The high temperature microstructure of the solid phases within the electric arc furnace (EAF) slag has a large effect on the process features such as foamability of the slag, chromium recovery, consumption of the ferroalloys and the wear rate of the refractory. The knowledge of the microstructural and compositional evolution of the slag phases during the EAF process stages is necessary for a good slag praxis. In supplement 1, an investigation of the typical characteristics of EAF slags in the production of the AISI 304L stainless steel was carried out. In addition, compositional and microstructural evolution of the slag during the different EAF process stages was also investigated. Computational thermodynamics was also used as a tool to predict the equilibrium phases in the top slag as well as the amount of these phases at the process temperatures. Furthermore, the influence of different parameters (MgO wt%, Cr2O3 wt%, temperature and the top slag basicity) on the amount of the spinel phase in the slag was studied. In supplement 2, a novel study to characterize the electric arc furnace (EAF) slags in the production of duplex stainless steel at the process temperatures was performed. The investigation was focused on determining the microstructural and compositional evolution of the EAF slag during and at the end of the refining period. Slag samples were collected from 14 heats of AISI 304L steel (2 slag samples per heat) and 7 heats of duplex steel (3 slags sample per heat). Simultaneously with each slag sampling, the temperature of the slag was measured. The selected slag samples were studied both using SEM-EDS and LOM. In some cases (supplement 2), X-ray diffraction (XRD) analyses were also performed on fine-powdered samples to confirm the existence of the observed phases. It was observed that at the process temperature and at all process stages, the stainless steel EAF slag consists mainly of liquid oxides, magnesiochromite spinel particles and metallic droplets. Under normal operation and at the final stages of the EAF, 304L steelmaking slag contains 2-6 wt% magnesiochromite spinel crystals. It was also found that, within the compositional range of the slag samples, the only critical parameter affecting the amount of solid spinel particles in the slag is the chromium oxide content. Petrographical investigation of the EAF duplex stainless steelmaking showed that, before FeSi-addition, the slag samples contain large amounts of undissolved particles and the apparent viscosity of the slag is higher, relative to the subsequent stages. In this stage, the slag also includes solid stoichiometric calcium chromite. It was also found that, after FeSi-injection into the EAF and during the refining period, the composition and the basicity of the slag in the EAF duplex steelmaking and EAF stainless steelmaking are fairly similar. This indicates that, during the refining period, the basic condition for the utilization of an EAF foaming-slag praxis, in both austenitic and duplex stainless steel cases, is the same. Depending on the slag basicity, the slag may contain perovskite and/or dicalcium silicate too. More specifically, the duplex stainless steel slag samples with a higher basicity than 1.55 found to contain perovskite crystals. / QC 20110413

Nos últimos anos, devido ao elevado preço do níquel, uma nova série de aços inoxidáveis austeníticos com um menor teor de níquel foi criada. A essa nova série foi dado o nome de série 200. Dentre os aços dessa classe, o AISI 201 tem sido utilizado em aplicações onde a elevada resistência à corrosão não é tão necessária. Neste trabalho de Mestrado investigou-se a formação e a reversão da martensita induzida por deformação em um aço inoxidável austenítico AISI 201 laminado a frio em 20, 40 e 60% de redução em espessura. Das chapas laminadas foram retiradas amostras que foram recozidas em várias temperaturas (200-800oC) por 1 hora. Amostras do material laminado em 60% de redução em espessura também foram recozidas por várias temperaturas (200-800oC) e por vários tempos (5-180min). Com isso, avaliou-se a evolução microestrutural do material durante a laminação frio e durante o recozimento por meio de medidas de microdureza Vickers, microscopias óptica, eletrônica de varredura e eletrônica de transmissão, difração de elétrons retroespalhados, difração de raios X e medidas de magnetização. Além disso, foram realizados cálculos termodinâmicos para a previsão da formação de fases nesse material. Constatou-se que o material de partida não era completamente austenítico, possuindo uma pequena fração de ferrita ? residual em sua microestrutura. Com relação às medidas de magnetização, observou-se que a fração de fase ferromagnética (martensita) aumenta com o aumento da deformação, aumentando a magnetização de saturação (Ms) do material. Para pequenas deformações (20% de redução em espessura) houve a ocorrência de um pico no valor de campo coercivo do material (Hc). Com o aumento da deformação (40 e 60%) os valores de Hc diminuíram. Com relação à reversão da martensita induzida por deformação durante os recozimentos, observou-se que ela ocorre na faixa de temperatura de 500-700oC para o material laminado em 60% de redução em espessura. O comportamento do material nesse estudo corrobora o que tem sido reportado na literatura para os aços da série 300. Entretanto, pouco tem sido publicado com relação às propriedades magnéticas do aço inoxidável austenítico AISI 201, principalmente com relação ao campo coercivo. Neste trabalho também foram realizadas medidas de magnetização durante o recozimento das amostras (condição in situ). Os parâmetros obtidos desses experimentos in situ foram comparados com aqueles obtidos para as amostras recozidas isotermicamente. / In the last years, since nickel price increased, another series of austenitic stainless steel with less amount of nickel has emerged: the series 200. The AISI 201 stainless steel has been used where intermediated corrosion resistance is needed. In this work, the formation of strain-induced martensite and its reversion in an AISI 201 austenitic stainless steel were studied. The material was characterized in terms of microstructure and then cold rolled up to 20, 40 and 60% of thickness reduction. For all degree of reduction, samples were annealed at several temperatures (200-800oC) for 1 hour. Additional samples taken from the 60% cold-rolled material were also annealed at several temperatures (200-800oC) for several times (5-180minutes). The microstructural evolution during cold rolling and annealing was evaluated using microhardness Vikers testing, light optical microscopy, scanning electron microscopy, transmission electron microscopy, electron backscatter diffraction, X-Ray diffraction and magnetization measurements. Phase predictions were also performed using software Thermo-calc©. It was observed that the as-received material was not fully austenitic. It has a small fraction of ?-ferrite within its matrix. The amount of ferromagnetic phase (martensite) increases with increasing deformation. For small deformation (20%), there is a peak in the coercive field of the material (Hc). As deformation increases, Hc values decrease. It was also observed that the martensite reversion takes place at 500-700oC. The behavior of the material is in accordance with what has been reported in the literature for the 300 series. However, only few works have been reported concerning AISI 201 stainless steel and its magnetic properties. In this work, magnetic measurements were also carried out during annealing (in situ condition). The obtained parameters from the in situ magnetic measurements were compared to those ones obtained from the isothermally annealed samples.

Dans le cadre du développement des Réacteurs à Haute Température (RHT), un des systèmes retenus pour la quatrième génération de centrale nucléaire, l’utilisation d’un cycle indirect est envisagée. Ce type d’installation, utilisant de l’hélium comme caloporteur, nécessite un échangeur intermédiaire de chaleur (Intermediate Heat eXchanger, IHX) le plus compact possible entre les circuits primaire et secondaire. Les contraintes imposées par la conception ainsi que les conditions sévères d’utilisation pour ce type d’installation (température maximale 850°C à 950°C, durée de vie 20000 h) ont orienté le choix des matériaux constitutifs de l’IHX vers deux alliages base nickel en solution solide : l’Inconel 617 et le Haynes 230. Le premier matériau a été largement étudié dans les années 1980 lors du projet allemand sur les RHT car possédant de bonnes propriétés mécaniques et en corrosion à haute température mais sa forte teneur en cobalt potentiellement activable est à considérer. Le Haynes 230, plus récent, possède des caractéristiques similaires à celles de l’alliage 617, le cobalt ayant été remplacé par du tungstène. L’objectif de cette thèse est d’étudier le comportement mécanique à haute température de ces deux alliages en relation avec les évolutions de leur microstructure. Les observations microstructurales à l’état de réception révèlent la présence de carbures primaires (M6C), la majorité étant répartie de manière homogène. Des carbures secondaires M23C6, peu nombreux, sont visibles à l’état de réception pour les deux matériaux. Les vieillissements thermiques imposés aux alliages à 850°C permettent une précipitation importante de carbures M23C6 sur les lignes de glissement et aux joints de grains, la taille de ces carbures augmentant et leur nombre réduisant avec la durée de traitement. A 950°C, l’évolution microstructurale conduit à une précipitation intragranulaire beaucoup plus limitée et à une évolution intergranulaire plus importante. Pour les deux matériaux, les observations de la microstructure et les résultats de dureté montrent que la majorité des évolutions microstructurales se produisent avant 1000 h aux deux températures étudiées. Les caractéristiques mécaniques de ces alliages ont été testées en traction, en fluage et en fatigue et fatigue relaxation. En particulier, les propriétés à 850°C et 950°C ont été étudiées pour différentes charges (en fluage), vitesses de déformation (en traction) et durées de relaxation (fatigue relaxation). Les effets d’un traitement initial ont également été étudiés, tels que l’effet d’un vieillissement thermique testé en fluage et traction et l’effet d’une prédéformation sur le fluage. Il ressort de cette étude que différents mécanismes de déformation sont mis en jeu successivement ou en parallèle au cours des essais réalisés. Ainsi, l’importance de la précipitation des carbures sur les propriétés mécaniques de l’Inconel 617 et du Haynes 230 a pu être démontrée, malgré leur statut d’alliages en solution solide. Par ailleurs, un même mécanisme thermiquement activé opère sur une très large gamme de vitesses de déformation, correspondant aux essais de traction, fluage et relaxation. Cette mise en relation entre microstructure et propriétés mécaniques permet de déterminer les avantages de chaque alliage ainsi que leurs limites d’utilisation dans le cadre de la fabrication d’un échangeur de chaleur de centrale nucléaire. / High Temperature Reactors (HTR), is one of the innovative nuclear reactor designed to be inherently safer than previous generation and to produce minimal waste. The most critical metallic component in that type of reactor is the Intermediate Heat eXchanger (IHX). The constraints imposed by the conception and the severe operational conditions (high temperature of 850°C to 950°C, lifetime of 20,000 h) have guided the IHX material selection toward two solid solution nickel base alloys, the Inconel 617 and the Haynes 230. Inconel 617 is the primary candidate alloy thanks to its good high temperature mechanical and corrosion properties and the large data base developed in previous programs. However, its high cobalt content has to be considered as an issue (nuclear activation). The more recent alloy Haynes 230, in which most of the cobalt has been replaced by tungsten, present characteristics similar to the 617 alloy. The objective of this thesis is to study the high temperature mechanical behaviour of both alloys in relation with their microstructural evolutions. The as received microstructural observations have revealed primary carbides (M6C). Most of this precipitates are evenly distributed in the materials. Few M23C6 secondary carbides are observed in both alloys in the as received state. Thermal ageing treatments at 850°C lead to an important M23C6 precipitation on slip lines and at grain boundaries. The size of this carbides increases and their number decreases with increasing ageing duration. The intragranular precipitation of secondary carbides at 950°C is more limited and the intergranular evolution more important than at 850°C. The microstructural observations and the hardness evolution of both alloys show that the main microstructural evolutions occur before 1,000 h at both studied temperatures. The mechanical properties of the Inconel 617 and the Haynes 230 have been studied using tensile, creep, fatigue and relaxation-fatigue tests. Particularly, the properties at 850°C and 950°C have been evaluated using several stress levels (creep), strain rates (tensile) and relaxation duration (fatigue). The effects of initial treatments have also been studied, i.e.ageing treatments effects on creep and tensile properties and cold-work effects on creep properties. At high temperature, the as received Inconel 617 does not show classical creep behaviour. This study shows the importance of the fast carbides precipitation on their mechanical properties, despite the fact that the Inconel 617 and the Haynes 230 are listed as solid solution alloys. Low cycle fatigue tests with and without holding time have been performed at 850°C under air and under vacuum on both alloys. The results showed that cyclic hardening, cyclic stability and life time are closely related to the duration of the holding time. Furthermore, a single thermally activated mechanism operates over a very wide range of strain rates, corresponding to tensile tests, creep and relaxation. The link between microstructure and mechanical behaviour presented in this thesis helps to determine the advantages as the operation limits of each alloy in order to manufacture a nuclear power plant heat exchanger

Submitted by Caroline Periotto (carol@ufscar.br) on 2016-09-26T15:05:24Z No. of bitstreams: 1 DissGTV.pdf: 1872903 bytes, checksum: 8df6b2f211cfc4236fc723147c24d9bf (MD5) / Approved for entry into archive by Marina Freitas (marinapf@ufscar.br) on 2016-09-26T20:50:51Z (GMT) No. of bitstreams: 1 DissGTV.pdf: 1872903 bytes, checksum: 8df6b2f211cfc4236fc723147c24d9bf (MD5) / Approved for entry into archive by Marina Freitas (marinapf@ufscar.br) on 2016-09-26T20:50:56Z (GMT) No. of bitstreams: 1 DissGTV.pdf: 1872903 bytes, checksum: 8df6b2f211cfc4236fc723147c24d9bf (MD5) / Made available in DSpace on 2016-09-26T20:51:03Z (GMT). No. of bitstreams: 1 DissGTV.pdf: 1872903 bytes, checksum: 8df6b2f211cfc4236fc723147c24d9bf (MD5) Previous issue date: 2015-07-03 / Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) / Due to the current growth in the fossil fuels consumption, there is a great concern about the increase in pollutant emissions. In order to reduce these emissions, research indicates that the decrease in vehicle weight can be one of the solutions to reduce these gas emissions. One possible way to reduce the car weight is the replacement of parts that uses high density metals by Magnesium alloys. The major problem with this replacement is the lack of ductility that this material has at room temperature, being necessary to heat the plates before the conformation. This heating process has a high production costs and it is unfeasible to use in the automotive industry today. In view of this problem, this work aims to study this lack of conformity to room temperature using a microstructure modification technique located in the regions of conformation. The technic used was Friction Stir Processing (FSP) at high speed. This processing is similar to Friction Stir Welding (FSW), but without joining materials. The FSP is just a localized microstructural modification. The analysis performed in this study after processing at 1, 7 and 10 m/min show that the microstructure and mechanical properties undergoes various changes at for every processing speed output different. The results showed that the material after processing improves the ductility at room temperature as grain size decreases. / Com o atual crescimento do consumo de combustíveis fosseis, existe uma grande preocupação com o aumento de emissões de gases poluente. Para redução dessas emissões, pesquisas apontam que a diminuição do peso de veículos pode ser uma das soluções para reduzir as emissões de gases poluentes pelo aumento da eficiência energética. Uma forma possível de diminuir o peso de automóveis é pela substituição de partes que utilizam metais com alta densidade por ligas de Magnésio. O grande problema desta substituição é a falta de dutilidade que este material possui a temperatura ambiente, sendo necessário aquecer as chapas antes da conformação. Atualmente este processo de aquecimento gera um alto custo de produção dificultando sua utilização na indústria automotiva. Tendo em vista este problema, o presente trabalho tem como objetivo entender esta dificuldade na conformação a temperatura ambiente e propor uma solução utilizando uma técnica de modificação microestrutural localizada nas regiões de conformação. Esta técnica é o Processamento por Fricção e Mistura (FSP – Friction Stir Processing) à altas velocidade. Este processamento é semelhante ao de Soldagem por Fricção e Mistura (FSW – Friction Stir Welding), mas sem a formação de uma região de união entre materiais. O FSP é apenas uma modificação microestrutural localizada. As análises realizadas neste estudo após o processamento à 1, 7 e 10m/min apontam que a microestrutura e as propriedades mecânicas sofrem variações diferentes a cada velocidade de processamento. Os resultados mostraram que o material obteve uma melhora na dutilidade à temperatura ambiente devido à diminuição do tamanho de grão.

Nos últimos anos, devido ao elevado preço do níquel, uma nova série de aços inoxidáveis austeníticos com um menor teor de níquel foi criada. A essa nova série foi dado o nome de série 200. Dentre os aços dessa classe, o AISI 201 tem sido utilizado em aplicações onde a elevada resistência à corrosão não é tão necessária. Neste trabalho de Mestrado investigou-se a formação e a reversão da martensita induzida por deformação em um aço inoxidável austenítico AISI 201 laminado a frio em 20, 40 e 60% de redução em espessura. Das chapas laminadas foram retiradas amostras que foram recozidas em várias temperaturas (200-800oC) por 1 hora. Amostras do material laminado em 60% de redução em espessura também foram recozidas por várias temperaturas (200-800oC) e por vários tempos (5-180min). Com isso, avaliou-se a evolução microestrutural do material durante a laminação frio e durante o recozimento por meio de medidas de microdureza Vickers, microscopias óptica, eletrônica de varredura e eletrônica de transmissão, difração de elétrons retroespalhados, difração de raios X e medidas de magnetização. Além disso, foram realizados cálculos termodinâmicos para a previsão da formação de fases nesse material. Constatou-se que o material de partida não era completamente austenítico, possuindo uma pequena fração de ferrita ? residual em sua microestrutura. Com relação às medidas de magnetização, observou-se que a fração de fase ferromagnética (martensita) aumenta com o aumento da deformação, aumentando a magnetização de saturação (Ms) do material. Para pequenas deformações (20% de redução em espessura) houve a ocorrência de um pico no valor de campo coercivo do material (Hc). Com o aumento da deformação (40 e 60%) os valores de Hc diminuíram. Com relação à reversão da martensita induzida por deformação durante os recozimentos, observou-se que ela ocorre na faixa de temperatura de 500-700oC para o material laminado em 60% de redução em espessura. O comportamento do material nesse estudo corrobora o que tem sido reportado na literatura para os aços da série 300. Entretanto, pouco tem sido publicado com relação às propriedades magnéticas do aço inoxidável austenítico AISI 201, principalmente com relação ao campo coercivo. Neste trabalho também foram realizadas medidas de magnetização durante o recozimento das amostras (condição in situ). Os parâmetros obtidos desses experimentos in situ foram comparados com aqueles obtidos para as amostras recozidas isotermicamente. / In the last years, since nickel price increased, another series of austenitic stainless steel with less amount of nickel has emerged: the series 200. The AISI 201 stainless steel has been used where intermediated corrosion resistance is needed. In this work, the formation of strain-induced martensite and its reversion in an AISI 201 austenitic stainless steel were studied. The material was characterized in terms of microstructure and then cold rolled up to 20, 40 and 60% of thickness reduction. For all degree of reduction, samples were annealed at several temperatures (200-800oC) for 1 hour. Additional samples taken from the 60% cold-rolled material were also annealed at several temperatures (200-800oC) for several times (5-180minutes). The microstructural evolution during cold rolling and annealing was evaluated using microhardness Vikers testing, light optical microscopy, scanning electron microscopy, transmission electron microscopy, electron backscatter diffraction, X-Ray diffraction and magnetization measurements. Phase predictions were also performed using software Thermo-calc©. It was observed that the as-received material was not fully austenitic. It has a small fraction of ?-ferrite within its matrix. The amount of ferromagnetic phase (martensite) increases with increasing deformation. For small deformation (20%), there is a peak in the coercive field of the material (Hc). As deformation increases, Hc values decrease. It was also observed that the martensite reversion takes place at 500-700oC. The behavior of the material is in accordance with what has been reported in the literature for the 300 series. However, only few works have been reported concerning AISI 201 stainless steel and its magnetic properties. In this work, magnetic measurements were also carried out during annealing (in situ condition). The obtained parameters from the in situ magnetic measurements were compared to those ones obtained from the isothermally annealed samples.

[pt] A presente tese tem como objetivo estudar a estabilidade microestrutural da superliga 625 a base de Ni pelas suas propriedades mecânicas e suas várias aplicações na indústria, em três condições distintas: maciça (placa forjada industrialmente), partículas de pó precursora da peça 3D e uma peça produzida por impressão a laser (Deposição Direta de Metais - DMD). Amostras destas condições foram submetidas a tratamentos de solubilização e envelhecimento isotérmico a 650 graus Celsius e 750 graus Celsius durante 10 horas e 100 horas, de modo a promover fenômeno de precipitação e, assim, correlacionar com as propriedades mecânicas do material. A caracterização microestrutural foi realizada por microscopia ótica (MO), microscopia eletrônica de varredura (MEV), microscopia eletrônica de transmissão (MET) no modo convencional utilizando contraste de difração, na modalidade analítica de transmissão/varredura (STEM), e em alta resolução (HRTEM). Espectroscopias de raios X por dispersão em energia (EDS) e de perdas de energia de elétrons (EELS) foram utilizadas para analisar a composição local da matriz e das fases presentes. Foram realizados ensaios de microdureza para avaliar o efeito dos tratamentos térmicos. A análise microestrutural da amostra maciça na condição como recebida apresentou grãos equiaxiais com fases NbTiC e M6C. Com o tratamento térmico de solubilização a 1100 graus Celsius por 40 minutos houve uma dissolução parcial dos carbetos. O envelhecimento a 650 graus Celsius por 10 horas resultou em carbetos de NbTiC e um aumento da dureza em 5 porcento em relação a amostra como solubilizada. Entretanto no tratamento de envelhecimento a 100 horas ocorreu precipitação homogênea da fase gama aumentando a dureza do material em 45 porcento, se comparada à mesma como solubilizada. A liga maciça envelhecida a 750 graus Celsius por 10 horas apresentou os carbetos NbTiC e M23C6 nos contornos de grãos e dispersos na matriz. Já a liga maciça envelhecida por 100 horas a esta mesma temperatura, apresentou a fase δ dispersa na matriz. A análise microestrutural do pó precursor mostrou ser policristalino constituído predominantemente de grãos colunares da matriz austenítica. Análises das amostras produzidas por DMD como recebida revelou estrutura dendrítica com carbetos de Nb e fase Laves nas regiões interdendríticas. A solubilização das amostras DMD durante 40 minutos por 1100 graus Celsius e 1200 graus Celsius mostrou ser insuficientes para a dissolução dos precipitados. A fim de melhorar a difusão do Nb e a dissolução dos carbetos e da fase Laves, foi realizado o tratamento de solubilização a 1200 graus Celsius por 100 horas. Esta amostra tratada a 650 graus Celsius por 100 horas apresentou carbetos M23C6 precipitados nos contornos de grão e nas interfaces entre matriz CFC e a fase Laves. Entretanto, no envelhecimento a 750 graus Celsius durante 100 horas ocorreu à precipitação dos carbetos M23C6 e M6C nos contornos de grão e dispersos na matriz, aumentando assim a dureza do material em 18 porcento, se comparada à mesma como solubilizada. O aumento da microdureza em 12 porcento após o tratamento térmico está relacionado à precipitação dos carbetos nos contornos de grão e dispersos na matriz resultado dos tratamentos térmicos de envelhecimento. / [en] This thesis studies the microstructural stability of Ni-base Super alloy 625 for its mechanical properties and its varieties of applications in the industry, in three different conditions: bulk (industrially forged plate), precursor powder particles for 3D printing process and a sample produced by laser Direct Metal Deposition (DMD). Aiming at promoting precipitation processes and, therefore, correlate with the mechanical properties of the material, samples of these conditions were submitted to solution annealing and isothermal aging treatments at 650 Celsius degrees and 750 Celsius degrees for 10 hours and 100 hours. Characterization of the microstructure was performed by optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), in the conventional diffraction contrast mode, scanning/transmission (STEM) analytical mode, and high resolution microscopy (HRTEM). Energy dispersive X-ray spectrometry (EDXS) and electron energy loss spectroscopy (EELS) were used to analyze the local composition of the matrix and precipitated phases. Micro hardness measurements were performed to evaluate the effect of thermal treatments. The microstructural analysis of the bulk sample in the as-received condition showed an equiaxial grain structure with NbTiC and M6C precipitated phases. Solid solution treatment at 1100 Celsius degrees for 40 minutes allowed partial dissolution of the carbides. Aging at 650 Celsius degrees for 10 hours showed NbTiC carbides and a hardness increase of 5 percent compared to the as-solubilized sample. However, aging at this temperature for 100 hours promoted the homogeneous precipitation of the gama phase, thus increasing the material s hardness by 45 percent, when compared to it as solubilized. The bulk sample aged at 750 Celsius degrees for 10 hours showed grain boundary and homogeneous precipitation of NbTiC and M23C6 carbides. This sample condition upon aging at this temperature for 100 hours shows δ phase homogeneously precipitated in the matrix. The microstructural analysis of the precursor powder showed micrometer size individual particles as polycrystalline, consisting predominantly of columnar grains of the austenitic matrix. Analysis of samples produced by DMD in the as-received condition revealed dendritic microstructure with carbides of Nb and Laves phase in the interdendritic regions. The solution treatment of the DMD samples for 40 minutes at 1100 Celsius degrees and 1200 Celsius degrees proved to be insufficient for the dissolution of the precipitate. In order to enhance diffusion of Nb and so carbide and Laves phase dissolution, a solution anneal was carried out at 1200 Celsius degrees for 100 hours. This sample treated at 650 Celsius degrees for 100 hours showed M23C6 carbides precipitated at grain boundaries and also at the Laves phase/matrix interfaces. However, upon aging at 750 Celsius degrees for 100 hours the precipitation of M23C6 and M6C takes place at the grain boundary and in the austenitic matrix, thus increasing the material s hardness by 18 percent, when compared to it as solubilized. The increase of the hardness by 12 percent after the heat treatment is related to the precipitation of the carbides in the grain boundaries and dispersed in the matrix resulting from the aging thermal treatments.

[ES] Los procesos convencionales de transformación de materiales requieren afrontar nuevos retos que se presentan en la actual sociedad industrial como es la propia sostenibilidad medioambiental. De la misma forma, los productos fabricados en el futuro deberán cumplir ciertos requisitos medioambientales, como la reciclabilidad de la materia prima utilizada. Dentro de este contexto la fabricación de productos mediante técnicas tridimensionales como la fabricación aditiva, permite utilizar únicamente el material necesario que se requiere para un producto completo. Dichas técnicas de fabricación son las solicitadas por el sector aeronáutico, entre otros, que requiere de unos valores de calidad muy exigentes. Dentro de estos ensayos, el estudio del comportamiento del material ante crecimiento de grieta es de gran importancia. Mediante este tipo de fabricación se obtiene un producto en estado casi final a través de la adición de capas de alrededor de 100 micras, que da como resultado una orientación de grano metalúrgico preferente y diferente a la misma aleación fabricada por forja convencional. Los fenómenos ocurridos durante la fabricación pueden dar lugar a defectos como grietas o porosidades que disminuyen las capacidades resistentes, por lo que un estudio para predecir la vida del componente es importante. Dentro de los procesos de fabricación aditiva nos encontramos con la fabricación por haz de electrones, que consigue calidades de material casi con porosidad nula, por lo que empresas del sector aeronáutico o médico consideran esta técnica como de gran fiabilidad. El trabajo desarrollado en esta tesis se basa en el estudio de aleaciones de titanio fabricadas mediante fabricación aditiva por haz de electrones. En concreto, el estudio se centra en el comportamiento a tenacidad a la fractura para relacionarlo con las características microestructurales más relevantes. Los análisis llevados a cabo consideran diversas orientaciones que tienen lugar en la bandeja de fabricación, realizándose ensayos mecánicos tanto estáticos como dinámicos. Una segunda parte de la tesis se basa en el modelado mediante elementos finitos extendido, XFEM, que se desarrolla como alternativa a los métodos tradicionales de mallado. En el XFEM una aproximación de elementos finitos se construye de forma que sea capaz de representar funciones de enriquecimiento dentro de los elementos mediante grados de libertad adicionales. Un punto crítico en el proceso de cálculo mediante elementos finitos es el proceso de mallado. La precisión obtenida en la aproximación depende del tamaño de los elementos de la malla. Por tanto, el cálculo con precisión en puntos importantes como la zona cercana a grieta exige una malla con un tamaño de elemento muy pequeño. Con la técnica XFEM se alcanza una mayor precisión mediante un proceso de enriquecimiento de extremo de grieta. Los resultados que ofrece la herramienta XFEM se comparan con los obtenidos experimentalmente con componentes fabricados mediante impresión 3D. Esta comparativa se lleva a cabo sobre diversas geometrías con la presencia de agujeros, de tal forma que se ha podido predecir el crecimiento de grieta que tiene lugar en materiales por impresión 3D. De la misma forma, se llevan a cabo comparativas de piezas con geometría compleja, para validar el modelo desarrollado. / [CA] Els processos convencionals de transformació de materials requereixen afrontar nous reptes que es presenten en l'actual societat industrial com és la pròpia sostenibilitat mediambiental. De la mateixa forma, els productes fabricats en el futur hauran de complir certs requisits mediambientals, com el reciclatge de la matèria primera. Dins d'aquest context, la fabricació de productes mitjançant tecnologia 3D com la fabricació additiva, permet usar només el material necessari que es requereix per a un producte complet. Aquestes tècniques de fabricació són les sol·licitades pel sector aeronàutic que requereix d'uns valors de qualitat molt exigents. Dins d'aquests assajos, l'estudi del comportament del material a través de creixement de clivella és vital. Mitjançant aquesta mena de fabricació s'obté un producte en estat quasi final a través de l'addició de capes d'alçària al voltant de 100 micres, que dona com a resultat una orientació de gra metal·lúrgic preferent i diferent al mateix però fabricat convencionalment. Els fenòmens ocorreguts durant la fabricació poden donar lloc a defectes com a clivelles o porositats que poden disminuir les capacitats resistents, per la qual cosa un estudi per a predir la vida del material és important. Dins dels processos de fabricació additiva ens trobem amb la fabricació per feix d'electrons la qual aconsegueix qualitats de material quasi amb porositat nul·la, per la qual cosa empreses del sector aeronàutic i mèdic han conclòs a aquesta tècnica com la més fiable. El treball desenvolupat en aquesta tesi es basa en l'estudi d'aliatges de titani fabricades mitjançant fabricació additiva per feix d'electrons, principalment el seu comportament a la tenacitat a la fractura per a relacionar-ho amb les característiques microestructurals més rellevants. Les anàlisis dutes a terme se centren en diverses orientacions que tenen lloc en la plataforma de fabricació, realitzant-se assajos mecànics tant estàtics com dinàmics. Una segona part de la tesi es basa en el modelatge mitjançant elements finits estesos, XFEM, que es desenvolupa com a alternativa als mètodes lliures de malla. En el XFEM una aproximació d'elements finits es construeix de manera que siga capaç de representar funcions (enriquiment) dins dels elements. Un punt crític en el procés de càlcul en qualsevol mètode que usa una malla és el procés d'emmallat. La precisió obtinguda en l'aproximació depén de la grandària dels elements de malla. Per tant, el càlcul amb precisió en punts importants, com la zona pròxima a clivella, exigeix l'ús d'una malla amb una grandària d'element molt xicoteta. Amb la tècnica XFEM aconseguim aqueixa precisió mitjançant un procés de enriquiment. / [EN] Conventional material transformation processes require facing new challenges that arise in today's industrial society, such as environmental sustainability. Similarly, products manufactured in the future must meet certain environmental requirements, such as the recyclability of the raw material used. Within this context, the manufacture of products using 3D technology such as additive manufacturing, allows using only the necessary material that is required for a complete product. These manufacturing techniques are requested by the aeronautical sector, which requires very demanding quality values. Within these tests, the study of the behavior of the material through crack growth is of great importance. By means of this manufacturing technology, a product is obtained in an almost final state through the addition of layers of about 100 microns, which results in a preferential metallurgical grain orientation and different from the same alloy manufactured by conventional methods. The phenomena occurring during manufacturing can lead to defects such as cracks or porosities that can reduce the strength capabilities, so a study to predict the life of the component is important. Within the additive manufacturing processes we find the electron beam manufacturing which achieves material qualities with almost zero porosity. As a consequence, companies in the aeronautical or medical sector have concluded this technique as very reliable. The work developed in this thesis is based on the study of titanium alloys manufactured by electron beam additive manufacturing. More precisely, the work is focused on the fracture toughness behavior in order to relate it to the most relevant microstructural characteristics. The analyses carried out consider different orientations and positions that take place in the fabrication tray, performing both static and dynamic mechanical tests. A second part of the thesis is based on the application of the extended finite element method, XFEM, which is developed as an alternative to conventional finite element method. In XFEM a finite element approximation is constructed in such a way that it is able to represent functions within the elements. A critical point in the calculation process in the finite element method is the meshing process. The accuracy obtained in the approximation depends on the size of the elements of the mesh. Therefore, accurate computation at important points such as the near-crack zone requires the use of a mesh with a very small element size. With the XFEM technique, we achieve this accuracy by means of an enrichment process. The results provided by the XFEM tool are compared with those obtained experimentally with respect to components manufactured by 3D printing. This comparison is carried out on different geometries with the presence of holes, in such a way that it has been possible to predict the crack growth that takes place in 3D printed materials. In the same way, comparisons of parts with complex geometry are carried out to validate the developed model. / Niñerola González, R. (2022). Estudio del comportamiento por crecimiento de grieta de aleaciones fabricadas por adición mediante haz de electrones [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/183818 / TESIS