As research continues for the habitation of the Lunar and Martian surfaces, the need for materials for construction of structural parts, mechanical components, and tools remains as a major milestone. The use of in-situ resource utilization (ISRU) techniques is critical due to the financial, physical, and logistical burdens of sending supplies beyond low-Earth orbit. The Bosch process is currently in development as a life support system at the National Aeronautics and Space Administration’s (NASA) Marshall Space Flight Center (MSFC) to regenerate oxygen (O2) from metabolic carbon dioxide (CO2) with the byproduct of elemental carbon (C). The Bosch process presents a possible way of regenerating O2 without the disposal of hydrogen (H2) like the Sabatier. Ionic liquids (ILs) are also studied at MSFC as a means to harvest metallic elements from regolith oxides and meteorites. IL technology provides an energy efficient method of extracting critical manufacturing materials, such as iron (Fe) that could be used for ferrous alloy production. This dissertation seeks to explore the use of Bosch C and IL-Fe for ferrous alloy production through a series of studies. These studies included individually using Bosch C with commercial elements to cast low carbon steel and gray cast iron, investigating as-produced IL-Fe in a laser-based powder bed fusion (PBF-LB) printer to determine IL-Fe metallurgical characteristics, using the IL-Fe composition to design a ductile iron (DI) alloy of similar performance to a commercially available DI alloy, and lastly, refining this DI alloy to produce a DI alloy more representative of an alloy producible from IL-Fe and Bosch byproduct C in a Martian environment. The results presented here suggest that with advances in production rate and control of IL-Fe oxidation, and by providing a sufficient energy grid to operate equipment, a range of high quality DI materials could be manufactured with IL and Bosch process ISRU feedstocks.

Pt-aluminide (PtAl) coatings form an integral part of thermal barrier coating (TBC) systems that are applied on Ni-based superalloy components operating in the hot sections of gas turbine engines. These coatings serve as a bond coat between the superalloy substrate and the ceramic yttrium stabilized zirconia (YSZ) coating in the TBC system and provide oxidation resistance to the superalloy component during service at high temperatures. The PtAl coatings are formed by the diffusion aluminizing process and form an integral part of the superalloy substrate. The microstructure of the PtAl coatings is heavily graded in composition as well as phase constitution. The matrix phase of the coating is constituted of the B2-NiAl phase. Pt, in the coating, is present as a separate PtAl2 phase as well as in solid solution in B2-NiAl. The oxidation resistance of the PtAl bond coat is derived from the B2-NiAl phase. At high temperatures, Al from the B2-NiAl phase forms a regenerative layer of alumina on the coating surface which, thereby, lowers the overall oxidation rate of the superalloy substrate. The presence of Pt is beneficial in improving the adherence of the alumina scale to the surface and thereby enhancing the oxidation resistance of the coating. However, despite its excellent oxidation resistance, the B2-NiAl being an intermetallic phase, renders the PtAl coating brittle and imparts it with a high brittle-to-ductile-transition-temperature (BDTT). The PtAl coating, therefore, remains prone to cracking during service. The penetration of these cracks into the substrate is known to degrade the strain tolerance of the components. Evaluation of the mechanical behavior of these coatings, therefore, becomes important from the point of views of scientific understanding as well as application of these coatings in gas turbine engine components. Studies on the mechanical behavior of coatings have been mostly carried on coated bulk superalloy specimens. However, since the coating is brittle and the superalloy substrate more ductile when compared to the coating, the results obtained from these studies may not be representative of the coating. Therefore, it is imperative that the mechanical behavior of the coating in stand-alone condition, i.e. the free-standing coating specimen without any substrate attached to it, be evaluated for ascertaining the true mechanical response of the coating. Study of stand-alone bond coats involves complex specimen preparation techniques and challenging testing procedures. Therefore, reports on the evaluation of mechanical properties of stand-alone coatings are limited in open literature. Further, no systematic effort has so far been made to examine important aspects such as the effect of temperature and strain rate on the tensile behavior of these coatings. The deformation mechanisms associated with these bond coats have also not been reported in the literature. In light of the above, the present research study aims at evaluating the tensile behavior of free-standing PtAl coatings by the micro-tensile testing technique. The micro-tensile testing method was chosen for property evaluation because of its inherent ability to generate uniform strain in the specimen while testing, which makes the results easy to interpret. Further, since the technique offers the feasibility to test the entire graded PtAl coating in-situ, the results remain representative of the coating. Using the above testing technique, the tensile behavior of the PtAl coating has been evaluated at various temperatures and strain rates. The effect of strain rate on the BDTT of the coating has been ascertained. Further, the effect of Pt content on the tensile behavior of these coatings has also been evaluated. Attempts have been made to identify the mechanisms associated with tensile deformation and fracture in these coatings. The thesis is divided into nine chapters. Chapter 1 presents a brief introduction on the operating environment in gas turbine engines and the materials that are used in the hot sections of gas turbine engines. The degradation mechanisms taking place in the superalloy in gas turbine environments and the need for application of coatings has also been highlighted. The basic architecture of a typical thermal barrier coating (TBC) system applied on gas turbine engine components has been presented. The constituents of the TBC system, i.e. the ceramic YSZ coating, MCrAlY overlay as well as diffusion aluminide bond coats and, the various techniques adopted for the deposition of these coatings have been described in brief. Chapter 2 presents an overview of the literature relevant to this study. This chapter is divided into four sub-chapters. The formation of diffusion aluminide coatings on Ni-based superalloys has been described in the first sub-chapter. Emphasis has been laid on pack cementation process for the formation of the coatings. The fundamentals of pack aluminizing process, including the thermodynamic and kinetic aspects, have been mentioned in brief. The microstructural aspects of high activity and low activity plain aluminide and Pt-aluminide coatings have also been illustrated. The techniques applied for the mechanical testing of bond coats have been discussed in the second sub-chapter. The macro-scale testing techniques have been mentioned in brief. The small scale testing methods such as indentation, bend tests and micro-tensile testing have also been discussed in the context of evaluation of mechanical properties of bond coats. Since the matrix in the aluminide bond coats is constituted of the B2-NiAl phase, a description of the crystal structure and deformation characteristics of this phase including the flow behavior, ductility and fracture behavior has been mentioned in the third sub-chapter. In the fourth sub-chapter, reported literature on the tensile behavior and brittle-to-ductile-transition-temperature (BDTT) of diffusion aluminide bond coats has been discussed. In Chapter 3, details on experiments carried out for the formation of various coatings used in the present study and, their microstructural characterization, are provided. The method for extraction of stand-alone coating specimens and their testing is discussed. The microstructure and composition of the various coatings used in the present study are discussed in detail in Chapter 4. Unlike in case of bulk tensile testing, for which standards on the design of specimens exist, there are no standards available for the design of micro-tensile specimens. Therefore, as part of the present research work, a finite element method (FEM)-based study was carried out for ascertaining the dimensions of the specimens. The simulation studies predicted that failure of the specimens within the gage length can be ensured only when certain correlations between the dimensional parameters are satisfied. Further, the predictions from the simulation study were validated experimentally by carrying out actual testing of specimens of various dimensions. Details on the above mentioned aspects of specimen design are provided in Chapter 5. The PtAl coatings undergo brittle fracture at lower temperatures while ductile fracture occurs at higher temperatures. Further, the coatings exhibit a scatter in the yielding behavior at temperatures in the vicinity of BDTT. Therefore, the BDTT, determined as the temperature at which yielding is first observed in the stress-strain curves, may not be representative of the PtAl coatings. In Chapter 6, a method for the precise determination of BDTT of aluminide bond coats, based on the variation in the plastic strain to fracture with temperature, has been demonstrated. The BDTT determined by the above method correlated well with the variation in fracture surface features of the coating and was found representative of these coatings. In Chapter 7, the effect of temperature and strain rate on the tensile properties of a PtAl bond coat has been evaluated. The temperature and strain rate was varied between room temperature (RT)-1100°C and 10-5 s-1-10-1 s-1, respectively. The effect of strain rate on the BDTT of the PtAl bond coat has been examined. Further, the variation in fracture surface features and mechanism of fracture with temperature and strain rate are illustrated. The micro-mechanisms of deformation and fracture in the coating at different temperature regimes have also been discussed. The coating exhibited brittle-to-ductile transition with increase in temperature at all strain rates. The BDTT was strain rate sensitive and increased significantly at higher strain rates. Above BDTT, YS and UTS of the coating decreased and its ductility increased with increase in the test temperature at all strain rates. Brittle behavior occurring in the coating at temperatures below the BDTT has been attributed to the lack of operative slip systems in the B2-NiAl phase of the coating. The onset of ductility in the coating in the vicinity of BDTT has been ascribed to generation of additional slip systems caused by climb of dislocations onto high index planes. The coating exhibited two distinct mechanisms for plastic deformation as the temperature was increased from BDTT to 1100°C. For temperatures in the range BDTT to about 100°C above it, deformation was controlled by dislocations overcoming the Peierls-Nabarro barrier. Above this temperature range, non-conservative motion of jogs by jog dragging mechanism controlled the deformation. The transition temperature for change of deformation mechanism also increased with increase in strain rate. For all strain rates, fracture in the coating at test temperatures below the BDTT, occurred by initiation of cracks in the intermediate single phase B2-NiAl layer of the coating and subsequent inside-out propagation of the cracks across the coating thickness. Ductile fracture in the coating above the BDTT was associated with micro-void formation throughout the coating. The effect of Pt content on the tensile behavior of PtAl coating, evaluated at various temperatures ranging from room temperature (RT) to 1100°C and at a nominal strain rate of 10-3 s-1, is presented in Chapter 8. Irrespective of Pt content in the coating, the variation in tensile behavior of the coating with temperature remained similar. At temperatures below BDTT, the coatings exhibited linear stress-strain response (brittle behavior) while yielding (ductile behavior) was observed at temperatures above BDTT. At any given temperature, the elastic modulus decreased while the strength increased with increase in Pt content in the coating. On the other hand, the ductility of the coating remained unaffected with Pt content. The BDTT of the coating also increased with increase in Pt content in the coating. Addition of Pt did not affect the fracture mechanism in the coating. Fracture at temperatures below BDTT was caused by nucleation of cracks at the intermediate layer and their subsequent inside-out propagation. At high temperatures, fracture occurred in a ductile manner comprising void formation, void linkage and subsequent joining with cracks. The deformation sub-structure of the coating did not get affected with Pt incorporation. Short straight dislocations were observed at temperatures below BDTT, while, curved dislocations marked by jog formation were observed at temperatures above BDTT. The factors controlling fracture stress and strength in the PtAl coatings at various temperatures have also been assessed. The overall summary of the present research study and recommendations for future studies are presented in the last chapter, i.e. Chapter 9.

L'objectif de cette thèse est le développement d'un modèle numérique fiable et précis pour prédire l'évolution de l'endommagement jusqu'à la rupture dans une structure soumise à des grandes déformations plastiques. Ces développements contribuent à l'enrichissement d'une librairie EF parallèle appelée CIMLib. Pour mieux traiter l'incompressibilité des déformations plastiques, une approximation éléments finis mixtes vitesse-pression avec une discrétisation stabilisée P1+/P1 est utilisée pour la résolution des équations mécaniques. L'intégration d'une loi de comportement élastoplastique endommageable dans cette approximation a été largement abordée. L'évolution de l'endommagement obéit à un modèle de Lemaitre enrichi, où les phénomènes dissipatifs sont couplés et qui prend en compte la nature des sollicitations et l'effet de refermeture des fissures en compression. L'approximation éléments finis avec un comportement adoucissant est fortement dépendante de la discrétisation spatiale dans la phase post-critique. Pour pallier à ce problème, nous avons adopté une méthode de régularisation non locale du gradient implicite. Nous avons choisi un exemple où la localisation est très marquée en bande de cisaillement pour montrer la fiabilité de notre modèle à prédire l'évolution de l'endommagement jusqu'à la rupture de la structure. Un autre axe principal de cette thèse est l'adaptation anisotrope de maillage au phénomène d'endommagement. Une stratégie d'adaptation anisotrope de maillage pilotée par un estimateur de l'erreur d'interpolation a été utilisée afin d'améliorer la précision pour l'endommagement avec un temps de calcul minimal. L'apport de l'adaptation de maillage permet de garantir une meilleure prédiction de l'évolution de l'endommagement jusqu'à la rupture. Son utilisation nous a permis de retrouver numériquement des modes de rupture observés expérimentalement. Dans le cadre de grands cas industriels irréductibles, par exemple à cause de la croissance de l'endommagement, le temps de calcul peut devenir pénalisant. Nous nous sommes donc intéressé à l'accélération de la résolution des grands systèmes linéaires issus d'une approximation éléments finis par les méthodes multigrilles. Un préconditionneur multigrille géométrique a été mis en place. Les premières validations ont montré que ce préconditionneur permet d'avoir une complexité quasi-linéaire en fonction des degrés de liberté. Le modèle numérique ainsi développé peut servir à la simulation des procédés de pose de points d'assemblage des tôles par déformations plastiques, à l'étude de leur tenue mécanique en les soumettant à des sollicitations variées, et à la simulation des procédés de mises en forme à froid des corps solides (emboutissage, forgeage, hydroformage, semi découpe ou découpe des tôles ...)

The current thesis focuses on the deformation behaviour and strain distribution in the microstructure of ductile iron during tensile loading. Utilizing Digital Image Correlation (DIC) and in-situ tensile test under optical microscope, a method was developed to measure high resolution strain in microstructural constitutes. In this method, a pit etching procedure was applied to generate a random speckle pattern for DIC measurement. The method was validated by benchmarking the measured properties with the material’s standard properties. Using DIC, strain maps in the microstructure of the ductile iron were measured, which showed a high level of heterogeneity even during elastic deformation. The early micro-cracks were initiated around graphite particles, where the highest amount of local strain was detected. Local strain at the onset of the micro-cracks were measured. It was observed that the micro-cracks were initiated above a threshold strain level, but with a large variation in the overall strain. A continuum Finite Element (FE) model containing a physical length scale was developed to predict strain on the microstructure of ductile iron. The materials parameters for this model were calculated by optimization, utilizing Ramberg-Osgood equation. For benchmarking, the predicted strain maps were compared to the strain maps measured by DIC, both qualitatively and quantitatively. The DIC and simulation strain maps conformed to a large extent resulting in the validation of the model in micro-scale level. Furthermore, the results obtained from the in-situ tensile test were compared to a FE-model which compromised cohesive elements to enable cracking. The stress-strain curve prediction of the FE simulation showed a good agreement with the stress-strain curve that was measured from the experiment. The cohesive model was able to accurately capture the main trends of microscale deformation such as localized elastic and plastic deformation and micro-crack initiation and propagation.

Cette thèse a pour objectif de caractériser les circulations de fluides en contexte d’effondrement d’un prisme d’accrétion crustal. Le Metamorphic Core Complex (MCC) de Naxos comprend un système de détachement/décollement caractérisé par mylonites, ultramylonites, cataclasites et failles normales dont les relations géométriques témoignent du litage rhéologique de la croûte continentale. La chimie des inclusions fluides déterminée par l’analyse microthermométrique, la spectroscopie RAMAN, l’ablation laser couplée à l’analyse spectroscopique (LA-ICP-MS), le « crush-leach », et les signatures isotopiques C et H des inclusions fluides permettent d’identifier trois grands types de fluides (1) des fluides salés riche en métaux, ii) des fluides aquo-carboniques en équilibre avec les encaissants métamorphiques, et iii) des fluides aqueux, probablement d’origine météorique. Ces données indiquent que la croûte est subdivisée en deux réservoirs séparés par la transition fragile-ductile. Les fluides météoriques circulent en association avec la déformation fragile de la croûte supérieure alors que les fluides salés et les fluides aquo-carboniques circulent en relation avec la déformation ductile. La géométrie de ces réservoirs évolue lors de la formation du MCC, conjointement avec l’exhumation et le refroidissement des roches métamorphiques. Le passage des roches du réservoir ductile au réservoir fragile est associée à un changement depuis un gradient géothermique élevé (60-100°C/km) vers un gradient géothermique plus faible (35-60°C/km). La transition fragile-ductile correspond ainsi à la fois à une limite rhéologique corrélée à une limite thermique et une limite de perméabilité. / The aim of this thesis is to characterize fluid circulations in the context of the collapse of a crustal accretionary belt. The Naxos Metamorphic Core Complex comprises a detachment/decollement system characterized by mylonites, ultramylonites, cataclasites and normal faults with structural relationships reflecting the rheological layering at the crustal scale. Fluid inclusion chemistry is determined by microthermometry, Raman spectroscopy; laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), crush-leach and stable isotopes (C and H) analyses. These data characterize three different types of fluids: (1) high salinity fluids with a high metal content and high Th, (2) aqueous-carbonic fluids in equilibrium with the wall rocks and (3) aqueous probably surface-derived fluids. These data indicate that the crust is subdivided into two crustal reservoirs separated by the brittle/ductile transition. Surface-derived aqueous fluids circulate in association with the brittle deformation within the upper crust whereas aqueous-carbonic and high salinity fluids circulate in relation with ductile deformation. The characteristics of the trapped fluids indicate that as rocks have passed through the ductile/brittle transition they undergo a drastic change in geothermal gradient from 60 to 100°C/km within a lithostatic pressure regime to 35-60°C/km within a hydrostatic pressure regime. This implies that the fluid circulations are closely related to the rheological layering within the crust and its evolution during crustal extension. The ductile/brittle transition corresponds to a rheological boundary correlated to a thermal boundary and impermeable cap.

Le travail présenté a pour objectif la prédiction numérique de la résistance résiduellede grandes structures vis-à-vis d’évènements accidentels, tels que ceux rencontrés p.ex. dans le cas de la collision de navires ou d’impact d’oiseaux en aéronautique. Cesévènements peuvent dans certain cas conduire à la rupture, qui est ici considéréeductile. La difficulté de cette étude, consiste à reproduire dans une méthodologieunifiée basée sur la méthode des éléments finis les étapes successives menant àla ruine ultime de la structure. Ces étapes sont : l’endommagement ductile, lalocalisation de la déformation et la propagation de la fissure. Un élément essentiel pour la conception d’un modèle de fissuration ductile prédictif est le traitement numérique de la phase transitoire critique de localisation de la déformation induite par l’endommagement dans une bande de matière étroite.A cet effet, trois points de vue différents en termes de champ de déplacement àtravers la bande de localisation sont proposés. Ces trois approches se distinguentpar le type de discontinuité considérée : forte, faible et régularisée (expression nonlinéaire). Un cadre variationnel consistant est élaboré pour chacune des trois approches.Ainsi la cinématique enrichie est incorporée dans la formulation de l’élément fini enutilisant la méthode des éléments finis enrichis (X-FEM). Puis, la performance deces méthodes est évaluée vis-à-vis de leur capacité à modéliser la phase transitoireentre endommagement diffus (mécanique des milieux continus) et propagation defissure (mécanique de la rupture). Ces travaux sont réalisés dans le contexte dematériaux ductiles. D’après les analyses réalisées, la combinaison du modèle de ’discontinuité fortecohésive’ et la X-FEM semble être la plus prometteuse des trois approches étudiéespour allier physique et numérique. Le développement d’un tel modèle est discutéen détail. Enfin, deux critères supplémentaires sont définis : le premier pour lepassage de l’endommagement diffus au modèle de bande cohésive et un deuxièmepour le passage du modèle de bande cohésive à la rupture. / The present work aims at numerically predicting the current residual strengthof large engineering structures made of ductile metals regarding accidental events,e.g. ships collision or bird strike in aviation, which may potentially lead to failure.With this aim in view, the challenge consists in reproducing within a unified finiteelement (FE)-based methodology the successive steps of micro-voiding-induceddamage, strain localization and crack propagation, if any.A key ingredient for a predictive ductile fracture model is the proper numericaltreatment of the critical transition phase of damage-induced strain localizationinside a narrow band. For this purpose, three different viewpoints in terms ofdisplacement field across the localization band are proposed involving a strong,weak and (non-linearly) regularized discontinuity, respectively.A consistent variational framework is elaborated for each of the three methods,whereby the enriched kinematics is embedded into the FE formulation using theeXtended FEM. Then, within a comparative procedure, the performance of thesemethods is assessed regarding their ability of modeling the transition phase betweendiffuse damage (continuum mechanics framework) and crack propagation (fracturemechanics framework), always in the context of ductile materials.According to the aforementioned analyses, the combination of the strong discontinuitycohesive model and the X-FEM appears to be the most promising of thethree studied approaches to bring together physics and numerics. The developmentof such a model is discussed in detail. Finally, two supplementary criteria aredefined: the first one for the passage from diffuse damage to the cohesive bandmodel and the second one for the passage from the cohesive band model to thecrack.

A aplicação do novo conceito de tratamento térmico, chamado de têmpera e partição (Q&P), desenvolvido para a obtenção de aços da terceira geração da classe AHSS (Advanced high strengh steel ou aços avançados de alta resistência), mostra-se uma alternativa para o processamento de ferros fundidos nodulares com alta resistência mecânica. No processo Q&P, o carbono presente na martensita supersaturada, formada na etapa de têmpera, é utilizado para estabilizar a austenita não transformada durante a etapa de partição, mantendo-a estável na temperatura ambiente. Essa rota de tratamento térmico consiste em realizar uma têmpera no material (após uma etapa prévia de austenitização) numa faixa de temperatura entre o Ms e Mf (temperatura de início e fim da transformação martensítica, respectivamente), seguido de um reaquecimento e manutenção a uma temperatura acima do Ms (etapa isotérmica de partição) com o objetivo de que o carbono migre da martensita supersaturada para a austenita remanescente promovendo sua estabilização. Essa partição do carbono só é possível caso a precipitação da cementita seja suprimida, e isso é conseguido com a presença de elementos de liga, como o Si e/ou Al. Neste trabalho foi feito um estudo sobre as características microestruturais e mecânicas de um ferro fundido nodular (3,47%C; 2,47%Si; 0,2%Mn) submetido ao tratamento térmico de têmpera e partição, o qual foi denominado neste trabalho como, Q&PDI (Quenched and Partitioned Ductile Iron ou Ferro Fundido Nodular Temperado e Particionado). Para isso foi realizada uma austenitização plena nas amostras, a 880°C, por duas horas, seguida de uma têmpera em óleo pré-aquecido nas temperaturas de 140 e 170°C. A etapa de partição foi feita nas temperaturas de 300, 375 e 450°C, com intervalos de tempo variando de 5 a 120 minutos. A caracterização microestrutural foi realizada através de microscopia ótica, microscopia eletrônica de varredura e EBSD. A técnica de difração de raios-X foi empregada para quantificar a fração volumétrica e o teor de carbono na austenita retida. Ensaios de dilatometria, difração de raios-X \"in situ\" e nanoindentação foram empregados para auxiliar na análise das transformações de fases que ocorreram na etapa de partição, como a transformação bainítica e a precipitação de carbonetos de transição nas placas de martensita. A caracterização mecânica foi feita através de ensaios de tração, impacto, dureza, nanoindentação, tenacidade à fratura e resistência à fadiga. Ensaios de compressão auxiliaram na análise da transformação martensítica induzida por deformação. Os resultados obtidos mostraram que é possível obter ferros fundidos nodulares com alta resistência mecânica (limite de resistência >1450 MPa), com consideráveis ductilidade (de até 9%) e energia absorvida sob impacto (de até 81 J), bem como tenacidades à fratura de 55 MPa.m1/2 e limites de fadiga de 550 MPa. Este comportamento é proporcionado por uma microestrutura singular, constituída por uma dispersão homogênea de placas de martensita numa matriz de ausferrita bastante refinada, com consideráveis frações volumétricas de austenita retida (max. 23%). / Quenching and partitioning (Q & P), a new heat treatment concept developed to obtain third generation AHSS (Advanced High Strength Steel), is an alternative for processing of nodular cast irons in order to obtain high mechanical strength. In the Q & P process, the carbon present in the supersaturated martensite formed in the quenching step diffuses towards the untransformed austenite during the partition step, keeping it stable at room temperature. This heat treatment route consists of quenching the material (after a previous step of austenitization) in a temperature range between Ms and Mf (beginning and end temperature of the martensitic transformation, respectively), followed by reheating and maintenance at a temperature above the Ms (isothermal stage of partition) allowing the carbon to migrate from the supersaturated martensite to the remaining austenite, promoting its stabilization. This partition of carbon is only possible if precipitation of cementite is suppressed; this is achieved adding alloying elements such as Si and/or Al. In this work a study was made on the microstructural and mechanical characteristics of a ductile iron (3.47%C; 2.47%Si; 0.2%Mn), submitted to a Q&P heat treatment, in this work named Q & PDI (Quenched and Partitioned Ductile Iron). A full sample austenitization was carried out at 880 ° C for two hours, followed by a pre-heated oil quanching at temperatures of 140 and 170 ° C. The partitioning step was at temperatures of 300, 375 and 450Â ° C, with time intervals ranging from 5 to 120 minutes. Microstructural characterization was performed through optical microscopy, scanning electron microscopy and EBSD. The X-ray diffraction technique was used to quantify the volumetric fraction and the carbon content in the retained austenite. Dilatometry, X-ray diffraction \"in situ\" and nanoindentation were also used to aid in the analysis of the phase transformations that occurred in the partitioning stage, such as the bainitic transformation and the precipitation of transition carbides in the martensite plates. Mechanical characterization was performed through tensile, impact, hardness, nanoindentation, fracture toughness and fatigue strength tests. Compression tests aided in the analysis of the deformation induced martensitic transformation. The results showed that it is possible to obtain nodular cast irons with high mechanical strength (resistance limit> 1450 MPa), with considerable ductility (up to 9%) and energy absorbed under impact (up to 81 J), as well as fracture toughness of 55 MPa.m -1 / 2 and fatigue limits of 550 Mpa. This behavior is provided by a unique microstructure, consisting of a homogeneous dispersion of martensite plates in a very refined ausferrite matrix, with considerable volumetric fractions of retained austenite (max. 23%).

Investigou-se o efeito do tamanho de grão austenítico na cinética e na morfologia do produto da reação bainítica de um ferro fundido nodular austemperado (FFNA). Foram estudados 3 tamanhos de grão austeníticos, a saber: GG (grão grosseiro), GM (grao mediano); e GR (grao refinado). A condição GR foi obtida pela austenitização rápida de microestruturas martensíticas. A condição GG foi obtida por tratamento de austenitização em duas etapas, de modo a, respectivamente, provocar o crescimento de grão e manter o teor de carbono igual aos das demais condições. Na segunda etapa do tratamento da condição GG ocorreu precipitação de grafita secundária, que acelerou significativamente a taxa de reação bainítica, possibilitando estudar o efeito da.variação na quantidade de interfaces austenita/grafita e austenita/ austenita sobre a cinética e a morfologia da reação bainítica. O refino do grão austenítico acelerou a cinética de reação, aumentou a proporção de ferrita alotriomorfa de contorno de grão, refinou a microestrutura bainítica (ferrita + austenita retida) e melhorou em 14% o limite de escoamento dos FFNA. Finalmente, a predominância de ferrira alotriomorfa na condição mais fina indica que a formação de interfaces incoerentes (mecanismo difusional ao inves de reação displaciva) durante a austenitização rápida da martensita (aquecimento de 100°C/ s). / The effect of austenite grain size on the kinetics and the morphology of the bainitic reaction in an austempered ductile iron (ADI) has been investigated, Three austenite grain sizes were produced: GG (coarse grain), GH (medium grain) and GR (fine grain), The GR condition was obtained by the rapid austenitization of martensitic microstructures The secondary graphite precipitation observed in GG condition strongly accelerated the rate of bainite formation and made possible the study of the effect of austenite/graphite interface on the kinetics of this reaction, The austenite grain refinement also accelerated the bainite precipitation, increased the proportion of grain boundary alotriomorphs ferrite, refined the bainitic microstructure and improved by 14% the yield stress of ADI, The predominance of grain boundary alotriomorphs in GR was associated to the structure of austenite/austenite interface formed during the rapid austenitization of the studied ductile iron at heating rates of 100oC/s. It is suggested that the dominant mechanism of austenitization in this condition is a thermally activated one (not a displacive transformation). The different morphologies of the austenite decomposition used the Duhê\'s morphological system.

Em projetos de oleodutos e gasodutos utilizam-se aços de alta resistência e baixa liga (ARBL), como o aço API 5L X80. Na soldagem multipasse destas tubulações, a zona afetada pelo calor (ZAC) do passe de raiz é submetida a um novo ciclo térmico pelos passes de soldagem subsequentes. Isto resulta em alterações nos valores das propriedades físicas. Nos aços ARBL, a ZAC de grãos grosseiros reaquecida intercriticamente (IC-ZACGG) pode se tornar uma zona frágil localizada, isto é, uma zona com maior dureza. Consequentemente, falhas estruturais podem ocorrer, ocasionando paradas não desejadas no transporte de fluidos. O objetivo deste trabalho é desenvolver uma metodologia baseada no modelo de fontes de calor distribuídas de Mhyr e Gröng, para avaliar o fluxo de calor na soldagem considerando as propriedades físicas dependentes da temperatura. Estender a aplicação desta ferramenta em soldagens multipasses para identificar sub-regiões da ZAC de um passe anterior sendo afetada pela ZAC de passes subsequentes. As isotermas simuladas foram validadas através de medições realizadas em macrografias de juntas soldadas. Os ciclos térmicos simulados foram validados através das temperaturas máximas atingidas e pelos tempos de resfriamento de 800 a 500 ºC (?t8-5) dos ciclos térmicos experimentais. Ao aplicar a metodologia proposta, foi possível delimitar com acurácia as regiões reaquecidas da ZAC e analisar os efeitos dos passes subsequentes em cada uma das sub-regiões da ZAC do passe de raiz. A IC-ZACGG na região do passe de raiz foi localizada, mas não se comportou como zona frágil devido à boa soldabilidade do aço API 5L X80 comprovada pelos ensaios de dureza e de tenacidade ao impacto Charpy-V. / In pipelines projects, the high strength low alloy (HSLA) steels are used, such as the API 5L X80 steel. During the multipass welding of these pipes, the heat affected zone (HAZ) of the root pass is subjected to a new thermal cycle by the subsequent welding passes. This results in changes in the values of the physical properties. In the HSLA steels, the intercritical reheated coarse-grained heat-affected zone (IR-CGHAZ) can become a local brittle zone, that is, a region with greater hardness. Consequently, structural failures could happen, causing undesired shutdowns in fluid transportation. The objective of this work is to develop a methodology based on the distributed heat sources model of Mhyr and Gröng, to evaluate the heat flux in the welding considering the temperature-dependent physical properties. Extend the application of this tool in multipass welds to identify HAZ subregions of a previous pass being affected by the HAZ of subsequent passes. The simulated isotherms were validated through measurements made on macrographs of welded joints. The simulated thermal cycles were validated through the maximum temperatures reached and the cooling times from 800 °C to 500 ºC (?t8-5) of the experimental thermal cycles. By applying the proposed methodology, it was possible to accurately delimit reheated HAZ regions and analyze the effects of subsequent passes in each of the root pass HAZ subregions. The IRCGHAZ in the root pass region was localized, but it did not behave as a brittle zone due to the good weldability of the API 5L X80 steel as proven by the hardness and Charpy-V impact tests.

Para o correto dimensionamento da maioria dos componentes estruturais é necessário informações sobre a resposta do material quando submetido à fadiga de alto e baixo ciclo, bem como conhecer as propriedades monotônicas (não-cíclicas) e cíclicas dos materiais. Na literatura são encontradas amplas divulgações de dados sobre diversos materiais de engenharia (Ex. SAE J1099 Technical Report on Fatigue Properties). Porém, quando se trata de ferro fundido nodular estas informações são limitadas, sendo assim, visa-se neste trabalho caracterizar as propriedades monotônicas e cíclicas destes materiais em complemento aos trabalhos já publicados na literatura e propor métodos para a estimativa destas propriedades a partir da dureza. Faz-se necessário a proposição de métodos estimativos das propriedades mecânicas destes materiais baseados na dureza devido às suas grandes variações que são inerentes ao processo de fundição. Em um mesmo componente podem existir diferentes classes de ferro fundido, que apesar de possuir a mesma composição química, podem apresentar variações nas propriedades mecânicas devido à formação de diferentes estruturas metalúrgicas que são sensíveis às taxas de resfriamento do material que variam de acordo com as características geométricas da peça que está sendo fundida, principalmente a variação da espessura. Neste estudo a determinação das relações entre as propriedades monotônicas e cíclicas dos ferros fundidos nodulares foram obtidas a partir do tratamento dos dados publicados na literatura levando-se em consideração o índice de qualidade. Foi proposto um modelo contínuo com relação à dureza para a estimativa das propriedades monotônicas, do coeficiente de resistência cíclico e do expoente de encruamento cíclico e para a estimativa das propriedades cíclicas que experimentalmente demonstraram não ter correlação com a dureza foi proposto uma forma discreta, que consistiu na recomendação de valores típicos definidas por faixas de dureza. / For the correct design of the most part of structural components is necessary to have information about the material response under both high cycle and low cycle fatigue, as well as the knowledge of monotonic and cyclic materials properties. In literature a major publication of several engineering material data can be found (e.g, SAE J1099 - Technical Report on Fatigue Properties), but regarding to ductile iron this information is quite limited. Therefore, this work aims to characterize the monotonic and cyclic properties of this material in complementing to the available data in the literature and also make a proposition of methods to estimate this properties from hardness. The mechanical properties estimation model from hardness is relevant to take into account the inherent variations of casting process, which for the same chemical composition can be found different grades in a same part. This fact occurs due to the formation of different metallurgical structures that is influenced by cooling ratio which changes accordingly to geometrical characteristic of the part, especially the thickness variation. In this study the determination of the relation between monotonic and cyclic properties from hardness has been determined from literature data processing taking into account the Quality Index. For monotonic properties, the cyclic strength coefficient and the cyclic strain hardening exponent estimation has been proposed a continuous method based on hardness and for the cyclic properties that experimentally showed to remain independent of hardness has been recommended one set of properties for specific hardness ranges.