CoordenaÃÃo de AperfeiÃoamento de NÃvel Superior / Os aÃos inoxidÃveis austenÃticos sÃo conhecidos pela sua maior resistÃncia à corrosÃo e boas propriedades mecÃnicas a altas temperaturas. No entanto estes aÃos sÃo suscetÃveis à corrosÃo intergranular, causada pela segregaÃÃo de carboneto de cromo (M23C6) nos contornos de grÃo. Esse tipo de corrosÃo à causado pelo empobrecimento de cromo nas regiÃes adjacentes aos contornos de grÃo, fazendo com que o aÃo se caracterize como sensitizado. Uma alternativa para reduzir esse efeito à a reduÃÃo do teor de carbono em soluÃÃo sÃlida, diminuindo assim a formaÃÃo de carbonetos a elevadas temperaturas. Neste trabalho foi avaliada a resistÃncia à sensitizaÃÃo dos aÃos AISI 317 e AISI 317L a partir do estado como recebido quando submetido na faixa de temperatura de 400ÂC a 700ÂC por diferentes perÃodos de tempo. Foi tambÃm estudado um tratamento de solubilizaÃÃo adequado para minimizar os efeitos da sensitizaÃÃo no material como recebido submetido nas condiÃÃes escolhidas de tratamento tÃrmico. Foram realizados tratamentos tÃrmicos nos tempos de 1h, 12h, 24h, 72h e 96h nas temperaturas de 400ÂC, 500ÂC, 600ÂC e 700ÂC. Foram realizados tratamentos de solubilizaÃÃo na temperatura de 1100ÂC por 20, 60 e 240 minutos em ambos os aÃos e em seguida foram repetidos os tratamentos tÃrmicos nas condiÃÃes onde o material apresentou sensitizaÃÃo na condiÃÃo como recebido. ApÃs cada tratamento foi realizada uma caracterizaÃÃo microestrutural pelas tÃcnicas de microscopia eletrÃnica de varredura e microscopia Ãtica. Foram realizados ensaios de reativaÃÃo potenciocinÃtica por Double Loop (DL-EPR) para uma avaliaÃÃo quantitativa do grau de sensitizaÃÃo das amostras. A exposiÃÃo dos aÃos na temperatura de 700ÂC acarretou a sensitizaÃÃo dos mesmos, porÃm na condiÃÃo como recebido, o aÃo AISI 317L mostrou-se sensitizado mais cedo em comparaÃÃo ao aÃo AISI 317. O tratamento tÃrmico de solubilizaÃÃo à 1100ÂC foi mais efetivo em reduzir a sensitizaÃÃo do aÃo AISI 317L, mostrando que o tempo de 20 minutos à suficiente para melhorar sua resistÃncia ao empobrecimento de cromo. / Austenitic stainless steels are known for their higher corrosion resistance and good mechanical properties at high temperatures. However, these steels are susceptible to intergranular corrosion caused by segregation of chromium carbide (M23C6) at grain boundaries. This type of corrosion is caused by the depletion of chromium in the regions adjacent to grain boundaries, making the steel as sensitized. An alternative to reduce this effect is to reduction of the carbon content in solid solution, thus decreasing the formation of carbides at high temperatures. In this work it was evaluated the resistance to sensitization of AISI 317 and AISI 317L steels from the state as received when submitted in the temperature range 400  C to 700  C for different periods of time. It was also investigated a solution annealing temperature appropriate that it could minimize the sensitization effects for the material in the as received condition under the selected conditions of heat treatment. Heat treatments were performed in the time of 1h, 12h, 24h. 72h and 96h at temperatures of 400 ÂC, 500 ÂC, 600 ÂC and 700 ÂC. Solution annealing treatments were performed at temperature of 1100ÂC for 20, 60 and 240 minutes in both steel and then heat treatments were repeated under conditions where the material presented in the sensitization condition as received. After each treatment a micro structural characterization was held using both a metallurgical and a scanning electron microscope. Tests were performed with Double Loop potenciokinetic reactivation method (DL-EPR) to quantitatively assess the sensitization degree of the samples. The exposure of the samples at a temperature of 700  C led to the sensitization, but as received AISI 317L steel was sensitized early in comparison to the AISI 317 steel. The solution anneal heat treatment at 1100ÂC was more effective in reducing the sensitization of the AISI 317L steel, showing that the time of 20 minutes is enough to improve their resistance to depletion of chromium.

La prédiction des durées de vie des pièces de structures aéronautiques a toujours été une problématique à la fois complexe et capitale dans ce domaine de l’industrie. Néanmoins, la majorité des tests existant à l’heure actuelle cherche à évaluer la capacité des matériaux à résister aux sollicitations mécaniques notamment en fatigue. Les problématiques liées à l’endommagement causé par l’environnement comme la corrosion sont encore mal comprises. En effet, bien que certains tests permettent de détecter et de caractériser cet endommagement, aucun outil fiable de prédiction des vitesses de propagation des défauts de corrosion intergranulaire n’existe. Ainsi, actuellement, un défaut de corrosion détecté induit systématiquement un changement de la pièce. Les travaux de cette thèse s’inscrivent dans cette problématique ; ils ont pour but de comprendre les phénomènes de corrosion intergranulaire sur l’alliage d’aluminium 2024, le plus utilisé dans le secteur aéronautique, et d’étudier les cinétiques de propagation des défauts de corrosion. L’étude s’appuie sur une approche multi-échelle des processus de corrosion, des états microstructuraux et de l’influence de l’hydrogène. Ce projet s’inscrit également dans une dynamique de collaboration avec Airbus Group et l’Université de Bourgogne dans le cadre du projet ANR M-SCOT (Multi-Scale Corrosion Testing ANR-14-CE07-0027-01). / Nowadays, cracks kinetics is a key point in aircraft risk and reliability analysis. In particular, the propagation of corrosion defects is of special interest and could promote an early mechanical crack initiation. However, today most of the tests are calibrated to control mechanical damage and do not take into account the propagation of the corrosion defects. Indeed, when a corrosion defect is observed, the airplane part is automatically changed which leads to high manufacturing costs. The aim of this work is to understand the intergranular corrosion mechanisms and to study the propagation kinetics of the corrosion defects in an aeronautical reference alloy, i.e. the 2024-T351 aluminium alloy. A multiscale approach of the corrosion processes, the microstructural states as well as hydrogen influence was performed. This work is supported by ANR-14-CE07-0027-01 – M-SCOT: Multi Scale COrrosion Testing.

No description available.

No description available.

Nos últimos anos houve, no Brasil, um significativo investimento em usinas de álcool para suprir a demanda. Todavia, surgiram problemas de natureza econômica e ambiental, já que a tecnologia atualmente utilizada nas destilarias de álcool produz em média 13 litros de vinhaça para cada litro de álcool. Na busca de uma solução para reduzir o volume deste resíduo, desenvolveu-se um equipamento para concentração de vinhaça, denominado Ecovin, pela empresa Citrotec localizada em Araraquara-SP. Para cada Ecovin são utilizados cerca de 4000 tubos com costura nos trocadores de calor, e para reduzir seu custo de fabricação, avaliou-se como opção o uso de tubos da liga AISI 444. Inserido neste contexto, o presente trabalho procurou caracterizar os mecanismos de corrosão e mostrar de forma comparativa o desempenho dos tubos nas juntas tubo-espelho. Estudo-se, portanto, dois tipos de junta, a do projeto atual, composta por chapa e tubo da liga AISI 316L; e a nova proposta, composta por chapa da liga AISI 316L e tubo da liga AISI 444. Para tanto, iniciou-se com a avaliação da soldabilidade das ligas estudadas, através da caracterização microestrutural, qualificação do procedimento de soldagem da junta tubo-espelho e de ensaios de sensitização nas soldas. Em seguida, ensaios de perda de massa por imersão foram realizados nas soluções de 0,5 M \'H IND.2\'SO IND.4\' e 0,5 M \'H\'CL\', nas temperaturas de 30°C, 50°C, 70°C e 90°C, de acordo com o intervalo de temperatura de operação do Ecovin. Nas mesmas soluções, e na temperatura ambiente, foram realizados ensaios eletroquímicos de polarização potenciodinâmica em amostras que reproduziram o ciclo térmico de soldagem das juntas tubo-espelho estudadas, nas regiões do metal de base, zona afetada pelo calor (ZAC) e no metal de solda. Na junta tubo-espelho a corrosão ocorreu preferencialmente na ZAC formada entre a interface tubo-metal de solda, e no cordão de solda à margem do tubo, com a atuação de mecanismos de corrosão generalizada e localizada. Na junta tubo-espelho dissimilar observou-se que o processo corrosivo foi predominante na superfície do tubo AISI 444, típico do mecanismo de corrosão galvânica, onde o tubo AISI 444 caracterizou-se como a região anódica. O desempenho da liga AISI 316L, assim como a junta soldada composta somente por essa liga, apresentou um melhor desempenho em corrosão, porém, na solução contendo cloreto, a variação da temperatura exerceu uma influência proporcional para ambos os casos avaliados nesse estudo. Destaca-se ainda que a liga AISI 316L sofreu corrosão por pite na ZAC e no metal de solda, em ambas as soluções, com maior severidade do que a liga AISI 444. Os resultados obtidos indicam que para a aplicação requerida, o tubo AISI 444 pode ser utilizado na temperatura de 50°C com satisfatório desempenho e similar à junta composta somente por AISI 316L. / Recently in Brazil there has been constant investments in ethanol plants, to supply the internal and external market, resulting at a high increase of the volume of this product. However, economical and environmental problems arose because of this new demand, whereas the current technologies produce thirteen liters of vinasse for each liter of alcohol. Each ECOVIN uses nearly 4000 welded tubes in the heat exchangers, and there is an option to use welded AISI 444 alloy tubes in order to reduce the manufacture costs of the ECOVIN. In this context, this work determines the corrosion mechanisms and analyzes the performance of welded tubes and the tube-to-tubesheet welded joints. The following types of tube-to-tubesheet were evaluated: current welded joints of this project, with all components manufactured with AISI 316L alloy; and the welded joint suggested for the project, using the welded tubes of AISI 444 alloy and the plate of AISI 316L alloy. For this purpose, the first step was to evaluate the weldability of the studied alloys, through microstructural characterization, welding procedure qualification and the intergranular corrosion test. After that, mass loss tests were conducted in 0,5 M \'H IND.2\'SO IND.4\' and 0,5 M \'H\'CL\' solutions, at 30°C, 50°C, 70°C and 90°C, according to the temperature range of the equipment operating. Electrochemical polarization tests were made in the same solution concentration used in the mass loss tests, but only in room temperature. These tests were made in samples that were welded with the same thermal cycle of the tube-to-tubesheet welded joints, and the evaluations were made on the base metal, heat affected zones and weld metal. The uniform and localized corrosion process occurred preferentially in the interface formed between tube and weld metal, and on weld metal near the tubes. In the tube-to-tubesheet dissimilar welded joints, it was observed that the corrosion process was predominant on the surface of AISI 444 alloy, probably because of the galvanic corrosion process, where the AISI 444 was an anodic region. The best performance on corrosion process was observed in AISI 316L, both the base metal and the similar welded joints. However, for the tests in chloride environment, in this process, the temperature caused a proportional influence in the corrosion rate of AISI 316L and AISI 444. In the AISI 316L alloy it was observed nucleation of pitting in HAZ and in weld metal, in both solutions, and more aggressive than observed in the AISI 444 alloy. The results showed that the AISI 444 alloy can be applied for the initial ranging temperatures of the equipments operation, with satisfactory performance.

Nos últimos anos houve, no Brasil, um significativo investimento em usinas de álcool para suprir a demanda. Todavia, surgiram problemas de natureza econômica e ambiental, já que a tecnologia atualmente utilizada nas destilarias de álcool produz em média 13 litros de vinhaça para cada litro de álcool. Na busca de uma solução para reduzir o volume deste resíduo, desenvolveu-se um equipamento para concentração de vinhaça, denominado Ecovin, pela empresa Citrotec localizada em Araraquara-SP. Para cada Ecovin são utilizados cerca de 4000 tubos com costura nos trocadores de calor, e para reduzir seu custo de fabricação, avaliou-se como opção o uso de tubos da liga AISI 444. Inserido neste contexto, o presente trabalho procurou caracterizar os mecanismos de corrosão e mostrar de forma comparativa o desempenho dos tubos nas juntas tubo-espelho. Estudo-se, portanto, dois tipos de junta, a do projeto atual, composta por chapa e tubo da liga AISI 316L; e a nova proposta, composta por chapa da liga AISI 316L e tubo da liga AISI 444. Para tanto, iniciou-se com a avaliação da soldabilidade das ligas estudadas, através da caracterização microestrutural, qualificação do procedimento de soldagem da junta tubo-espelho e de ensaios de sensitização nas soldas. Em seguida, ensaios de perda de massa por imersão foram realizados nas soluções de 0,5 M \'H IND.2\'SO IND.4\' e 0,5 M \'H\'CL\', nas temperaturas de 30°C, 50°C, 70°C e 90°C, de acordo com o intervalo de temperatura de operação do Ecovin. Nas mesmas soluções, e na temperatura ambiente, foram realizados ensaios eletroquímicos de polarização potenciodinâmica em amostras que reproduziram o ciclo térmico de soldagem das juntas tubo-espelho estudadas, nas regiões do metal de base, zona afetada pelo calor (ZAC) e no metal de solda. Na junta tubo-espelho a corrosão ocorreu preferencialmente na ZAC formada entre a interface tubo-metal de solda, e no cordão de solda à margem do tubo, com a atuação de mecanismos de corrosão generalizada e localizada. Na junta tubo-espelho dissimilar observou-se que o processo corrosivo foi predominante na superfície do tubo AISI 444, típico do mecanismo de corrosão galvânica, onde o tubo AISI 444 caracterizou-se como a região anódica. O desempenho da liga AISI 316L, assim como a junta soldada composta somente por essa liga, apresentou um melhor desempenho em corrosão, porém, na solução contendo cloreto, a variação da temperatura exerceu uma influência proporcional para ambos os casos avaliados nesse estudo. Destaca-se ainda que a liga AISI 316L sofreu corrosão por pite na ZAC e no metal de solda, em ambas as soluções, com maior severidade do que a liga AISI 444. Os resultados obtidos indicam que para a aplicação requerida, o tubo AISI 444 pode ser utilizado na temperatura de 50°C com satisfatório desempenho e similar à junta composta somente por AISI 316L. / Recently in Brazil there has been constant investments in ethanol plants, to supply the internal and external market, resulting at a high increase of the volume of this product. However, economical and environmental problems arose because of this new demand, whereas the current technologies produce thirteen liters of vinasse for each liter of alcohol. Each ECOVIN uses nearly 4000 welded tubes in the heat exchangers, and there is an option to use welded AISI 444 alloy tubes in order to reduce the manufacture costs of the ECOVIN. In this context, this work determines the corrosion mechanisms and analyzes the performance of welded tubes and the tube-to-tubesheet welded joints. The following types of tube-to-tubesheet were evaluated: current welded joints of this project, with all components manufactured with AISI 316L alloy; and the welded joint suggested for the project, using the welded tubes of AISI 444 alloy and the plate of AISI 316L alloy. For this purpose, the first step was to evaluate the weldability of the studied alloys, through microstructural characterization, welding procedure qualification and the intergranular corrosion test. After that, mass loss tests were conducted in 0,5 M \'H IND.2\'SO IND.4\' and 0,5 M \'H\'CL\' solutions, at 30°C, 50°C, 70°C and 90°C, according to the temperature range of the equipment operating. Electrochemical polarization tests were made in the same solution concentration used in the mass loss tests, but only in room temperature. These tests were made in samples that were welded with the same thermal cycle of the tube-to-tubesheet welded joints, and the evaluations were made on the base metal, heat affected zones and weld metal. The uniform and localized corrosion process occurred preferentially in the interface formed between tube and weld metal, and on weld metal near the tubes. In the tube-to-tubesheet dissimilar welded joints, it was observed that the corrosion process was predominant on the surface of AISI 444 alloy, probably because of the galvanic corrosion process, where the AISI 444 was an anodic region. The best performance on corrosion process was observed in AISI 316L, both the base metal and the similar welded joints. However, for the tests in chloride environment, in this process, the temperature caused a proportional influence in the corrosion rate of AISI 316L and AISI 444. In the AISI 316L alloy it was observed nucleation of pitting in HAZ and in weld metal, in both solutions, and more aggressive than observed in the AISI 444 alloy. The results showed that the AISI 444 alloy can be applied for the initial ranging temperatures of the equipments operation, with satisfactory performance.

L’objectif de cette étude est de quantifier la contribution intra et intergranulaire lors d’une sollicitation à haute température d’un alliage de magnésium (AZ31). Afin de répondre à cette problématique scientifique, un essai de traction in situ à haute température dans un MEB a été mis en place. Un important travail de développement a été réalisé autour de cet essai afin de lever un nombre de verrous technique conséquent. Ces verrous expliquent en partie pourquoi il existe aujourd’hui peu d’étude in situ à haute température sur des alliages de magnésium. Un marqueur local ayant la forme d’une microgrille a été déposé sur notre échantillon étant donné que celui-ci n’offre aucun contraste local pour la corrélation d’image numérique (CIN). Afin le dépôt du marqueur local, une cartographie EBSD a été réalisée. À l’aide des joints de grains issus de la carte EBSD, on peut venir superposer les joints de grains aux champs de déformation issue de la CIN.À l’aide des essais de traction in situ à haute température, on a pu mettre en avant l’effet de la température sur les différents mécanismes de déformation actif. Tout ce travail de développement nous permet ainsi de pouvoir localiser les hétérogénéités de déformation plastique à la fois en fonction de l’évolution de la déformation et pour plusieurs températures. D’après les essais menés, on a pu mettre en évidence le fait que plus la température est élevée, que plus les hétérogénéités de déformation plastique se localisent au voisinage des joints de grains. Basé sur une hypothèse cœur/manteau, on a pu venir quantifier la contribution intergranulaire, et mettre en avant que celle-ci devenait plus importante avec la température. / The aim of this study is to quantify the intra and intergranular contribution of the deformation during a high temperature micromechanical test on a magnesium alloy (AZ31). In order to answer this scientific issue, we have developed an in situ tensile test at high temperature within a SEM. It has required a significant preparation work in order to push the current technical limits of this type of test on magnesium alloy. These technical limits can partly explain why there are currently few in situ studies at high temperature on magnesium alloys. A local marker in the form of a microgrid was placed on our sample as it does not provide any local contrast for digital image correlation (DIC). Before the deposition of the microgrid, EBSD mapping was made. Using the grain boundaries from the EBSD, we can superimpose the deformed grain boundaries on the strain map from the DIC.Using high temperature in-situ tensile tests, we were able to highlight the effect of the temperature on the different active deformation mechanisms. This whole development work enables us to locate the plastic deformation heterogeneities both according to the evolution of the deformation and for several temperatures. From the tests conducted, it has been shown that the higher the temperature, the more heterogeneous the plastic deformation heterogeneities are located in the vicinity of the grain boundaries. Based on a heart/coat hypothesis, we were able to quantify the intra and intergranular contribution, and show that it became more important with temperature.

Zr-2.5Nb is currently used for pressure tubes in the CANDU (CANada Deuterium Uranium) reactor. A complete understanding of the deformation mechanism of Zr-2.5Nb is important if we are to accurately predict the in-reactor performance of pressure tubes and guarantee normal operation of the reactors. This thesis is a first step in gaining such an understanding; the deformation mechanism of ZrNb alloys at room temperature has been evaluated through studying the effect of texture and microstructure on deformation. In-situ neutron diffraction was used to monitor the evolution of the lattice strain of individual grain families along both the loading and Poisson’s directions and to track the development of interphase and intergranular strains during deformation. The following experiments were carried out with data interpreted using elasto-plastic modeling techniques: 1) Compression tests of a 100%Zr material at room temperature. 2) Tension and compression tests of hot rolled Zr-2.5Nb plate material. 3) Compression of annealed Zr-2.5Nb. 4) Cyclic loading of the hot rolled Zr-2.5Nb. 5) Compression tests of ZrNb alloys with different Nb and oxygen contents. The experimental results were interpreted using a combination of finite element (FE) and elasto-plastic self-consistent (EPSC) models. The phase properties and phase interactions well represented by the FE model, the EPSC model successfully captured the evolution of intergranular constraint during deformation and provided reasonable estimates of the critical resolved shear stress and hardening parameters of different slip systems under different conditions. The consistency of the material parameters obtained by the EPSC model allows the deformation mechanism at room temperature and the effect of textures and microstructures of ZrNb alloys to be understood. This work provides useful information towards manufacturing of Zr-2.5Nb components and helps in producing ideal microstructures and material properties for pressure tubes. Also it is helpful in guiding the development of new materials for the next generation of nuclear reactors. Furthermore, the large data set obtained from this study can be used in evaluation and improving current and future polycrystalline deformation models. / Thesis (Ph.D, Mechanical and Materials Engineering) -- Queen's University, 2008-09-05 13:51:30.42

Inhomogeneous deformation fields arising from the grain-grain interactions in polycrystalline materials have been evaluated using a crystal plasticity finite element method and extensively compared to neutron diffraction measurements under fatigue crack growth conditions. The roles of intergranular deformation anisotropy, grain boundary damage, and non-common deformation mechanisms (such as twinning for hexagonal close packed crystals) are systematically evaluated. The lattice misorientation field can be used to determine the intragranular deformation behavior in polycrystals or to describe the deformation inhomogeneity due to dislocation plasticity in single crystals. The study of indentation-induced lattice misorientation fields in single crystals sheds lights on the understanding of the scale-dependent plasticity mechanisms. A two-scale micromechanical analysis is performed to study the lattice strain distributions near a fatigue crack tip. The experimental finding of vanishing residual intergranular strain in polycrystals as the increase of the fully reversed loading cycles suggests the intergranular damage be the dominant failure mechanism. Our model predictions are compared to in situ neutron diffraction measurements of Ni-based superalloys under fatigue crack growth conditions. Predicted and measured lattice strains in the vicinity of fatigue crack tips illustrate the important roles played by the intergranular damage and the surrounding plasticity in fatigue growth. Motivated by the synchrotron x-ray measurements of lattice rotation fields in single crystals under indentation, the effect of the orientation of slip systems on the 2D wedge indentation of a model single crystal is investigated. Furthermore, the crystallographic orientations of the indented solids are gradually rotated, resulting changes of lattice misorientation patterns under the indenter. These 2D simulations, as well as a 3D Berkovich indentation simulation, suggest a kinematic relationship between the lattice misorientation and crystalline slip fields. Advanced structural materials such as light-weighted materials, nanocrystalline metals/alloys, and hierarchically structured alloys often encounter unconventional deformation mechanisms. The convolution of crystalline slip and deformation twin are considered in the hexagonal close packed polycrystals. Specifically, we have determined the lattice strain distributions near fatigue crack tips in Zircaloy-4, and the role of tensile-twins on intergranular strain evolution in a wrought Mg alloy, which compare favorable to available neutron diffraction measurements.

Made available in DSpace on 2014-10-09T12:54:28Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:07:42Z (GMT). No. of bitstreams: 0 / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energéticas e Nucleares - IPEN/CNEN-SP