Stainless steels are very important engineering materials in a variety of applications such as in the food industry and nuclear power plants due to their combination of good mechanical properties and high corrosion resistance. However, ferrite-containing stainless steels are sensitive to the so-called ‘475°C embrittlement’, which is induced by phase separation of the ferrite phase, where it decomposes into Fe-rich ferrite (α) and Cr-rich ferrite (α'). The phase separation is accompanied with a severe loss of toughness. Therefore, the upper service temperature of ferrite-containing stainless steels in industrial applications has been limited to around 250°. In the present work, Fe-Cr based steels were mainly investigated by atom probe tomography. A new method based on the radial distribution function (RDF) was proposed to quantitatively evaluate both the wavelength and amplitude of phase separation in Fe-Cr alloys from the atom probe tomography data. Moreover, a simplified equation was derived to calculate the amplitude of phase separation. The wavelength and amplitude was compared with evaluations using the auto-correlation function (ACF) and Langer-Bar-on-Miller (LBM) method, respectively. The results show that the commonly used LBM method underestimates the amplitude of phase separation and the wavelengths obtained by RDF shows a good exponential relation with aging time which is expected from the theory. The RDF is also an effective method in detecting the phenomena of clustering and elemental partitioning. Furthermore, atom probe tomography and the developed quantitative analysis method have been applied to investigate the influence of different factors on the phase separation in Fe-Cr based alloys by the help of mainly mechanical property tests and atom probe tomography analysis. The study shows that: (1) the external tensile stress during aging enhances the phase separation in ferrite. (2) Phase separation in weld bead metals decomposes more rapidly than both the heat-affected-zone metals and the base metals mainly due to the high density of dislocations in the welding bead metals which could facilitate the diffusion. (3) The results show that Ni and Mn can enhance the phase separation comparing to the binary Fe-Cr alloy whereas Cu forms clusters during aging. (4) Initial clustering of Cr atoms was found after homogenization. Two factors, namely, clustering of Cr above the miscibility gap and clustering during quenching was suggested as the two responsible mechanisms. (5) The homogenization temperatures significantly influence the evolution of phase separation in Fe-46.5at.%Cr. / <p>QC 20140910</p> / Spinodal Project

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Le matériau principal de cette étude est l’acier inoxydable austénitique 316L(N) (X2CrNiMo17-12-2 à teneur en azote contrôlée) envisagé dans la conception de la cuve et des structures du circuit primaire des futurs réacteurs de quatrième génération refroidis au sodium. Pour assembler des composants de forte épaisseur, il faut réaliser des soudages multipasses avec métal d'apport. Lors du soudage, il a parfois été constaté des défauts de fissuration à chaud de solidification au refroidissement dans la zone pâteuse, près du bain de fusion. Ces fissures sont des décohésions du matériau apparaissant à haut température le long des joints de grains lorsque la déformation dépasse un seuil critique. Il est donc nécessaire de prévenir ce risque en utilisant un critère de fissuration à chaud. L'approche utilisée dans cette étude est double : développer un essai de fissuration à chaud à chargement extérieur, puis simuler numériquement ces expériences pour déterminer un seuil critique en déformation en utilisant un critère proposé par Kerrouault. Une version améliorée d’un essai de fissuration à chaud (Controlled Restraint Weldability (CRW) test) a été proposé dans cette étude afin d'analyser la susceptibilité à la fissuration de solidification du matériau 316L(N) et d’un métal d'apport de nuance Thermanit 19-15H. L'objectif de ce test est, en fonction de l'intensité du chargement extérieur, d'amorcer une fissure dans un régime thermique établi, puis d’arrêter la propagation de cette fissure si les conditions thermomécaniques locales sont remplies. Le modèle de comportement du matériau choisi est une loi élasto-visco-plastique à écrouissage mixte. Des essais thermomécaniques sur un simulateur Gleeble ont été réalisés à haute température afin d'identifier et d’améliorer la loi de comportement du matériau 316L(N). Le grossissement des grains dans la zone affectée thermiquement a été modélisé et intégré dans ce modèle. Les intervalles de fusion et de solidification du matériau 316L(N) ont été déterminés par des essais ATD (Analyse Thermique Différentielle). Des analyses des microstructures de solidification ont été également menées afin de mieux comprendre le phénomène de fissuration à chaud. Certains essais CRW ont ensuite été modélisés et simulés par éléments finis en utilisant les logiciels Cast3M et Abaqus afin valider le critère de fissuration à chaud et de déterminer un seuil critique de fissuration pour l'acier 316L(N). / The austenitic stainless steel AISI 316L(N) (X2CrNiMo17-12-2) with controlled nitrogen content is widely used for manufacture of vessel and primary circuit structures of the 4th Generation sodium- cooled fast reactors. Multi-pass welds with an appropriate filler metal is used to assemble thick components. Solidification cracks may occur in the mushy zone near the melting weld poor during solidification when a liquid film is distributed along grains boundaries and interdendritic regions and the shrinkage strains across the boundaries cannot be accommodated. It is therefore necessary to prevent this defect using a hot cracking criterion. The approach used in this study is to initiate experimentally a hot crack by a weldability test, and then to simulate these tests to identify a critical strain using a hot crack criterion for the prediction of solidification cracking. Therefore, a hot cracking test (Controlled Restraint Weldability (CRW) test) is proposed in the present study to analyze the susceptibility to hot cracking for base metal 316L(N) and its filler metal 19-15H Thermanit grade. This test is designed to initiate a hot crack in thermal steady state, and then to stop the crack once the local thermomechanical conditions are met. The initiation and stop of the crack depend on external mechanical preload. The material constitutive equations chosen for the material is a visco-plastic model with isotropic and kinematic hardening. The Gleeble thermomechanical tests have been performed at high temperature in order to identify material parameters. The increase of the grain size in the thermally affected zone was modeled and integrated into constitutive equations. The temperature range of melting and solidification of 316L(N) were determine by using the Differential Thermal Analysis (DTA). The analysis of the solidification microstructures were also carried out in order to better understand the phenomenon of hot cracking. Some CRW tests were then simulated by finite element method using the Cast3M and Abaqus software in order to valid the hot cracking criterion and to determine a thermomechanical criterion of hot cracking for 316L(N).

Les aciers inoxydables sont de plus en plus utilisés comme renfort du béton dans lesconstructions marines et côtières, afin de prévenir la corrosion induite par les ions chloruresqui pénètrent dans le béton poreux. L’ajout de molybdène dans les aciers inox contribue àaugmenter leur résistance à la corrosion par piqure lorsqu’ils sont utilisés dans desenvironnements acides et neutres. Cependant, le rôle du Mo sur la corrosion par piqûre desaciers en milieu alcalin chloruré reste à ce jour flou et peu étudié. Par conséquence, lacompréhension de l’action du Mo dans la résistance à la corrosion en milieu alcalin est doncd'une importance majeure. Cela permettra l'optimisation de la composition finale des alliagesinoxydables en vue des applications potentiels comme renfort dans le béton. Ainsi, cette thèsevise à étudier l'effet de l'addition du Mo sur les propriétés de corrosion par piqûre des aciersinoxydables austénitiques, ferritiques et surtout lean duplex en milieu alcalin. Finalement, lerôle du Mo sur les aciers inoxydables a été discuté en termes de leur résistance à la corrosionlocalisée, cinétique de repassivation et propriétés de passivation dans plusieurs milieuxagressifs, mais surtout dans une solution chlorurée synthétique qui simule les environnementsporeux du béton (solution de pH10 avec des ions carbonates et chlorures). / The use of stainless steels (SS) as concrete reinforcement is becoming increasinglypopular in coastal and marine constructions in order to prevent corrosion induced by chlorideions penetrating into the concrete. However, the influence of Mo addition on pitting corrosionresistance of these steels is not fully understood in alkaline chloride conditions although thiselement is widely associated to an increasing corrosion resistance in acidic and neutralenvironments. Therefore, understanding Mo mechanism on corrosion resistance in alkalineconditions is hence of major importance for the setting of optimized alloy composition. ThisPhD work aims to study the effect of Mo addition on pitting corrosion properties of austenitic,ferritic and mainly lean duplex stainless steels in alkaline media, which simulates the concreteenvironment. As far as the role of Mo is concerned, it will be discussed in terms of, pittingcorrosion resistance, repassivation kinetics, and passivation properties from acidic to alkalineconditions.

L’acier austénitique inoxydable 316L(N) et l’alliage 800 sont des candidats potentiels pour des éléments de structures des réacteurs nucléaires de génération IV. Les durées de vie envisagées peuvent atteindre 60 années sous chargement de fluage. Il est donc nécessaire de caractériser et de prendre en compte les mécanismes d’endommagement de fluage afin de proposer des prédictions de durées de vie. Le modèle de Riedel est basé sur la germination continue de cavités (loi de Dyson) et la croissance de cavités par diffusion des lacunes le long des joints de grains. Les durées de vie en fluage sont prédites par la combinaison des modèles de striction (court terme) et de Riedel (long terme), en accord avec les données expérimentales. Aucun paramètre ajusté n’a été utilisé dans le modèle de Riedel. Cependant, le préfacteur de la loi de Dyson devait être mesuré expérimentalement.Les cavités se forment aux interfaces entre particules de phase secondaire intergranulaires et matrice austénitique. Grâce à des calculs par éléments finis cristallins (logiciel Cast3M), les concentrations de contraintes aux interfaces matrice-précipité ont été calculées en considérant les hétérogénéités microstructurales. Les résultats des calculs nous permettent de proposer une formule multiplicative visant à calculer la distribution des contraintes normales d’interface, en prenant en compte toutes les hétérogénéités microstructurales. En appliquant un critère en contrainte et un critère énergétique de rupture, le préfacteur de la loi de Dyson prédit est du même ordre de grandeur que celui mesuré expérimentalement. Notre travail conduit à proposer un fondement théorique de la loi de Dyson. / Austenitic stainless steel 316L (N) and alloy 800 are potential candidates for structural components of Generation IV nuclear reactors. Their in-service lifetime may be extended up to 60 years under creep condition. It is thus necessary to characterize the dominant damage mechanisms during creep in order to propose long term lifetime predictions. The Riedel model is based on continuous cavity nucleation (the Dyson law) and cavity growth by vacancy diffusion along grain boundaries. The creep lifetimes are predicted by the combination of a necking (short-term) and the Riedel (long-term) models, agree well with numerous experimental data. No adjusted parameter was used as applying in the Riedel model. However, the Dyson law prefactor is evaluated experimentally. Cavities are produced at the interfaces of intergranular second phase particles and austenitic matrix. Using crystal viscoplasticity finite element computations (Cast3M software), the stress fields along the particle-matrix interfaces are calculated by considering the main microstructure heterogeneities. The Finite element calculation results allow us to propose a multiplication formula to compute the distribution of interface normal stresses, accounting for all microstructural heterogeneities. Applying an interface fracture stress criterion and a simplified energy balance equation, the predicted Dyson law prefactor is close to measured values. Our work provides a theoretical explanation of the phenomenological law of Dyson.

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Submitted by OTACILIO DONISETE FRANZINI null (otaciliodf@hotmail.com) on 2016-12-21T11:37:28Z No. of bitstreams: 1 APLICAÇÃO DE LASER PULSADO Nd YAG NA SOLDAGEM DO AÇO SUPER DUPLEX UNS S32750.pdf: 3133785 bytes, checksum: 7f73ce4a1615cca31edb63d392f368f2 (MD5) / Approved for entry into archive by Felipe Augusto Arakaki (arakaki@reitoria.unesp.br) on 2016-12-22T12:59:13Z (GMT) No. of bitstreams: 1 franzini_od_me_ilha.pdf: 3133785 bytes, checksum: 7f73ce4a1615cca31edb63d392f368f2 (MD5) / Made available in DSpace on 2016-12-22T12:59:13Z (GMT). No. of bitstreams: 1 franzini_od_me_ilha.pdf: 3133785 bytes, checksum: 7f73ce4a1615cca31edb63d392f368f2 (MD5) Previous issue date: 2016-12-13 / Os aços inoxidáveis Duplex e Super Duplex, 50% austenita e 50% ferrita, combinam as características mais desejáveis dos aços ferríticos e austeníticos, possuem excelente resistência mecânica e à corrosão para uma ampla variedade de meios, com expressiva resistência à corrosão em água do mar e outros ambientes contendo cloreto, devido a seu elevado nível de cromo, molibdênio, e nitrogênio. Quando soldado a região do metal de solda desses aços perdem suas características de resistência mecânica e à corrosão devido ao desbalanceamento das fases ferrita e austenita. No presente trabalho foi analisado a influência do processo de soldagem autógena a laser Pulsado Nd:YAG nas características mecânicas e microestruturais da junta soldada, variando a taxa de sobreposição dos pulsos de 40 a 90% em chapas de aço inoxidável Super Duplex UNS S32750 com 1,5 mm de espessura. Utilizou-se uma fonte laser pulsada Nd.YAG, United Winner 150A, com potência máxima de 150 W. A energia do pulso de soldagem foi fixada em 10J, potência de pico de 2 kW, largura temporal de 5 ms e frequência variando entre 1,5 e 9,0 Hz. Como gás de proteção utilizou-se argônio puro com vazão de 10 l/min. A caracterização microestrutural foi realizada através de microscopia ótica e microscopia eletrônica de varredura. Os resultados mostraram que o aumento da taxa de sobreposição da junta de 40% até 90% aumenta a resistência mecânica e a dureza do metal de solda. Em relação à microestrutura do metal de solda observou-se uma ferritização da mesma com pequena fração volumétrica de austenita nas regiões de contorno de grão. Não foi observada a presença de fases frágeis no metal de solda. / Duplex Stainless steels and Super Duplex 50% austenite and 50% ferrite, combine the most desirable traits of ferritic and austenitic steels possess excellent mechanical strength and corrosion resistance to a wide variety of ways, with substantial corrosion resistance in seawater and other environments containing chloride, due to its high level of chromium, molybdenum, and nitrogen. When welded to the weld metal region of these steels lose their mechanical strength features and corrosion due to the imbalance of the ferrite and austenite phases. In this paper we analyzed the influence of the welding process autogenous laser Pulsed Nd: YAG laser on the mechanical and microstructural features of the welded joint, by varying the overlap rate of pulses from 40 to 90% in stainless steel plates Super Duplex UNS S32750 with 1.5 mm thick. We used a pulsed laser source Nd.YAG, United Winner 150A, with maximum power of 150 W. The power of the welding pulse was set at 10 J, peak power of 2 kW, temporal width of 5 ms and frequency ranging from 1.5 and 9.0 Hz. As shielding gas used is pure argon with a flow rate of 10 l / min. Microstructural characterization was performed by optical microscopy and scanning electron microscopy. The results showed that increasing the overlap rate of 40% to 90% joint strength increases and the hardness of the weld metal. Regarding the welding ferritização observed a metal microstructure thereof with small volume fraction of the austenite grain boundary regions. It was observed the presence of brittle phases in the weld metal.

Orientador: Vicente Afonso Ventrella / Resumo: Os aços inoxidáveis Duplex e Super Duplex, 50% austenita e 50% ferrita, combinam as características mais desejáveis dos aços ferríticos e austeníticos, possuem excelente resistência mecânica e à corrosão para uma ampla variedade de meios, com expressiva resistência à corrosão em água do mar e outros ambientes contendo cloreto, devido a seu elevado nível de cromo, molibdênio, e nitrogênio. Quando soldado a região do metal de solda desses aços perdem suas características de resistência mecânica e à corrosão devido ao desbalanceamento das fases ferrita e austenita. No presente trabalho foi analisado a influência do processo de soldagem autógena a laser Pulsado Nd:YAG nas características mecânicas e microestruturais da junta soldada, variando a taxa de sobreposição dos pulsos de 40 a 90% em chapas de aço inoxidável Super Duplex UNS S32750 com 1,5 mm de espessura. Utilizou-se uma fonte laser pulsada Nd.YAG, United Winner 150A, com potência máxima de 150 W. A energia do pulso de soldagem foi fixada em 10J, potência de pico de 2 kW, largura temporal de 5 ms e frequência variando entre 1,5 e 9,0 Hz. Como gás de proteção utilizou-se argônio puro com vazão de 10 l/min. A caracterização microestrutural foi realizada através de microscopia ótica e microscopia eletrônica de varredura. Os resultados mostraram que o aumento da taxa de sobreposição da junta de 40% até 90% aumenta a resistência mecânica e a dureza do metal de solda. Em relação à microestrutura do metal de solda observou-se u... (Resumo completo, clicar acesso eletrônico abaixo) / Mestre