the first experiment, three seed lots of turnip rape hybrid (B. rapa x campestris), turnip (B. campestris) and forage rape (B. napus); and seven seed lots of Asian rape (B. napus), six seed lots of Asian kale (B. oleraceae var. alboglabra L.) and five seed lots of choisum (B. rapa var. pekinensis) with germinations above 90% were aged at two different temperatures (41 and 42°C ± 0.3°C) and three ageing times (24, 48 and 72 ± 15 minutes). The second experiment was divided into three sections. In the first, the same seed lots and species were aged at one temperature (41°C) and time (72 h), but either 40 ml of saturated salts; KCl (83%RH), NaCl (76%RH), NaBr (55%RH); or distilled water (96%RH) were used as the ageing solutions. In the second, one turnip rape hyprid seed lot was aged at three temperatures (41, 42 and 45°C) and two times (72 and 96h), again using the three saturated salts and distilled water as ageing solutions. In the third, three turnip rape hybrid seed lots and three Asian kale seed lots were surface sterilised (1 % sodium hypochlorite) prior to ageing at one temperature (41°C) and time (72 h). In the third experiment, the same species and seed lots used in experiment one at their original seed moisture content (SMC) were tested for conductivity after soaking in deionised water for 4, 8, 12, 16, 20 and 24 h. They were then re-tested after the SMC had been adjusted to 8.5%. In the fourth experiment, three seed lots of forage rape and three seed lots of Asian kale were graded into three seed size categories; large (retained on a 2.0 mm screen), medium (retained on a 1.7 mm screen) and small (passed through a 1.7 mm screen). Graded seeds were then tested for standard germination, AA (41°C/48 h) and conductivity (measured at 16 and 24 h). In the final experiment, the relationships between laboratory tests for the six species (each consisting of three seed lots), field emergence from three sowings, and cold room emergence were evaluated. Both time and temperature influenced post-AA germination. Increasing the ageing period from 48 to 72 hours at 41°C, and 24 to 48 hours at 42°C resulted in decreased mean germination percentage for all species but not always clear separation of seed lots. While there were sometimes few differences between ageing at 41°C and 42°C, the former is preferred because it is already the temperature used for other species. For Asian rape, choisum and turnip, the previously recommended testing conditions of 41°C/72 h provided good seed lot separation, but for Asian kale and turnip rape hybrid, AA testing at 41°C/48 h provided better results. Seed moisture content after ageing ranged from 29-37% depending on species. Fungal growth on seeds during the ageing period appeared to reduce post-ageing germination in some seed lots . Substituting saturated salts for distilled water did not stress seed lots in the AA test, due to the lowered RH%, the exception being seed lots 1210 and 1296. For forage and Asian species, seed lot germination mostly remained above 90% when aged for 72 h at lowered RH%. Increasing the ageing duration from 72 to 96 hours resulted in some decreases in post-AA germination but no clear separation of seed lots. Surface sterilising the seeds prior to the AA test resulted in a lower incidence of contaminant fungi which was associated with a lower percentage of abnormal seedlings. The conductivity test was mostly able to identify vigour differences among forage and Asian vegetable brassica seed lots. Differences in conductivity readings were observed among seed lots in all species. Increasing the period of imbibition resulted in increased conductivity from most seed lots but radicle emergence occurred after 16-20 h of imbibition. Variation was observed in the time to reach 95% maximum of the imbibition curve for most species. Conductivity readings at 16 h would avoid possible influences of radicle emergence on results. Adjusting the SMC to 8.5% resulted in reduced variation in conductivity among replicates of seed lots, due to a reduction in imbibition damage. Seed size had a significant effect on both post-AA germination and conductivity results. In forage rape, large size seeds had higher post-AA germination cf. medium cf. small size seeds. In Asian kale, large size seeds had higher post-AA germination compared with small size seeds. For both forage rape and Asian kale, large size seeds had lower conductivity readings cf. small size seeds. The correlation analyses demonstrated significant relationships between AA testing and field emergence parameters (percentage emergence, emergence index and emergence rate). Significant relationships were also observed between conductivity testing and these field emergence parameters. Based on the correlation analysis, AA testing at 41°C/48 hand/or 42°C/48 h could be recommended to be used as an AA test for turnip and Asian rape; and 41°C/48 hand/or 41°C/72 h for Asian kale and choisum. Based on the correlation analysis, conductivity testing at 16 h can be used to predict the field emergence potential of forage and Asian vegetable seed lots. Vigour tests were consistently able to provide better indicators of field perfonnance than the standard germination test, although these relationships did vary with the different field sowings.

In alkalischen Lösungen führt die Reaktion von Hydroxylionen mit den Si-O-Si-Bindungen des Glasnetzwerks zur Bildung hydratisierter Oberflächen und gelöstem Silikat. Der Grad der Korrosion bzw. der Alterung der Glasfaser ist abhängig von der chemischen Zusammensetzung des Glases und Korrosionslösung sowie von Zeit und Temperatur. Die Untersuchung von Glasfasern verschiedener chemischer Zusammensetzung in NaOH- sowie Zementlösungen zeigte, dass die inhibierende Wirkung von Ca-Ionen zu einem veränderten Korrosionsmechanismus führt. Dies konnte anhand der mechanischen Eigenschaften der Glasfasern sowie rasterelektronenmikroskopischen Untersuchungen gezeigt werden. Während die Korrosion in NaOH-Lösung zu einer ausgeprägten Umwandlung der gesamten äußeren Glasfaserschicht in Reaktionsprodukte führte, zeigten Glasfasern in Zementlösung bei gleichem pH-Wert einen stark lokal begrenzten, punktförmigen Angriff. Daraus resultieren unterschiedliche mechanische Eigenschaften der Glasfasern in Abhängigkeit von der gewählten Korrosionslösung.

AR-Glas wird in Form von Multifilamentgarn zur Verstärkung in textilbewehrtem Beton eingesetzt. Während des Herstellungsprozesses wird auf die AR-Glasfilamente die Schlichte aufgebracht, deren chemische Zusammensetzung maßgeblich die Qualität der Filament-Matrix-Grenzschicht bestimmt, sowie die chemische Beständigkeit im alkalischen Milieu gewährleistet. Zur Beurteilung der chemischen Beständigkeit in alkalischer Umgebung werden beschleunigte Alterungsversuche in wässrigen, alkalischen Lösungen durchgeführt. Die Reaktion von Hydroxid-Ionen mit dem Si-O-Si-Gruppen des Glasnetzwerkes führt zur Ausbildung hydratisierter Oberflächen und gelösten Silikaten. Das Ausmaß der Glaskorrosion ist von der chemischen Zusammensetzung der Glasfaser, der Schlichte bzw. Beschichtung und der alkalischen Lösung sowie von Zeit und Temperatur abhängig. Die beschleunigte Alterung von verschiedenen AR-Glasfasern in NaOH-Lösung sowie Zementlösung zeigt, dass sich der Korrosionsmechanismus aufgrund der vorhandenen Calcium-Ionen unterscheidet. Die Filamentbruchspannung wird anhand der Weibull-Verteilungsfunktion analysiert. Das mechanische Verhalten hängt deutlich von der chemischen Zusammensetzung der Alterungslösung ab, was zu unterschiedlichen Parametern der Weibull-Verteilungsfunktion sowie vermengten Verteilungen führen kann. Die Alterung in NaOH-Lösung führt zur Ausbildung einer korrodierten Schicht an der Filamentoberfläche. In Ca-haltigen Zementlösungen kommt es dagegen zu einer lokal begrenzten Korrosion. Für die Beurteilung verschiedener Polymerbeschichtungen werden Betonverbunde bei unterschiedlichen Temperaturen und Umgebungsfeuchten gelagert, wodurch geeignete Alterungsbedingungen evaluiert werden und den Vergleich der chemischen Beständigkeit unterschiedlicher Beschichtungen ermöglichen. / Rovings made of AR-glass are used in textile reinforced concrete. During the manufacturing process the sizing is applied on the AR-glass filaments. The chemical constitution of the sizing determines the quality of the filament-matrix-interface but also the chemical durability of the glass filaments in alkaline environment. The durability is evaluated by accelerated ageing tests in aqueous, alkaline solutions. In alkaline solutions, the reaction of hydroxyl ions with Si-O-Si-groups of the glass network leads to the formation of hydrated surfaces and dissolved silicate. The rate of this corrosion depends on the chemical constitution of the fibre and the alkaline solution as well as on time and temperature. The investigation of the ageing of glass fibres with different chemical constitutions in NaOH and cement solutions shows that the corrosion mechanism changes due to the inhibiting effect of calcium ions. The strength distributions have been evaluated using a Weibull distribution function. The mechanical behaviour strongly depends on the chemistry of the solution and determines the parameters of the Weibull distribution function in terms of either single or mixed distributions. The corrosion in NaOH solution leads to a strong dissolution of the outer layer of the glass fibres, whereas during aging in cement solution at the same pH-value a limited, local attack was revealed. The evaluation of polymer coatings is realised by the ageing of concrete composites at different temperatures and humidities to deduce adequate ageing conditions for the comparison of different coatings.

Variables for the accelerated ageing (AA) test, methods for reducing fungal contamination during the AA test, using the conductivity test as a vigour test, the effect of seed size on seed vigour and the relationship between laboratory test results and field perfonnance in selected Brassica spp were investigated. In the first experiment, three seed lots of turnip rape hybrid (B. rapa x campestris), turnip (B. campestris) and forage rape (B. napus); and seven seed lots of Asian rape (B. napus), six seed lots of Asian kale (B. oleraceae var. alboglabra L.) and five seed lots of choisum (B. rapa var. pekinensis) with germinations above 90% were aged at two different temperatures (41 and 42°C ± 0.3°C) and three ageing times (24, 48 and 72 ± 15 minutes). The second experiment was divided into three sections. In the first, the same seed lots and species were aged at one temperature (41°C) and time (72 h), but either 40 ml of saturated salts; KCl (83%RH), NaCl (76%RH), NaBr (55%RH); or distilled water (96%RH) were used as the ageing solutions. In the second, one turnip rape hyprid seed lot was aged at three temperatures (41, 42 and 45°C) and two times (72 and 96h), again using the three saturated salts and distilled water as ageing solutions. In the third, three turnip rape hybrid seed lots and three Asian kale seed lots were surface sterilised (1 % sodium hypochlorite) prior to ageing at one temperature (41°C) and time (72 h). In the third experiment, the same species and seed lots used in experiment one at their original seed moisture content (SMC) were tested for conductivity after soaking in deionised water for 4, 8, 12, 16, 20 and 24 h. They were then re-tested after the SMC had been adjusted to 8.5%. In the fourth experiment, three seed lots of forage rape and three seed lots of Asian kale were graded into three seed size categories; large (retained on a 2.0 mm screen), medium (retained on a 1.7 mm screen) and small (passed through a 1.7 mm screen). Graded seeds were then tested for standard germination, AA (41°C/48 h) and conductivity (measured at 16 and 24 h). In the final experiment, the relationships between laboratory tests for the six species (each consisting of three seed lots), field emergence from three sowings, and cold room emergence were evaluated. Both time and temperature influenced post-AA germination. Increasing the ageing period from 48 to 72 hours at 41°C, and 24 to 48 hours at 42°C resulted in decreased mean germination percentage for all species but not always clear separation of seed lots. While there were sometimes few differences between ageing at 41°C and 42°C, the former is preferred because it is already the temperature used for other species. For Asian rape, choisum and turnip, the previously recommended testing conditions of 41°C/72 h provided good seed lot separation, but for Asian kale and turnip rape hybrid, AA testing at 41°C/48 h provided better results. Seed moisture content after ageing ranged from 29-37% depending on species. Fungal growth on seeds during the ageing period appeared to reduce post-ageing germination in some seed lots . Substituting saturated salts for distilled water did not stress seed lots in the AA test, due to the lowered RH%, the exception being seed lots 1210 and 1296. For forage and Asian species, seed lot germination mostly remained above 90% when aged for 72 h at lowered RH%. Increasing the ageing duration from 72 to 96 hours resulted in some decreases in post-AA germination but no clear separation of seed lots. Surface sterilising the seeds prior to the AA test resulted in a lower incidence of contaminant fungi which was associated with a lower percentage of abnormal seedlings. The conductivity test was mostly able to identify vigour differences among forage and Asian vegetable brassica seed lots. Differences in conductivity readings were observed among seed lots in all species. Increasing the period of imbibition resulted in increased conductivity from most seed lots but radicle emergence occurred after 16-20 h of imbibition. Variation was observed in the time to reach 95% maximum of the imbibition curve for most species. Conductivity readings at 16 h would avoid possible influences of radicle emergence on results. Adjusting the SMC to 8.5% resulted in reduced variation in conductivity among replicates of seed lots, due to a reduction in imbibition damage. Seed size had a significant effect on both post-AA germination and conductivity results. In forage rape, large size seeds had higher post-AA germination cf. medium cf. small size seeds. In Asian kale, large size seeds had higher post-AA germination compared with small size seeds. For both forage rape and Asian kale, large size seeds had lower conductivity readings cf. small size seeds. The correlation analyses demonstrated significant relationships between AA testing and field emergence parameters (percentage emergence, emergence index and emergence rate). Significant relationships were also observed between conductivity testing and these field emergence parameters. Based on the correlation analysis, AA testing at 41°C/48 hand/or 42°C/48 h could be recommended to be used as an AA test for turnip and Asian rape; and 41°C/48 hand/or 41°C/72 h for Asian kale and choisum. Based on the correlation analysis, conductivity testing at 16 h can be used to predict the field emergence potential of forage and Asian vegetable seed lots. Vigour tests were consistently able to provide better indicators of field perfonnance than the standard germination test, although these relationships did vary with the different field sowings.

Estudos anteriores utilizando matriz cimentícia reforçada exclusivamente com fibras vegetais propiciaram a produção de telhas com desempenho aceitável nas idades iniciais. Porém, com o envelhecimento natural, as telhas apresentaram significativa redução do desempenho mecânico, fato este atribuído principalmente ao ataque alcalino da matriz cimentícia. A presente pesquisa teve como objetivo o aprimoramento de telhas onduladas de fibrocimento sem amianto, a partir de processo automatizado. A primeira etapa do trabalho consistiu na avaliação do efeito da intensidade de refino da polpa Kraft de sisal (Agave sisalana) nas propriedades mecânicas e físicas de placas planas baseadas em matriz de cimento Portland, e o uso conjunto com fibras de poliproprileno (PP). Esta etapa envolveu também a caracterização dos principais atributos das polpas celulósicas refinadas, bem como a caracterização microestrutural (microscopia eletrônica de varredura e porosimetria por intrusão de mercúrio) do material resultante após envelhecimento acelerado e em ambiente natural. Na segunda etapa, séries de telhas onduladas de fibrocimento foram produzidas por técnica de sucção do excesso de água e prensagem, utilizando os melhores parâmetros definidos na etapa anterior. Os efeitos da cura acelerada em autoclave e dos envelhecimentos acelerados (carbonatação acelerada, imersão-secagem e calor-chuva) nas propriedades mecânicas e físicas das telhas foram avaliados. Os resultados obtidos mostraram a grande contribuição do refino da polpa celulósica na melhoria da resistência dos compósitos. Altas intensidades de refino apresentaram os melhores resultados para compósitos reforçados somente com polpa celulósica, mesmo após os envelhecimentos, porém intensidades intermediárias em compósitos híbridos mostraram-se suficientes. A adição das fibras de polipropileno como reforço híbrido teve como ponto forte a manutenção da resistência ao impacto, propriedade esta fortemente afetada pelo envelhecimento acelerado nos compósitos reforçados somente com polpa de sisal. As telhas produzidas mostraram-se mais eficientes no amortecimento térmico do que telhas comerciais de fibrocimento amianto. Melhorias no processo de produção das telhas mostraram efetiva contribuição no desempenho mecânico em relação aos trabalhos anteriores, tanto no curto como no longo prazo. Os resultados também indicaram a utilização da carbonatação acelerada como um procedimento eficiente na mitigação da degradação sofrida pelas fibras celulósicas em meios menos agressivos, no caminho para tornar viáveis os materiais reforçados com fibras vegetais. / Previous studies using exclusively vegetal fibres as the sole reinforcement of cement matrix have propitiated the production of roofing tiles with acceptable performance at the first ages. However, with the natural ageing, the roofing tiles have presented significant reduction in the mechanical performance, attributed to the alkaline attack of the cimentitious matrix mainly. The present research had as objective the improvement of undulate fibrecement roofing tiles without asbestos with automated equipment for production. The study also evaluated the physical, mechanical and microstructural behaviour of the obtained composites. The first stage consisted of evaluating the refinement effect of sisal Kraft pulp on mechanical and physical properties of flat pads based on Ordinay Portland cement and the jointly use of polypropylene fibres (PP). This stage also involved the characterization of the main attributes of refined cellulosic pulps, as well as the microstructural characterization (scanning electron microscopy and mercury intrusion porosimetry) of the resultant material after the accelerated and natural ageing. In the second stage, series of fibrecement roofing tiles were produced by slurry dewatering technique and pressing, using the best parameters of the first stage. Efects of autoclaved curing and accelerated ageing (accelerated carbonation, soak-dry and heat-rain) on mechanical and physical properties of tiles were evaluated. Results showed the great contribution of pulp refinement on mechanical strengh improvement. Higher intensities of refinement provided the best results for composites only reinforced with sisal pulp, despite ageing mechanism. Intermediate refinement revealed to be enough for hybrid composites. Adition of polypropylene fibres as hybrid reinforcement provided toughness maintenance after ageing, which was strongly affected only in sisal reinforced composites. Asbestos free tiles showed to be more efficient on thermal insulating properties than commercial asbestos cement. Improvements on tiles production process showed effective contribution on mechanical performance in relation to the previous works, both at initial ages and after ageing. The results have also indicated the utilization of accelerated carbonation as an effective procedure to mitigate the degradation suffered by the cellulosic fibres in the less aggressive medium, in way of the viability of the cement based materials reinforced by vegetal fibres.