O aço SAE 1552 modificado é um desenvolvimento recente da família do aço carbono manganês ligado ao silício, sendo utilizado para confecção de grampo U que tem como finalidade prender o feixe de molas no eixo do veículo. A somatória das fases de produção dessa matéria prima introduz os limites de resistência mecânica final necessária para atender a classe de resistência normativa. A peça produzida com esse aço tem alcançado crescimento de utilização na indústria automotiva devido à mesma apresentar propriedades mecânicas que atendem a requisitos normativos de classe de resistência e com vantagem de evitar tratamento térmico na fase de confecção do grampo e sendo esse processo realizado a frio em todas as suas fases. O objetivo desse trabalho foi estudar falha de grampo na etapa do processo de dobramento em forma de U e aplicar ensaios como: programa de simulação de tratamento térmico Stecal 3.0, ultrassom, fadiga, teste de cela e análise de fratura para solucionar essas falhas. Também foi realizado ensaios para prever fraturas catastróficas como: elementos finitos através de programa de computador Abaqus, ensaio de extensometria, tenacidade a fratura e medições de tensões residuais através de técnica de difração de raios-x. Foi concluído através dos resultados dos estudos de microestrutura resultante de tratamento térmico da matéria prima que o processo com resfriamento controlado em esteira é mais adequado para a produção do aço para confecção de grampo. O ensaio de ultrassom antes e após ensaio de fadiga possibilitou dimensionar o crescimento da profundidade da trinca em cotovelo de grampo e através de elementos finitos e extensometria associado com mecânica da fratura foi possível conhecer as tensões em ponto de estudo e entender o motivo de não ocorrer falha catastrófica. O ensaio de difração de raios-x permitiu o entendimento das tensões residuais introduzidas na peça de estudo. / SAE 1552 steel modified is a recent development of manganese carbon steel group linked to silicon, which is used to manufacture u-bolt that aims to fix leaf spring at vehicle axle in the back part. The sum of production stages of this raw material introduces the final mechanical resistance limits to meet class rules resistance. The piece produced with this steel has achieved growth of use in the automotive industry due to the mechanical properties it presents, which meet regulatory requirements for strength class and the advantage of avoiding heat treatment during manufacturing of the u-bolt and all the phases of this process are carried out in cold. This work aims to study the u-bolt failure during the folding process in the form of U and apply tests such as heat treatment simulation -Stecal 3.0, ultrasonic test, fatigue test, cell testing and analysis of crack. Other tests have been carried out to predict catastrophic fractures such as: finite element through computer program called Abaqus, extensometry testing, toughness testing for fracture and residual stress measurement by X ray diffraction technique. Results of heat treatment studies, by microstructure analysis, allowed choosing appropriate process for steel production. Ultrasonic testing before and after fatigue testing enabled to measure growth of crack depth on u-bolt elbow, and through finite element and extensometry testing associated with Mechanical of Fracture it was possible to know the stress concentrated at a point and to understand why catastrophic failure did not occur. Residual stress understanding has provided overall vision of u-bolt studied and contributed to have precision in measurement at inner and outer part of the u-bolt elbow.

Materiais frágeis, tal como o silício, têm sido utilizados em sistemas microeletromecânicos, semicondutores e dispositivos ópticos infravermelhos. Estes materiais são considerados de difícil usinabilidade devido à tendência de sofrerem fraturas. O grande desafio na usinagem dos materiais cristalinos é alcançar uma remoção de material por deformações plásticas (regime dúctil), pois, nessas condições as superfícies ópticas usinadas são geradas sem nenhum dano. Esse regime de usinagem pode ser alcançado em escalas submicrométricas, de forma que, em muitos cristais, as pressões impostas pela ferramenta são altas o suficiente para conduzirem uma transformação de fase do material, favorecendo, assim, a usinagem. Embora pesquisas sobre a relação entre a endentação e a usinagem tenham sido desenvolvidas, a busca por métodos matemáticos com base nas forças e deformações de endentação para serem usados em usinagem de modo a identificar as condições ótimas para remoção de material em regime dúctil não são triviais. O presente trabalho propõe uma relação mais direta com os resultados de endentação para determinar os parâmetros ótimos de usinagem dos materiais frágeis, correlacionando a área da face do endentador em contato e a área efetiva da secção de corte em usinagem. Para isso, ensaios de endentação e experimentos de usinagem com ferramenta de diamante foram realizados em escala micro e nanométrica. O material analisado aqui foi o silício monocristalino (100). Uma matriz experimental foi planejada para as possíveis correlações da variação do ângulo de saída da ferramenta e do avanço de usinagem com as áreas de endentação e o surgimento das trincas e fraturas; forças de usinagem e a pressão de transição frágil-dúctil; tensão residual; espessura crítica de corte e o estado das superfícies usinadas. Em relação às durezas obtidas, foi preciso separá-las em dois estágios: antes do surgimento das trincas durante a endentação e depois desse ponto. Durante a usinagem, a melhor remoção de material em regime dúctil foi obtida na direção mais dura do silício. Os ângulos de saída que proporcionaram resultados desfavoráveis em termos de integridade superficial foram o de -25° e ângulos mais negativos que -60°. A pressão de transição se apresentou de 12 GPa a 13 GPa, sendo que as energias específicas de corte seguiram o mesmo comportamento: 9 j/mm³ a 10 j/mm³ respectivamente. A tensão residual se mostrou inversamente proporcional às forças de usinagem. As espessuras crítica-efetivas de corte variaram de 100 nm a 560 nm. Os valores das espessuras críticas de corte estimadas pelos ensaios de endentação variaram de 200 nm a 530 nm. Portanto, foi possível mostrar que os valores de espessura crítica estimados pelo método proposto, com base nos resultados de endentação, corresponderam muito bem às espessuras críticas obtidas nos experimentos de usinagem. Assim sendo, torna-se possível determinar por meio de tal técnica os valores ótimos de usinagem, podendo ser aplicada para qualquer material cristalino. / Brittle materials, such as silicon, have been used in microelectromechanical systems, semiconductor and infrared optical devices. These types of materials are considered of difficult to machine due to the tendency to suffer fractures. The great challenge in the machining of crystalline materials is to achieve a removal of material by plastic deformations (ductile regime), because in these conditions the machined optical surfaces are generated without any superficial damage. This type of machining can be achieved on a submicrometric machining scale, so that the pressures imposed by the tool are high and lead to a phase transformation of many crystals favoring the machining in ductile regime. Although research on the relationship between microindentation and micromachining has been developed, the search for mathematical methods based on the forces and the deformations of indentation to be used in machining in order to identify the machining conditions under regime ductile are non-trivial. The present work proposes a more direct relationship with the results of the indentation to determine the optimal parameters of the fragile materials, correlating the indenter face area and the cutting section effective area in machining. For this purpose, indentation tests and diamond tool machining experiments were carried out on a micro and nanometric scale. The material analyzed here was monocrystalline silicon (100). An experimental matrix was planned for the possible correlations of the variation of the tool rake angle and of the machining feed with the areas of indentation and the beginning of cracks and fractures; cutting forces and the fragile-ductile transition pressure; residual stress; critical cutting thickness and the state of machined surfaces. In relation to the hardness obtained, it was necessary to separate them in two stages: before the emergence of the cracks during the indentation and after that point. During machining, the best removal of ductile material was obtained in the hardest direction of the silicon. The rake angles which gave unfavorable results in terms of surface integrity were -25° and angles more negative than -60°. The transition pressure reached values from 12 GPa to 13 GPa, and the specific shear energies followed the same behavior: 9 j/mm³ at 10 j/mm³ respectively. The residual stress was inversely proportional to the machining forces. Critical-effective uncut thicknesses ranged from 100 nm to 560 nm. The values of the critical uncut thicknesses estimated by the indentation tests ranged from 200 nm to 530 nm. Therefore, it was possible to show that the critical thickness values estimated by the proposed method, based on indentation results, corresponded very well to the critical thickness obtained in the machining experiments. Thus, it is possible to determine by means of such a technique the optimum values of machining, which can be applied to crystalline material.

Made available in DSpace on 2017-07-21T20:43:45Z (GMT). No. of bitstreams: 1 Natany Dayani de Souza Assai.pdf: 1950917 bytes, checksum: a6c8b87bcaabbbdbf5ca798360a90bcc (MD5) Previous issue date: 2014-08-27 / The residual stress may decrease and redistribute through a process called relaxation. The relaxation of the residual stress is an important phenomenon in relation to the estimated fatigue resistance of the material and can occur due to static mechanical loading, thermal, cyclical and extension fatigue effects. Residual stresses are usually harmful for overlapping the operating voltage, while the fatigue resistance of metals and alloys can be improved by compressive residual stresses present in the surface layer by means of shot peening surface. The fatigue life with the compressive residual stress field caused by shot peening or sophisticated models for modeling voltage field Compressive Residual (CTRC) usually does not take into account the possibility of this change during the cyclic loading, ie , place the relaxation process, which also changes the fatigue life. This study aimed to obtain the residual stress profile relaxation by cyclic loading on aluminum alloy samples 7050- T7541 with shot peening glass and ceramics subjected to axial fatigue test. The technique for determining the residual stress was the X-ray diffraction for measuring accurately the redistribution of residual stresses along the depth of fatigue produced by the process. The removal of layers of material was performed by electrolytic attack. Hereby, it was possible to establish the relationship between the maximum stress and number of cycles in relation to the greater or lesser relaxation test specimens in different regimes of cyclic peening conditions with spherical glass and ceramics in the longitudinal and transverse directions. The results showed that the samples with the longitudinal direction shot peening redistribution showed higher compressive residual stresses in the transverse direction along the depth. For the samples of shot peening ceramic was virtually no relaxation on the surface only in depth when compared to the original profile, samples of ceramic shot peening obtained relaxation in remote locations of the surface, due to the influence of roughness. The redistribution of stresses for samples of shot peening glass were higher than those with shot peening ceramic along the depth in all cyclic regimens studied in the L and T directions. The residual stress relaxation occurred in both directions did not compromise beneficial effect of shot peening increase the fatigue life thereof, in relation to the base material. / As tensões residuais podem diminuir e se redistribuir por meio de um processo chamado relaxação. A relaxação das tensões residuais é um fenômeno importante no que se refere à previsão da resistência à fadiga dos materiais e pode ocorrer devido a carga mecânica estática, térmica, cíclica como efeitos de extensão da fadiga. As tensões residuais geralmente são prejudiciais por se sobreporem às tensões de serviço, enquanto a resistência à fadiga dos metais e ligas pode ser melhorada por tensões residuais compressivas presentes nas camadas superficiais por meio do tratamento de superfície de shot peening. A vida em fadiga com o campo de tensão residual compressiva originada pelo shot peening ou modelos sofisticados para a modelagem do Campo de Tensão Residual Compressivo (CTRC), geralmente não leva em consideração, a possibilidade deste alterar-se durante o carregamento cíclico, ou seja, ocorrer o processo de relaxação, que também altera a vida em fadiga. Este trabalho teve como objetivo obter o perfil de tensão residual de relaxação por carregamento cíclico em amostras de liga de alumínio 7050- T7541 com shot peening de vidro e cerâmica submetidas a ensaio de fadiga axial. A técnica para determinação das tensões residuais foi a difração de raios X que permite medir com precisão a redistribuição de tensões residuais ao longo da profundidade produzidas pelo processo de fadiga. A remoção das camadas de material foi realizada por ataque eletrolítico. Por meio deste, foi possível constatar a relação entre a tensão máxima e quantidade de ciclos no que se refere à maior ou menor relaxação de corpos de prova em diferentes regimes cíclicos nas condições de shot peening com esfera de vidro e cerâmica nas direções longitudinal e transversal à laminação.Os resultados mostraram que as amostras com shot peening na direção longitudinal apresentaram redistribuição de tensões residuais compressivas maiores que no sentido transversal ao longo da profundidade. Para os corpos de prova de shot peening de cerâmica praticamente não houve relaxação na superfície apenas na profundidade quando comparado ao perfil original, as amostras de shot peening de cerâmica obtiveram a relaxação em posições mais afastadas da superfície, devido a influência da rugosidade. A redistribuição de tensões para as amostras de shot peening de vidro foram superiores em relação aquelas com shot peening de cerâmica ao longo da profundidade em todos os regimes cíclicos estudados nas direções L e T. A relaxação de tensão residual ocorrida em ambas direções não comprometeu o efeito benéfico do shot peening no aumento da vida em fadiga das mesmas em relação ao material base.

Este trabalho tem a intenção de contribuir com informações sobre a integridade superficial resultante do processo de torneamento em material endurecido de componentes mecânicos fabricados em aço cementado ABNT 8620 (DIN 21 NiCrMo 2). A análise das tensões residuais do corpo de prova foi experimentalmente conduzida pelo Método do Furo Cego Incremental, no qual um pequeno furo é introduzido na superfície do componente e a deformação aliviada é registrada por meio de extensômetros especiais, e também, pelo método da difração de raios-X. A superfície foi analisada através de parâmetros obtidos do mapeamento tridimensional da topografia superficial com instrumento de interferometria laser. Os parâmetros de rugosidade, selecionados para medição, visaram uma caracterização funcional das superfícies obtidas, tais como capacidade de carga, capacidade de retenção de fluidos lubrificantes e resistência ao desgaste. Também foram executados ensaios metalográficos para avaliar a existência de camadas de material alteradas abaixo da superfície. Os resultados indicaram que o torneamento em material endurecido foi capaz de produzir uma superfície resultante com boa área de contato, boa capacidade de carregamento e razoável capacidade de retenção de fluidos uma vez que nem todos os parâmetros se encontraram na faixa funcional ideal. O torneamento em material endurecido induziu tensão de compressão nas camadas das amostras cementadas, cuja condição original era tensão residual de tração. Não foram detectadas alterações expressivas na camada cementada, principalmente na região limítrofe da área transversal com a superfície devido ao aquecimento e rápido resfriamento imposto pelo processo de usinagem. / The aim of the present work is to provide relevant information regarding the obtained surface integrity during hard turning process of mechanical components manufactured from case hardened steel ABNT 8620 (DIN 21 NiCrMo 2). The sample residual stress analysis has been experimentally conducted by the incremental Blind Hole method, in which a small hole is machined on the surface of the component and the relieved deformation is recorded through special strain gages, and by the X-ray diffraction technique. The surface was examined by parameters obtained from the surface topography three-dimensional mapping with a laser interferometer instrument. The selected roughness parameters analysis intends to have a functional characterization such as bearing capacity, fluid and lubricants retention ability and contact wear resistance. In the search for altered material layers beneath the surface, metallographic studies were carried out. The functional bearing area curve analysis parameters indicated that the resulting surface has a good area contact, good bearing capacity and reasonable ability to fluid retention as the reduced valley depth parameter did not produced negative values for all conditions tested. The hard turnig process was able to add compression residual stress condition at the surface, and no significant changes were found at the case hardened layer due to rapid heating and cooling imposed by the hard turning process.

Les films de ZrO2 pur sont déposés par MOCVD (Metal-Organic Chemical Vapor Deposition) en variant de nombreux paramètres du processus. L’influence des conditions de dépôt sur l’évolution de la microstructure (morphologies, structure cristalline/phase, texture et contrainte résiduelle) a été étudiée et clarifiée. Par des analyses approfondies des résultats expérimentaux, trois mécanismes typiques de croissance de dépôt de ZrO2 ont été proposées. Les contraintes de croissance de compression sont en relation directe avec la diffusion atomique et la quantité d’espèces piégées dans les films. La formation de la texture cristallographique est complexe et deux types de textures ont été analysées dans la phase tétragonale : la texture de fibre {1 1 0}t est contribuée par l’effet superplastique des nano-cristallites de ZrO2 et par la contrainte de croissance de compression ; tandis que la morphologie en facette est due à la croissance concurrentielle de différents plans cristallographiques. La stabilisation de la phase tétragonale de ZrO2 a été analysée et discutée. En plus de la taille critique des cristallites, la stabilisation de la phase tétragonale est favorisée par deux autres mécanismes : la grande quantité des défauts cristallins et la morphologie des cristallites. / Pure ZrO2 films were deposited by MOCVD (Metal-Organic Chemical Vapor Deposition) by varying the deposition parameters over large range. The influence of deposition conditions on the evolution of the microstructure (morphology, crystal structure / phase, texture and residual stress) was studied and clarified. Through careful study and analysis of experimental results, three typical mechanisms of deposition of ZrO2 have been proposed. The compressive growth stresses are directly related to atomic diffusion and the trapped-in effects during deposition. The formation of crystallographic texture is complex and two types of textures were analyzed in the tetragonal phase: the fiber texture {1 1 0}t is supposed to be the result of the effect of superplastic of ZrO2 nano-crystallites and the compressive growth stress, while the facet morphology (the {0 1 1}t fiber) is due to the competitive growth of different crystallographic planes. The stabilization of the tetragonal phase of ZrO2 was analyzed and discussed. In addition to the critical size of crystallites, the stabilization of the tetragonal phase can be favored by two mechanisms: the large amount of crystal defects and morphology of crystallites.

L’imagerie multispectrale permet d’améliorer la détection et la reconnaissance de cibles dans les applications de surveillance. Elle consiste à analyser des images de la même scène acquises simultanément dans plusieurs bandes spectrales grâce à un filtrage. Cette thèse étudie la possibilité de réaliser une matrice de 4 filtres Fabry Pérot (FP) intégrés 3D et ajustables par actionnement électrostatique dans le domaine visible-proche infrarouge. Les miroirs fixes des filtres FP sont des multicouches ZnS/YF₃ déposés sur un wafer de borosilicate, et les miroirs mobiles sont des membranes multicouches PECVD SiNH/SiOH encastrées sur une structure mobile très compacte micro-usinée dans un wafer en silicium. Les performances optiques des filtres FP ont été optimisées en prenant en compte la dissymétrie et le déphasage à la réflexion des miroirs. La structure mobile a été modélisée par éléments finis pour minimiser ses déformations lors de l’actionnement. Les étapes critiques des procédés de fabrication des miroirs mobiles en technologie Si ou SOI ont été mises au point : i) la fabrication et la libération par gravures profondes DRIE et XeF₂ des membranes multicouches avec une contrainte résiduelle ajustée par recuit et une réflectance voisine de 50% dans une large gamme spectrale, ii) le contrôle des vitesse de la gravure DRIE avec des motifs temporaires permettant la gravure simultanée de motifs de largeur et de profondeur variables, et iii) la délimitation de motifs sur surfaces fortement structurées à l’aide de pochoirs alignés mécaniquement ou de films secs photosensibles. Ces travaux ouvrent la voie vers une réalisation complète d’une matrice de filtres FP intégrés 3D. / Multispectral imaging is used to improve target detection and identification in monitoring applications. It consists in analyzing images of the same scene simultaneously recorded in several spectral bands owing to a filtering. This thesis investigates the possibility to realize, an array of four 3D integrated Fabry-Perot (FP) filters that are tunable in the visible-near infrared range by electrostatic actuation. The fixed mirrors of the FP filters are ZnS/YF₃ multilayers deposited on a borosilicate wafer, and the movable mirrors are PECVD SiNH/SiOH multilayer membranes clamped in a very compact movable structure micromachined in a Si wafer. A 3rd glass wafer is used for filters packaging. Optical performances of the FP filters have been optimized by taking into account the asymmetry and the reflection phase shift of the mirrors and the mobile structure has been modeled by finite elements analysis notably to minimize its deformation during actuation. The critical steps of the movable mirrors fabrication process in Si or SOI technology have been developed : i) the fabrication and the release by DRIE and XeF₂ etching of 8 or 12 layers membranes with a residual stress tunable by annealing and a reflectance close to 50% in broad wavelength range (570-900nm), ii) the control with temporary patterns of the simultaneous deep etching of patterns with different widths and depths, and iv) various patterning techniques on highly structured surfaces based on shadow masks (with mechanical alignment) or laminated photosensitive dry films. These results open the way towards the full realization of an array of 3D integrated FP filters.

Materiais frágeis, tal como o silício, têm sido utilizados em sistemas microeletromecânicos, semicondutores e dispositivos ópticos infravermelhos. Estes materiais são considerados de difícil usinabilidade devido à tendência de sofrerem fraturas. O grande desafio na usinagem dos materiais cristalinos é alcançar uma remoção de material por deformações plásticas (regime dúctil), pois, nessas condições as superfícies ópticas usinadas são geradas sem nenhum dano. Esse regime de usinagem pode ser alcançado em escalas submicrométricas, de forma que, em muitos cristais, as pressões impostas pela ferramenta são altas o suficiente para conduzirem uma transformação de fase do material, favorecendo, assim, a usinagem. Embora pesquisas sobre a relação entre a endentação e a usinagem tenham sido desenvolvidas, a busca por métodos matemáticos com base nas forças e deformações de endentação para serem usados em usinagem de modo a identificar as condições ótimas para remoção de material em regime dúctil não são triviais. O presente trabalho propõe uma relação mais direta com os resultados de endentação para determinar os parâmetros ótimos de usinagem dos materiais frágeis, correlacionando a área da face do endentador em contato e a área efetiva da secção de corte em usinagem. Para isso, ensaios de endentação e experimentos de usinagem com ferramenta de diamante foram realizados em escala micro e nanométrica. O material analisado aqui foi o silício monocristalino (100). Uma matriz experimental foi planejada para as possíveis correlações da variação do ângulo de saída da ferramenta e do avanço de usinagem com as áreas de endentação e o surgimento das trincas e fraturas; forças de usinagem e a pressão de transição frágil-dúctil; tensão residual; espessura crítica de corte e o estado das superfícies usinadas. Em relação às durezas obtidas, foi preciso separá-las em dois estágios: antes do surgimento das trincas durante a endentação e depois desse ponto. Durante a usinagem, a melhor remoção de material em regime dúctil foi obtida na direção mais dura do silício. Os ângulos de saída que proporcionaram resultados desfavoráveis em termos de integridade superficial foram o de -25° e ângulos mais negativos que -60°. A pressão de transição se apresentou de 12 GPa a 13 GPa, sendo que as energias específicas de corte seguiram o mesmo comportamento: 9 j/mm³ a 10 j/mm³ respectivamente. A tensão residual se mostrou inversamente proporcional às forças de usinagem. As espessuras crítica-efetivas de corte variaram de 100 nm a 560 nm. Os valores das espessuras críticas de corte estimadas pelos ensaios de endentação variaram de 200 nm a 530 nm. Portanto, foi possível mostrar que os valores de espessura crítica estimados pelo método proposto, com base nos resultados de endentação, corresponderam muito bem às espessuras críticas obtidas nos experimentos de usinagem. Assim sendo, torna-se possível determinar por meio de tal técnica os valores ótimos de usinagem, podendo ser aplicada para qualquer material cristalino. / Brittle materials, such as silicon, have been used in microelectromechanical systems, semiconductor and infrared optical devices. These types of materials are considered of difficult to machine due to the tendency to suffer fractures. The great challenge in the machining of crystalline materials is to achieve a removal of material by plastic deformations (ductile regime), because in these conditions the machined optical surfaces are generated without any superficial damage. This type of machining can be achieved on a submicrometric machining scale, so that the pressures imposed by the tool are high and lead to a phase transformation of many crystals favoring the machining in ductile regime. Although research on the relationship between microindentation and micromachining has been developed, the search for mathematical methods based on the forces and the deformations of indentation to be used in machining in order to identify the machining conditions under regime ductile are non-trivial. The present work proposes a more direct relationship with the results of the indentation to determine the optimal parameters of the fragile materials, correlating the indenter face area and the cutting section effective area in machining. For this purpose, indentation tests and diamond tool machining experiments were carried out on a micro and nanometric scale. The material analyzed here was monocrystalline silicon (100). An experimental matrix was planned for the possible correlations of the variation of the tool rake angle and of the machining feed with the areas of indentation and the beginning of cracks and fractures; cutting forces and the fragile-ductile transition pressure; residual stress; critical cutting thickness and the state of machined surfaces. In relation to the hardness obtained, it was necessary to separate them in two stages: before the emergence of the cracks during the indentation and after that point. During machining, the best removal of ductile material was obtained in the hardest direction of the silicon. The rake angles which gave unfavorable results in terms of surface integrity were -25° and angles more negative than -60°. The transition pressure reached values from 12 GPa to 13 GPa, and the specific shear energies followed the same behavior: 9 j/mm³ at 10 j/mm³ respectively. The residual stress was inversely proportional to the machining forces. Critical-effective uncut thicknesses ranged from 100 nm to 560 nm. The values of the critical uncut thicknesses estimated by the indentation tests ranged from 200 nm to 530 nm. Therefore, it was possible to show that the critical thickness values estimated by the proposed method, based on indentation results, corresponded very well to the critical thickness obtained in the machining experiments. Thus, it is possible to determine by means of such a technique the optimum values of machining, which can be applied to crystalline material.

La corrosion sous contrainte par l’iode (CSC-I) est l’un des mécanismes de rupture potentiels des crayons combustibles en alliage de zirconium, pouvant intervenir au cours des transitoires de puissance des réacteurs nucléaires. La fissuration par CSC-I comporte trois étapes : amorçage de la fissure, développement intergranulaire puis propagation transgranulaire. Le but du travail est d’identifier des paramètres critiques gouvernant les transitions entre ces différentes étapes. En premier lieu, des essais sur des éprouvettes en Zircaloy présentant des finitions de surface et des états métallurgiques variés permettent de discriminer l’influence de différents paramètres sur l’amorçage des fissures. Nous mettons en évidence le rôle critique du niveau des contraintes résiduelles, de leur répartition en surface ainsi que de leur profil au sein du matériau. La sensibilité des alliages à l’amorçage des fissures n’est pas directement corrélée à la rugosité de la surface. Cependant, la dispersion des paramètres de rugosité traduit l’irrégularité du profil, l’hétérogénéité du niveau des contraintes résiduelles, et donc l’existence de zones où les contraintes résiduelles sont localement moins protectrices. Dans un second temps, des éprouvettes de Zircaloy-4 possédant différents états d’écrouissage sont sollicitées sous charge constante, en présence de méthanol iodé. Les modifications microstructurales induites par l’écrouissage favorisent l’apparition de la propagation transgranulaire des fissures de CSC-I. Des observations des faciès de rupture en MET révèlent que la transition inter/transgranulaire intervient dans des zones où les grains sont fortement désorientés les uns par rapport aux autres, suite à l’augmentation des contraintes locales résultant des incompatibilités de déformation grain à grain. / Iodine-induced stress corrosion cracking (I-SCC) is one of the potential failure modes of zirconium alloy fuel claddings during power transients in nuclear reactors. I-SCC failures are usually described in three steps: initiation of cracks, intergranular development and transgranular propagation. The objective of this work is to identify critical parameters controlling transitions between crack propagation modes. First of all, experiments conducted on Zircaloy samples with various surface conditions and metallurgical states lead to discriminate the influence of several parameters responsible for cracks initiation. The critical role of residual stresses level, their distribution at the subsurface and their evolution in the bulk of the material is evidenced. Sensitivity to I-SSC is not directly correlated to surface roughness. However, dispersion in roughness parameters indicates the presence of surface irregularities, heterogeneities of residual stresses and the existence of surface areas where residual stresses are less protective. In a second step, Zircaloy-4 samples with various strain-hardening pre-treatments are submitted to constant load tests in an iodine methanol solution. Microstructural modifications induced by a strain-hardening pre-treatment enhance transgranular propagation of I-SCC cracks. TEM observations of fracture surfaces show that the intergranular to transgranular crack transition takes place preferentially where the relative crystallographic orientation is large between two adjacent grains, because of local stress concentrations resulting from strain incompatibilities between neighbouring grains.

Welding of duplex stainless steel pipeline material for the oil and gas industry is now common practice. To date, research has been conducted primarily on the parent material and heat affected zones in terms of its susceptibility to various forms of corrosion. However, there has been little research conducted on the degree of sensitisation of the various successive weld layers, namely the root, fill and cap layers. The focus of this research study was to: (i) provide an in-depth microstructural analysis of the various weld passes, (ii) study the mechanical properties of the weld regions; (iii) determine degree of sensitisation of the various weld passes; and (iv) investigate the residual stress levels within the various regions/ phases of the welds. Four test conditions were prepared using manual Gas Tungsten Arc Welding with 'V' and 'U' bevel configuration. Structural analysis consisted of (i) optical microscopy, scanning electron microscopy and magnetic force microscopy; (ii) ferrite determination using Magna-Gauge, Fischer Ferrite-scope and Point Count method. Mechanical testing consisted of Vickers hardness measurements, Charpy impact studies and transverse tensile testing. The degree of sensitisation was determined by three test methods: a modified ASTM A262, ASTM A923 and a modified Double Loop Electrochemical Potentiodynamic Reactivation (DL-EPR) test. Residual stress levels were determined using two neutron diffraction techniques: a reactor source and a time of flight spallation source. Microstructure observed by optical microscopy and magnetic force microscopy shows the formation of both fine and coarse structures within the weld metal. There was no evidence of secondary austenite, being present in any of the weld metal conditions examined. In addition, no detrimental intermetallic phases or carbides were present. The DL-EPR test results revealed that the fill layer regions for all four conditions and the base material showed the highest values for Ir/Ia and Qr/Qa. All four test conditions passed the ASTM A262 and A923 qualitative type tests, even under restricted and modified conditions. Residual stress measurements by neutron diffraction conducted at Lucas Heights Hi-Flux Reactor revealed that the ferrite phase stress was tensile in the heat affected zones and weld, and appeared to be balanced by a local compressive austenite phase stresses in the normal and transverse directions. Residual stress measurements by neutron diffraction conducted at Los Alamos Nuclear Science Centre revealed that in the hoop direction, ferrite (211) and austenite (311) exhibit tensile strains in the weld. In the axial and radial direction, the strains for both phases were more compressive. Correlations between the degree of sensitization and microstructural changes / ferrite content were observed. Higher degrees of sensitization (Ir/Ia and Qr/Qa) were associated with reduced ferrite (increased austenite) content. Correlations between the stresses generated, the evolved microstructures and degree of sensitization were evident. Stresses within the cap region were generally shown to be of a tensile nature in the transverse and longitudinal direction. In summary, the study has shown that correlations exist between the weld microstructure, susceptibility to sensitisation and levels / distribution of internal stresses within the weld regions.

Durch erstmalige Anwendung des η-Umlaufverfahrens auf mechanisch ermüdete Ni-Polykristalle konnten – aufgrund konstanter Meßbedingungen und konstanter Eindringtiefe der Röntgenstrahlung – genauere Eigenspannungsmessungen durchgeführt werden als bisher. Ein speziell entwickeltes Auswertungsverfahren, das auf die Eigenspannungsanalyse von η-Umlaufmessungen abgestimmt ist, wird als „sin2η-Methode“ detailliert vorgestellt. Die experimentellen Resultate unterstreichen die Vorteile, die sich – besonders im Falle sehr geringer Eigenspannungen und wenn auch der dehnungsfreie Ausgangszustand (d0 -Wert) gemessen werden konnte – aus der Nutzung dieser Methode ergeben. Mit Hilfe des magnetischen Barkhausen-Rauschens durchgeführte Vergleichsuntersuchungen stehen im Einklang mit den röntgenographischen Messungen. / When applying the η-rotation-method to mechanically fatigued Ni polycrystals the first time, stress measurements with higher accuracy could be realized due to the constant penetration depth of the X-rays and because of constant measuring conditions. A specifically developed procedure, tuned to analyze residual stresses from η-rotation measurements, will be presented in detail as „sin2η-method“. The experimental results emphasize the benefits of using this method – especially in the case of very low residual stresses and if the initial strain-free state (d0 -value) was obtained from reference measurements. Comparative investigations by means of the magnetic Barkhausen noise agree with the X-ray measurements.