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L'utilisation de l'acier inoxydable duplex (DSS) pour des applications structurales est considérée comme l'un des progrès les plus notables et qui a le plus grand impact sur le secteur de la construction. Ceci est grâce à ses propriétés mécaniques élevées couplées avec des propriétés fonctionnelles intéressantes telles que la résistance à la corrosion, ou encore la faible conductivité thermique par rapport aux aciers au carbone. En raison de sa microstructure et l'interaction complexe entre les phases, DSS a un fort potentiel pour le développement des propriétés uniques. Une meilleure compréhension est nécessaire pour obtenir des propriétés exceptionnelles et fournir la possibilité de concevoir un DSS sur-mesure et architecturé pour des applications spécifiques. Dans ce travail, nous avons proposé une approche différente de celle utilisée jusqu'à présent pour comprendre le comportement du DSS. La stratégie adoptée dans ce travail était une stratégie dite top-down dans laquelle au moins deux métaux ayant un comportement et des propriétés bien connues sont mécaniquement assemblés par déformation plastique sévère (SPD). Cette stratégie proposée a pour objectifs: i) améliorer les propriétés par raffinement de microstructure jusqu’à une échelle sub-micrométrique ii) l'élaboration d'un matériau modèle permettant de comprendre le comportement DSS obtenu par les méthodes métallurgique conventionnelles. Le premier objectif de ce travail était, par conséquent, la mise en œuvre d'une méthodologie de fabrication en utilisant la technique SPD par co-tréfilage. Cette technique permettra l'obtention d'une microstructure ultrafine des composites 316L / 430LNb. L'un des défis rencontrés au cours de notre étude était l'inter-diffusion significative lors de traitement thermique susceptible de limiter un raffinement supplémentaire de la microstructure en question. Une étude d'optimisation a été effectuée pour tenir compte du rôle de cette inter-diffusion pour un couple 316L / 430LNb. Ainsi, des micro-composites multi-échelles ont été obtenus. Dans ce travail, nous avons montré la limitation de ce processus en termes de raffinement de microstructure. Une rationalisation de ces limites a été donnée par une étude thermocinétiques sur les micro-composites et matériaux brut initialement utilisés. Parallèlement à l'évaluation de la microstructure, le comportement mécanique de ces nouveaux micro-composites a été examiné. Afin de fournir une explication plus approfondie sur le comportement plastique de nos composites, des essais de traction in situ par rayonnement X synchrotron à haute énergie ont été effectués. / The use of duplex stainless steel (DSS) grades for structural applications is considered as one of the most significant advances impacting the construction sector. This is because of their high mechanical properties coupled with interesting functional properties such as corrosion resistance or even the low thermal conductivity compared to carbon steels. Due to their complex microstructure and interaction between the phases, DSS have a significant potential for unique properties. A better understanding is needed to give the possibility to obtain break through properties and to provide the possibility to design tailor-made, architectured DSS for specific applications. In this work we proposed a different approach from that used until now to understand the behavior of DSS. The strategy adopted in this work was a top-down strategy in which at least two bulk metals with well known behavior and properties are mechanically alloyed by Severe Plastic Deformation (SPD). This proposed strategy served two main objectives: i) enhancing the properties by microstructure refining down to sub-micron scale ii) elaborating a material model for understanding the DSS behavior obtained by the conventional metallurgical methods. The first objective of this work was, therefore, the implementation of a methodology of manufacturing using SPD technique by co-drawing. This technique will allow obtaining an ultra-fine microstructure of 316L/430LNb composites. One of the challenges met during our study was the significant inter-diffusion during heat-treatment step necessary during processing preventing by consequence further refining. An optimization investigation was carried out to account the role of this inter-diffusion for 316L/430LNb couple. Multi-scale micro-composites have been then obtained. In this work, we showed the limitation of this process in terms of microstructure refining. A rationalization of these limits was given by studying the thermo-kinetics of both micro-composites and bulk materials. In parallel with the microstructural evaluation, the mechanical behavior of these new micr-composites was examined. In order to provide a more in-depth explanation of the plastic behavior of our composites, in situ tensile test using high energy X-ray synchrotron have been performed.

O desenvolvimento de componentes com geometrias complexas e funcionalidade superficial representa um grande desafio científico atual. O processo Metal Injection Molding (MIM) tem representado, nos últimos anos, uma grande alternativa para a produção de aços com estas características e elevada produtividade. Existe uma crescente demanda referente ao estudo e utilização de aços inoxidáveis MIM e a melhora de suas propriedades mecânicas e metalúrgicas superficiais. Com a aplicação de engenharia de superfície é possível obter aumento da microdureza superficial, da resistência ao desgaste, da vida em fadiga e da resistência à corrosão. Uma das características emblemáticas dos aços MIM é seu maior volume de porosidade, quando comparado aos aços obtidos pelos processos convencionais. Destaca-se que o volume de porosidade pode ter efeito negativo em relação à resistência mecânica e à corrosão nestes aços. O volume de porosidade também colabora para que componentes produzidos por este processo sejam fortemente influenciados, por efeitos de erosão de bordas, e dificuldade de difusão uniforme, em regiões com furação, inibindo a homogeneização das camadas de compostos e difusão. Neste trabalho objetivou-se desenvolver as ligas em aços inoxidáveis a partir de pós metálicos aglutinados com polímeros e pesquisar as propriedades metalúrgicas e mecânicas superficiais, obtidas a partir da aplicação de tratamento termoquímico de Oxinitrocarbonetação (QPQ), nos aços inoxidáveis MIM AISI 316L e 17-4 PH e o efeito do acabamento intermediário jateado na resistência a corrosão, que representa modificação deste processo. Os ciclos de difusão utilizados foram referendados a partir de tempos de 30, 60 e 120 minutos utilizando-se temperatura de nitrocarbonetação 570ºC e de oxidação 380ºC. As avaliações das propriedades das amostras oxinitrocarbonetadas foram realizadas em ensaios de microscopia óptica, microscopia eletrônica de varredura, microdureza Vickers, polarização potenciodinâmica anódica, difração de raios - X (para determinação das fases na camada de compostos) e difração de raios - X (para determinação de tensões residuais). Os resultados obtidos demonstraram efetivo aumento da microdureza superficial, formação de camada de compostos monofásica, melhora da resistência a corrosão e tensões residuais compressivas na superfície dos aços AISI 316 L e 17 4 PH MIM. / The development of components with complex geometries and surface functionality is a current scientific challenge. There is an increasing demand related to the study and use of stainless steel Metal Injection Molding (MIM) and the improvement of their surface mechanical and metallurgical properties. With the application surface engineering it is possible to obtain increased surface hardness, wear resistance, fatigue life and corrosion resistance. One of the iconic features of MIM steels is its largest volume of porosity, when compared to conventional steels. It is noteworthy that the volume of porosity may have a negative effect on the mechanical and corrosion resistance. The volume porosity also contributes to components produced by this process are strongly influenced by edge effects of erosion and uniform diffusion regions difficulty with drilling, inhibiting the mixing of compounds and diffusion layers. Other research has shown that high volumes of porosity may be associated with the presence of corrosive pitting progressively accentuate the deterioration of these materials. In this work we were researched surface metallurgical and mechanical properties of the thermochemical treatment application Oxinitrocarburizing- QPQ in stainless steel AISI 316L ME and 17 4 PH and the effect of the intermediate blasted finish on the corrosion resistance. Assessments of properties of the samples Oxinitrocarburizing by QPQ process were carried out in optical microscopy tests, scanning electron microscopy, Vickers hardness, anodic potentiodynamic polarization, diffraction X - ray (determination of the phases in the compound layer), and - ray diffraction x (residual stresses).The results demonstrated effective increase of the surface hardness, forming a single phase compound layer improves the corrosion resistance and compressive residual stresses on the surface of steels AISI 316 L and 17 4 PH MIM.

No description available.

La demande croissante en énergie nécessite l'exploration de pétrole et de gaz dans des conditions plus difficiles. Ces systèmes de production exigent l'utilisation d'équipements forgés faits de nuances d'acier de plus haute résistance, comme les aciers inoxydables austéno-ferritiques (duplex). Ces composants tendent à présenter une perte de ductilité et de performance mécanique générale provoquée par l'hydrogène produit par p. ex. des systèmes de protection cathodique et des processus de corrosion. Les composants en aciers inoxydables duplex présentent une longue histoire d’endommagement par l'hydrogène à basse température provenant de diverses sources. Bien qui ce type de endommagement soit assez récurrent, diverses informations connexes restent à élucider, en raison de l'interaction complexe de l'hydrogène avec la microstructure et le caractère localisé de la production et du transport de l'hydrogène dans le matériau.Le présent travail vise à améliorer la compréhension physique de l'interaction entre l'hydrogène et la microstructure ainsi que les effets de différentes procédures de chargement d'hydrogène sur les propriétés mécaniques des composants forgés en acier inoxydable super duplex UNS S32750.Le développement d'une telle compréhension implique l'évaluation des effets de l'hydrogène sur les propriétés mécaniques du matériau au moyen d'essais de traction dans différents environnements riches en hydrogène. Basé sur des résultats d'essais de traction à vitesse de déformation faible, une relation quantitative entre la fragilisation provoquée par l'hydrogène gazeux et cathodique est proposée, et les effets possibles de la fragilisation par l’hydrogène provoquée par dislocations sont discutés.Des descriptions quantitatives et qualitatives du transport de l'hydrogène, incluant l'analyse des effets des différentes microstructures et voies de diffusion, et de sa position dans le réseau et dans la microstructure (ségrégation de l'hydrogène aux pièges) sont proposées. Ces descriptions sont obtenues en considérant les résultats de différentes techniques expérimentales: essais de perméation, spectroscopie de désorption thermique, spectroscopie de masse d'ions secondaires à temps de vol et diffusion de neutrons. / The increasing demand for energy requires the exploration of oil and gas at deeper water locations and on more severe conditions. These production systems have demanded the use of forged equipments made of higher strength steel grades, such as austenitic-ferritic (duplex) stainless steels. These components are more prone to exhibit loss of ductility and general mechanical performance caused by hydrogen generated e.g. by cathodic protection. Duplex stainless stainless steels components present a vast history of hydrogen damage at low temperatures, due to hydrogen derived from various sources. Even being this kind of damage fairly recurring, various related information remains to be elucidated, due to the complex interaction of hydrogen with the microstructure and localized character of hydrogen generation and transportation in the material. The present work aims to improve the physical understanding of the interaction between hydrogen and the microstructure as well as the effects of different hydrogen charging procedures on the mechanical properties of forged components made of the super duplex stainless steel grade UNS S32750.The development of such understanding involves the evaluation of the effects of hydrogen on the mechanical properties of the material through tensile tests in different hydrogen-rich environments. Based on results of slow-strain rate tensile tests, a quantitative relationship between embrittlement caused by gas hydrogen and cathodic charging is proposed, and possible effects of dislocation-assisted hydrogen transportation and embrittlement are discussed. Quantitative and qualitative descriptions of the hydrogen transportation, including analysis of the effects of different microstructures and diffusion paths, and of its position in the lattice and in the microstructure (hydrogen segregation to traps) are proposed. These descriptions are achieved considering results of different testing techniques: permeation tests, thermal desorption spectroscopy, time-of-flight secondary ion mass spectroscopy and neutron scattering.

O desenvolvimento de componentes com geometrias complexas e funcionalidade superficial representa um grande desafio científico atual. O processo Metal Injection Molding (MIM) tem representado, nos últimos anos, uma grande alternativa para a produção de aços com estas características e elevada produtividade. Existe uma crescente demanda referente ao estudo e utilização de aços inoxidáveis MIM e a melhora de suas propriedades mecânicas e metalúrgicas superficiais. Com a aplicação de engenharia de superfície é possível obter aumento da microdureza superficial, da resistência ao desgaste, da vida em fadiga e da resistência à corrosão. Uma das características emblemáticas dos aços MIM é seu maior volume de porosidade, quando comparado aos aços obtidos pelos processos convencionais. Destaca-se que o volume de porosidade pode ter efeito negativo em relação à resistência mecânica e à corrosão nestes aços. O volume de porosidade também colabora para que componentes produzidos por este processo sejam fortemente influenciados, por efeitos de erosão de bordas, e dificuldade de difusão uniforme, em regiões com furação, inibindo a homogeneização das camadas de compostos e difusão. Neste trabalho objetivou-se desenvolver as ligas em aços inoxidáveis a partir de pós metálicos aglutinados com polímeros e pesquisar as propriedades metalúrgicas e mecânicas superficiais, obtidas a partir da aplicação de tratamento termoquímico de Oxinitrocarbonetação (QPQ), nos aços inoxidáveis MIM AISI 316L e 17-4 PH e o efeito do acabamento intermediário jateado na resistência a corrosão, que representa modificação deste processo. Os ciclos de difusão utilizados foram referendados a partir de tempos de 30, 60 e 120 minutos utilizando-se temperatura de nitrocarbonetação 570ºC e de oxidação 380ºC. As avaliações das propriedades das amostras oxinitrocarbonetadas foram realizadas em ensaios de microscopia óptica, microscopia eletrônica de varredura, microdureza Vickers, polarização potenciodinâmica anódica, difração de raios - X (para determinação das fases na camada de compostos) e difração de raios - X (para determinação de tensões residuais). Os resultados obtidos demonstraram efetivo aumento da microdureza superficial, formação de camada de compostos monofásica, melhora da resistência a corrosão e tensões residuais compressivas na superfície dos aços AISI 316 L e 17 4 PH MIM. / The development of components with complex geometries and surface functionality is a current scientific challenge. There is an increasing demand related to the study and use of stainless steel Metal Injection Molding (MIM) and the improvement of their surface mechanical and metallurgical properties. With the application surface engineering it is possible to obtain increased surface hardness, wear resistance, fatigue life and corrosion resistance. One of the iconic features of MIM steels is its largest volume of porosity, when compared to conventional steels. It is noteworthy that the volume of porosity may have a negative effect on the mechanical and corrosion resistance. The volume porosity also contributes to components produced by this process are strongly influenced by edge effects of erosion and uniform diffusion regions difficulty with drilling, inhibiting the mixing of compounds and diffusion layers. Other research has shown that high volumes of porosity may be associated with the presence of corrosive pitting progressively accentuate the deterioration of these materials. In this work we were researched surface metallurgical and mechanical properties of the thermochemical treatment application Oxinitrocarburizing- QPQ in stainless steel AISI 316L ME and 17 4 PH and the effect of the intermediate blasted finish on the corrosion resistance. Assessments of properties of the samples Oxinitrocarburizing by QPQ process were carried out in optical microscopy tests, scanning electron microscopy, Vickers hardness, anodic potentiodynamic polarization, diffraction X - ray (determination of the phases in the compound layer), and - ray diffraction x (residual stresses).The results demonstrated effective increase of the surface hardness, forming a single phase compound layer improves the corrosion resistance and compressive residual stresses on the surface of steels AISI 316 L and 17 4 PH MIM.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / Com o objetivo de investigar a influência que o molibdênio exerce nas propriedades das camadas passivas das armaduras de aços austeníticos, barras redondas dos aços UNS S30400 e 31600 foram submetidas à ação de soluções que simulam as que são encontradas nos poros de concreto. Para caracterizar o efeito do molibdênio na resistência daqueles aços à corrosão por pites, foram conduzidos ensaios de circuito aberto, polarização anódica, espectroscopia de impedância eletroquímica, análise de Mott-Schottky, tração em baixa taxa de deformação e análise das superfícies por microscopias óptica e eletrônica de varredura. Os resultados obtidos demonstram que, de uma forma geral, o aço UNS S30400 (sem molibdênio) apresentou maior resistência à corrosão localizada que o UNS S31600 (2% de Mo) nas soluções alcalinas cloretadas naturalmente aeradas, comportamento este inverso ao que se observa nos mesmos materiais quando submetidos a soluções cloretadas neutras ou ácidas. / Aiming to investigate the influence that molybdenum has on properties of passive layers of austenitic steels, round bars of UNS S30400 and S31600 steels were subjected to the action of solutions that simulate those found in the concrete pores. To characterize the effect of molybdenum on the resistance of those steels to pitting corrosion, tests were conducted in open circuit, anodic polarization curves, electrochemical impedance spectroscopy, Mott- Schottky analysis, slow strain rate test and surface analysis by optical microscopy and scanning electron microscopy. The obtained results showed that, grosso modo, the stainless steel UNS S30400 (Mo free) has higher corrosion resistance than UNS S31600 (2% Mo) in naturally aerated alkaline solutions containing chloride ions, which characterizes an inverse behaviour in relation to the same materiais in neutral or acidic solutions.

Lors de l’élaboration des aciers plats inoxydables, un recuit haute température de courte durée (60 s environ), sous atmosphère oxydante (O2/H2O/CO2/N2) est mis en place après laminage à froid. Ce recuit entraîne la formation d’une couche d’oxyde de faible épaisseur qui est éliminée par un décapage. Ces étapes de recuit et décapage peuvent entraîner une perte de qualité du produit fini, se traduisant par une perte de brillance. L’acier bistabilisé Ti, Nb (AISI 441) est sensible à la dégradation de surface. L’objectif de la thèse est d’identifier les phénomènes à l’origine de la perte de brillance. Les travaux menés consistent à étudier les couches d’oxyde et le comportement de l’acier lors du décapage. Une morphologie originale de l’interface interne avec la présence de protrusions métalliques a été observée. L’étude des protrusions par la microscopie électronique à balayage couplée à une sonde ionique focalisée : MEB-FEG/FIB, a permis de proposer un mécanisme décrivant leur formation. Ce mécanisme s’appuie sur la précipitation de la silice qui semble également être un élément clé pour comprendre la dégradation de surface. Un lien entre perte de brillance et teneur en chrome dans le substrat a été établi. La déchromisation de l’acier liée au recuit est susceptible d’être facilitée par les protrusions. / During the industrial processing line of stainless steel flat products, a short annealing (60 s) at high temperature in a gas furnace-oxidizing atmosphere (O2/H2O/CO2/N2) takes place after cold rolling. This annealing leads to the formation of a thin oxide film which is then removed by a pickling step at the end of the process. The annealing and pickling stages may cause a loss of gloss, resulting in a loss of product quality. The steel bistabilizied Ti, Nb (AISI 441) is sensitive to this surface degradation. The aim of this thesis is to identify the phenomena leading to the loss of gloss. Our work consists in studying the oxide layers and the behavior of steel during pickling. A peculiar morphology of the internal interface with the presence of metallic protrusions was observed. The protrusions investigation using a scanning electron microscopy coupled with a focused ion beam: MEB-FEG/FIB, allowed us to propose a mechanism of their formation. This mechanism is based on the precipitation of silica which also appears to be a key point to understand the surface degradation. A link between the loss of gloss and the chromium content in the substrate was established and the chromium depletion related to the annealing is likely to be facilitated by protrusions.

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