En raison d’une combinaison de propriétés physiques, chimiques et mécaniques remarquables, les alliages de titane et de titane sont devenus des candidats prometteurs dans le domaine de l'industrie chimique, de l’aéronautique, de l'aérospatiale et des matériaux biomédicaux. Durant les procédures de fabrication ainsi qu’en service, les composants sont exposés à des environnements tels que la surface de ces composant seront exposées à l’hydrogène. Par conséquent, la compréhension de l’interaction de ces matériaux avec l'hydrogène lors de divers procédés de d’élaboration et de mise en forme est importante afin que leurs propriétés et leurs performances puissent être contrôlées et prédites de manière fiable. Dans le but d'améliorer les propriétés et les performances du titane et de réduire le coût de fabrication des produits en titane, le présent travail se concentre principalement sur les effets de l'hydrogène sur le laminage à froid et le phénomène de recristallisation de deux titanes caractérisés par une structure cristalline différente, c'est-à-dire une structure hexagonale et cubique cubique pour respectivement le titane de pureté commerciale Ti50A et l'alliage de titane β-métastable β-21S. Étant donné que la microstructure du titane et de ses alliages est le facteur contrôlant leurs propriétés et leurs performances, l'évolution microstructurale en présence d'hydrogène introduit par deux méthodes distinctes a été analysée par une combinaison de techniques expérimentales incluant DRX, SEM-EBSD et TEM. L'introduction de l'hydrogène dans le Ti50A par une méthode électrolytique a conduit à la précipitation de deux types d'hydrures (δ-TiHx, ε-TiH2) dans la matrice de phase , et il a été constaté que la fraction volumique de ces hydrures augmentait avec la durée du temps de chargement électrolytique. En raison du mode de formation par précipitation à partir des joints de grains, cinq relations d'orientation (OR) entre la -phase et l'hydrure δ-TiHx ont été déterminées par analyses des projections stéréographiques, et parmi celles-ci trois nouvelles relations d'orientation ont pu être mise en évidence. En outre, la corrélation entre la texture de laminage et la précipitation à l'hydrure a pu être établie. On a constaté que l'existence de la texture de de laminage facilitait la précipitation d'hydrure δ suivant l'orientation d’orientation de type OR2. Les analyses de rayons X révélaient un élargissement des pics de diffraction de la phase , ce qui indiquait une augmentation de la densité de dislocation, ces dislocations étant nécessaires pour tenir compte de l'inadéquation du réseau entre les hydrures et la matrice. Sur la surface d’échantillons déformés en compression, l'observation des traces de glissement et de macle de tension de type TT1 {10 2} < 011> dans les -grains contenant des hydrures a suggéré que les hydrures avaient une certaine capacité à supporter une déformation de cisaillement, en fonction des relations d'orientation entre la matrice et les hydrures mais aussi de leur épaisseur. Bien qu'aucune corrélation directe entre la nucléation des macles et la présence des hydrures n’ait été établie dans cette étude, l'effet des hydrures sur le développement des macles a été constaté. En étudiant l’effet de l'hydrogène sur le comportement au laminage à froid dans Ti50A, il a été possible de montrer que la formation de macle de type TT1 peut être facilitée par l'augmentation du rapport c/a de la maille hexagonale résultant de l’addition de l'hydrogène et de l'existence de contraintes locales générées par la précipitation des hydrures. Un raffinement de la microstructure a également été observé dans le Ti50A hydrogéné, ce qui suggère que la présence d'hydrures a tendance à générer de nouveaux grains de fortes désorientations (HAB). En outre, de nombreuses dislocations géométriquement nécessaires (GND) permettant de tenir compte de l'incompatibilité de contrainte entre l'hydrure et [...] / Due to an attractive combination of physical, chemical and mechanical properties, titanium and titanium alloys have become promising candidates in the field of chemical industry, aerospace and biomedical materials. During manufacturing procedures and applications, components are exposed to environments that can act as sources of hydrogen. Therefore, understanding their interaction with hydrogen upon various mechanical/thermal processing is important so that their properties and performance can be controlled and reliably predicted. With the aim of enhancing the properties and performance of titanium and reducing the cost of manufacturing products, the present work is primarily focusing on the effect of hydrogen on the cold rolling behavior and the subsequent annealing of titanium and titanium alloy characterized by different crystalline structure, i.e. hexagonal and body cubic centered (bcc) structure for the commercial pure titanium Ti50A and metastable β-titanium alloy β-21S, respectively. Since the microstructure of titanium and its alloys is the governing factor that determines their properties and performance, the microstructural evolution in the presence of hydrogen upon various procedures was analyzed by combination of XRD, SEM-EBSD and TEM. The introduction of hydrogen in Ti50A by electrolytic method induced the precipitation of two types of hydrides (δ-TiHx, ε-TiH2) in the  phase matrix, and it was found that the volume fraction of these hydrides increased as the charging time increased. Five orientation relationships (ORs), three of them being new orientation relationships ever reported, between the -phase and the hydride δ-TiHx were determined. Moreover, the correlation between the rolling texture and the hydride precipitation was also established. It was found that the existence of the rolling texture facilitated the precipitation of δ-hydride following the OR2-type orientation relationship. X-ray analyses revealed a broadening of the diffraction peaks corresponding to the  phase, indicating a increase of the dislocation density, these dislocations being necessary to accommodate the lattice misfit between hydrides and the matrix. Under compression loading, the observation of slip traces and tension twin {10 2}< 011> TT1 in the -grains containing hydrides, suggested that the hydrides had a certain ability to accommodate the imposed shear strain, depending on the orientation relationships between the matrix and the hydrides as well as on their thickness. Although no correlation between the nucleation of twinning and the hydride could be established in this study, the hydrides seemed to play an important role on the development of twinning deformation. The effects of hydrogen on the cold rolling behavior in Ti50A showed that, the formation of TT1tension twins can be facilitated due to the increase of the c/a ratio owing to the hydrogen addition and the existence of local stresses generated by the precipitation of hydrides. The refinement of the microstructure was also observed in the hydrogenated Ti50A-H suggesting that the presence of hydrides can enhance the generation of high angle boundaries (HABs). In addition, the formation of numerous geometrically necessary dislocations (GND) allowing the accommodation of the strain incompatibility between the hydride and matrix could be worked out by SEM-EBSD, which also confirmed analyses of the X-ray traces. In the case of β-21S alloy, with bcc structure that can accommodate a larger concentration of interstitial atoms, hydrogen was introduced by gas method. The effect of hydrogen on the microstructure was found to be closely related to the hydrogen concentration. In the range of hydrogen/metal ratio 0.052 < H/M < 0.300, the microstructure consisting of the single β-phase showed that the dissolved hydrogen atoms expanded the bcc β-lattice and suppressed the decomposition of the β phase upon cooling [...]

abstract: Aluminum alloys are ubiquitously used in almost all structural applications due to their high strength-to-weight ratio. Their superior mechanical performance can be attributed to complex dispersions of nanoscale intermetallic particles that precipitate out from the alloy’s solid solution and offer resistance to deformation. Although they have been extensively investigated in the last century, the traditional approaches employed in the past haven’t rendered an authoritative microstructural understanding in such materials. The effect of the precipitates’ inherent complex morphology and their three-dimensional (3D) spatial distribution on evolution and deformation behavior have often been precluded. In this study, for the first time, synchrotron-based hard X-ray nano-tomography has been implemented in Al-Cu alloys to measure growth kinetics of different nanoscale phases in 3D and reveal mechanistic insights behind some of the observed novel phase transformation reactions occurring at high temperatures. The experimental results were reconciled with coarsening models from the LSW theory to an unprecedented extent, thereby establishing a new paradigm for thermodynamic analysis of precipitate assemblies. By using a unique correlative approach, a non-destructive means of estimating precipitation-strengthening in such alloys has been introduced. Limitations of using existing mechanical strengthening models in such alloys have been discussed and a means to quantify individual contributions from different strengthening mechanisms has been established. The current rapid pace of technological progress necessitates the demand for more resilient and high-performance alloys. To achieve this, a thorough understanding of the relationships between material properties and its structure is indispensable. To establish this correlation and achieve desired properties from structural alloys, microstructural response to mechanical stimuli needs to be understood in three-dimensions (3D). To that effect, in situ tests were conducted at the synchrotron (Advanced Photon Source) using Transmission X-Ray Microscopy as well as in a scanning electron microscope (SEM) to study real-time damage evolution in such alloys. Findings of precipitate size-dependent transition in deformation behavior from these tests have inspired a novel resilient aluminum alloy design. / Dissertation/Thesis / Doctoral Dissertation Materials Science and Engineering 2017

<p>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.</p><p>In <strong>supplement 1</strong>, 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 <strong>supplement 2</strong>, 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.</p><p>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 (<strong>supplement 2</strong>), X-ray diffraction (XRD) analyses were also performed on fine-powdered samples to confirm the existence of the observed phases.</p><p>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.</p>

Among the commercial aluminum alloys, aluminum 319 (Al-7wt%Si-4wt%Cu) type alloys are popularly used in automobile engine parts. These alloys have good casting characteristics and excellent mechanical properties resulting from a suitable heat treatment. To get a high strength in the 319 type alloys, grain refining, reducing the porosity, solid solution hardening, and precipitation hardening are preferred. All experimental variables such as solidification condition, composition, and heat treatment are influence on the precipitation behavior; however, precipitation hardening is the most significant because excess alloying elements from supersaturated solid solution form fine particles which act as obstacles to dislocation movement. The challenges of the 319 type alloys arise due to small size of precipitate and complex aging response caused by multi components. It is important to determine the chemical composition, crystal structure, and orientation relationship as well as precipitate morphology in order to understand the precipitation behavior and strengthening mechanism. In this study, the mechanical properties and microstructure were investigated using transmission electron microscopy and three dimensional atom probe tomography. The Mn and Mg effects on the microstructure and mechanical properties are discussed with crystallographic study on the iron intermetallic phases. The microstructural evolution and nucleation study on the precipitates in the low-Si 319 type aluminum alloys are also presented with sample preparation and analysis condition of TEM and 3DAP tomography.

Cette thèse s’est déroulée dans le cadre d’une cotutelle internationale entre l’IMT - École des Mines d’Albi-Carmaux et l’Ecole Polytechnique de l’Université de Sao Paulo (EPUSP). Elle a pour but de contribuer à l’étude du comportement mécanique des alliages de titane Ti6Al4V, et plus spécialement dans le domaine du formage superplastique et du formage à chaud. L’objectif général de ce doctorat est de contribuer au développement de procédés de formages non conventionnels des alliages de titane pour applications aéronautiques. C’est pourquoi, en fonction des équipements disponibles sur les deux sites, les travaux de recherche se sont déroulés soit à l’Ecole des Mines soit à l’EPUSP. Cette thèse adresse la problématique scientifique des interactions entre le comportement mécanique dans le domaine du formage superplastique et de formage à chaud d’une part et la microstructure initiale et son évolution dans le domaine de sollicitation d’autre part. Pour cela une stratégie d’essais et de caractérisation a été développée et suivie. Les essais incluent des essais mécaniques uniaxiaux à haute température sur différents alliages Ti6Al4V présentant des microstructures initiales différentes (taille de grain 0,5; 3,0 et 4,9 μm). Une attention particulière a été portée à l’évolution microstructurale avant essai - c’est- à-dire durant sa montée en température et la stabilisation thermique de l’échantillon – et durant l’essai. Les conditions d’essai ont été choisies de façon à couvrir le domaine du formage à chaud et du formage superplastique, température de 700°C à 950°C et vitesse de déformation entre 10-1 s-1 et 10-4 s-1. La croissance de grain dépend de la microstructure initiale mais aussi de la durée de l’essai en température (croissance statique) et de la vitesse de déformation (croissance dynamique). Afin d’améliorer la validité du modèle des observations microstructurales de taille de grain sont effectués après les essais mécaniques par micrographie optique et Microscope Electronique à Balayage. Un modèle de comportement unifié a été introduit de façon à être capable de couvrir toute la plage de température et de vitesse de déformation : écrouissage cinématique non linéaire, sensibilité à la vitesse de déformation et loi de croissance de la taille des grains sont inclus dans le modèle. Afin de pouvoir valider le modèle, il a été introduit dans le code de simulation ABAQUS®. Les résultats des simulations (en particulier déformation macroscopique et taille de grain locale) ont été comparés, pour l’un des matériaux de l’étude, aux résultats d’un essai de gonflage axisymétrique de tôle. Pour obtenir un cycle de contrôle simple, les essais effectués au laboratoire de l’IPT/LEL à Sao José dos Campos au Brésil ont été opérés à vitesse de déformation constante. Les résultats montrent une très bonne corrélation avec les prédictions et permettent de conclure à une validation du modèle de comportement développé dans la thèse dans des conditions industrielles de formage de l’alliage de titane. / This thesis was developed in the frame of a Brazil-France cooperation agreement between the École des Mines d'Albi-Carmaux and the Polytechnic School of Engineering of the University of Sao Paulo (EPUSP). It aims to contribute to the study of the mechanical behaviour of Ti6Al4V alloys especially in terms of superplastic forming. The general objective of this research is to develop non-conventional forming processes for new titanium alloys applied to aerospace components. Therefore, in accordance of the equipment’s available in the two groups, the work will be conducted either at the Ecole des Mines d'Albi-Carmaux and either at EPUSP. This thesis aims to answer questions such as what are the implications in relation to the microstructural and mechanical behaviour of these alloys during superplastic and hot forming in order to establish a behaviour law for these alloys based on titanium. This requires a good knowledge of the properties of materials used in the superplastic and hot forming domain to control the parameters governing the phenomenon of superplasticity or high temperature plasticity. For this, a testing strategy and characterization methodology of those new titanium alloys was developed. The tests include high temperature uniaxial tensile tests on several Ti6Al4V alloys showing different initial grain sizes. Special focus was made on the microstructural evolution prior to testing (i.e. during specimen temperature increase and stabilization) and during testing. Testing range was chosen to cover the hot forming and superplastic deformation domain. Grain growth is depending on alloy initial microstructures but also on the duration of the test at testing temperature (static growth) and testing strain rate (dynamic growth). After testing microstructural evolutions of the alloys will be observed by optical micrograph or SEM and results are used to increase behaviour model accuracy. Advanced unified behaviour models where introduced in order to cover the whole strain rate and temperature range: kinematic hardening, strain rate sensitive and grain growth features are included in the model. In order to get validation of the behaviour model, it was introduced in ABAQUS numerical simulation code and model predictions (especially macroscopic deformation and local grain growth) were compared, for one of the material investigated, to axisymmetric inflation forming tests of sheet metal parts, also known as bulge test. To obtain a simple control cycle, tests performed at IPT/LEL laboratory in San José Dos Campos in Brazil were operated with a constant strain rate. Results show a very good correlation with predictions and allows to conclude on an accuracy of the behaviour models of the titanium alloys in industrial forming conditions.

Methods for and computed results of including the physics and spatial attributes of microstructures are presented for a number of materials applications in devices. The research in our group includes applications of computation of macroscopic response of material microstructures, the development of methods for calculating microstructural evolution, and the morphological stability of structures. In this review, research highlights are presented for particular methods for computing the response in: 1) ferroelectric materials for actuator devices; 2) coarse-graining of atomistic data for simulations of microstructural evolution during processing; 3) periodic and non-periodic photonic composites; and 4) re-chargeable battery microstructures. / Singapore-MIT Alliance (SMA)

A good slag practice is essential for production of a high-quality stainless steel. In addition, the electrical and material efficiency of the electric arc furnace (EAF) can considerably be improved by a good slag practice. The metallurgical properties of the slag are strongly influenced by its high-temperature microstructure. Thus, characterization of the phases within the EAF slag as well as the determination of the amount of these phases is of high importance.In addition, the knowledge about the chemical composition of the liquid slag and solid phases at the process temperatures is instrumental in developing a good slag practice.In order to study the slag in EAF high-chromium stainless steelmaking, slag samples were collected from 14 heats of AISI 304L steel (two samples per heat) and 7 heats of duplex steel (three samples per heat).The selected slag samples were petrographically studied both using scanning electron microscopy equipped with energy dispersive X-ray spectroscopy (SEM-EDS) and light optical microscopy (LOM). In some cases, X-ray diffraction (XRD) analyses were also performed. Moreover, computational thermodynamics was used to determine the equilibrium phases in the EAF steelmaking slags at the process temperatures. In addition, parameter studies were performed on the factors influencing the equilibria.More specifically, a petrographical and thermodynamic characterization was performed on the EAF austenitic steelmaking slags. Thereafter, the microstructural evolution of the slag during the EAF duplex steelmaking process was investigated. Moreover, an investigation with focus on the total amount of precipitates within the high-chromium stainless steelmaking slags was done. Finally, the foamability of these slags was quantified and evaluated.The petrographic investigations showed that, during the refining stage, in both austenitic and duplex cases, the main constituent of the EAF slag is a melt consisting of liquid oxides. In addition, the slag samples contain solid spinel particles. However, before ferrosilicon-addition (FeSi), the slag may also contain solid stoichiometric calcium chromite. Moreover, depending on the slag basicity, the slag may contain solid dicalcium silicate at the process temperatures.The evolution of the slag during the refining stage of the EAF was graphically illustrated in the calculated isothermal phase diagrams for the slag system Al2O3-Cr2O3-CaO-MgO-SiO2-TiO2.It was found that the only critical parameter affecting the amount of solid spinel particles in the slag is the chromium-oxide content. More specifically, it was shown that the amount of the spinel particles in the slag increases with an increased chromium-oxide content of the slag. It wasvialso shown that a higher basicity and a lower temperature of the slag contribute to the dicalcium silicate precipitation.In order to evaluate and quantify the foamability of the slags, the slag’s physical properties influencing its foaming index were determined. Computational thermodynamics was used as a tool to calculate the weight fractions of the solid phases within the slag at different EAF process stages. The computational thermophysics was used to estimate the viscosity of the liquid part of the slag samples at the process temperatures. The apparent viscosity of the samples was calculated by combining the above results. By estimating the density, surface tension and the foaming-gas bubble size, the foaming index of the slag samples were quantified. It could be shown that the foaming index of the EAF high-chromium stainless steelmaking slag may be on its minimum as the slag’s basicity takes a value in the range of 1.2 – 1.5. A basicity value of around 1.50 – 1.60 can be suitable for enhancing the foaming index of the slag, during the refining period in EAF high-chromium stainless steelmaking.

In this thesis, we present an experimental and numerical study of globularization during reheating of thixocast billet having non-dendritic microstructure. The process of reheating is an important step in the semisolid processing and is essential to control its microstructure and hence its mechanical properties. Material chosen for this study is Aluminum alloy, A356. The primary focus of this study is the heat treatment below eutectic temperature i.e. transformation in solid phase. It is found that during short duration heat treatment, globularization of primary α grains and spheroidization of eutectic Si flakes take place which improves the mechanical properties of semisolid cast products significantly. A prolonged heat treatment is found to degrade the properties of castings since it enhances the porosity and coarsening of Si. The study suggests that a precise heat treatment practice can be designed to improve the semisolid microstructure. A computational model based on Phase field approach has been proposed to study this phenomena. Predictions based on this model are qualitatively compared with corresponding experimental observations. Since eutectics form an important step in multiphase solidification, an attempt has been made to develop an enthalpy based explicit micro-scale model for eutectic solidification. In this preliminary study, growth of adjacent α and β phases in a two dimensional Eulerian framework has been simulated. The model is qualitatively validated with Jackson Hunt theory. Results show expected eutectic growth. This methodology promises significant saving in computational time compared to existing numerical models.

Le frittage par micro-ondes est une nouvelle technologie de chauffage rapide utilisée pour l’élaboration de matériaux par le procédé de métallurgie des poudres. Cette méthode de frittage est non seulement économique en temps et en énergie, mais peut aussi permettre d’améliorer les propriétés finales du matériau. Cependant, l’effet bénéfique que peut apporter le chauffage par rayonnement micro-ondes n'est pas encore complètement compris.Dans ce cadre, cette thèse porte sur la mise en œuvre et les comparaisons des comportements en frittages conventionnel et micro-ondes multimodes (2,45 GHz) de l’alumine. La densification et l'évolution de la microstructure des échantillons frittés ont été analysés et comparés entre ces deux processus de chauffage en relation avec la nature des poudres de l'alumine : surface spécifique et teneur en dopant magnésie.A partir du suivi dilatométrique du frittage au cours des traitements conventionnel et micro-ondes, nous déterminons en anisotherme les énergies d’activation apparentes, qui sont considérées comme les paramètres importants de la thermodynamique de frittage : les valeurs trouvées sont toujours plus faibles dans le cas du frittage sous champ électromagnétique, preuve que les diffusions conduisant à la densification sont favorisées. Le suivi in situ permet aussi de déterminer les mécanismes de frittage (étude cinétique), par exploitation des courbes obtenues en traitement isotherme : la diffusion aux joints de grains reste le mécanisme dominant dans la plupart des cas, sauf pour une nanopoudre où la réaction d’interface devient le mécanisme limitant sous champ micro-ondes, preuve là encore de l’influence du champ électromagnétique sur la diffusion.Nous avons ainsi mis en évidence et expliqué les effets d’un champ électromagnétique sur le phénomène de densification, contribuant à terme à la maîtrise de l’application du rayonnement micro-ondes dans l’industrie céramique. / Microwave energy has been successfully applied as a heating source in the field of powder metallurgy. Compared with conventional heating techniques, microwave sintering has a high potential to reduce the processing time as well as temperature, and to optimize functional properties. However, the detailed explanation of this enhanced effect underlying microwave sintering is still under debate.Taking into account those issues, the objective of this work was to investigate comparatively conventional and 2.45 GHz microwave multimode sintering of alumina. The densification behavior and microstructure evolution of alumina powders with different MgO doping levels as well as specific surface areas have been systematically and quantitatively studied.By the way of dilatometric measurements in both conventional and microwave processes, studies in terms of thermodynamics were carried out in non-isothermal conditions. The apparent activation energy values are significantly lowered when microwave is applied, indicating a microwave-induced enhancement on diffusion. Furthermore, densification kinetics was isothermally taken in order to study in more detailed manner the mechanism(s) involved during microwave sintering. It suggests that the grain boundary diffusion is the dominant mechanism in most cases, except for a nanopowder. In the case of fine-grained alumina, it was assumed that microwave-assisted densification is controlled by in-series “interface-reaction / grain-boundary diffusion” mechanism. But anyway, grain-boundary diffusion has been always enhanced by microwave non-thermal effect.This work will be meaningful to develop the in-depth understanding of the microwave sintering process at both the fundamental and the applied levels.

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