Thermo-Calc software AB develops high quality thermodynamic and kinetic databases to predict and simulate accurately multi-component phase behaviour in complex systems. One problem with their Ni-based alloys and superalloy solutions database (TCNI8) is poor description of tungsten partitioning for multi-component nickel based alloys. This work investigates the thermodynamic description of some lower-order systems i.e., Ni-W, Al-Ni-W and Cr-Ni-W by performing key experiments on three binary Ni-W alloys, and two ternary alloys (Al-Ni-W and Cr-Ni-W). Experiments at four different temperatures were carried out in which alloys were homogenized, equilibrated, quenched and investigated to determine the equilibrium solid/liquid compositions. Experimental results are used to validate the thermodynamic descriptions of the liquid and the fcc phase. Unlike ternary Al-Ni-W and Cr-Ni-W, binary Ni-W reproduced the experimental information in a satisfactory way. Ternary parameters for fcc are changed to fit the experimental results of this work. The findings of this work highlight that ternary parameters for the fcc of Al-Ni-W and Cr-Ni-W systems significantly effect the tungsten partitioning values in higher order systems. / Thermo-Calc Software AB utvecklar termodynamiska och kinetiska databaser av hög kvalitet för att korrekt kunna förutsäga och simulera jämvikter och fasomvandlingar i komplexa flerkomponentsystem. Ett problem med deras databas för Ni-baslegeringar och superlegeringar (TCNI8) är att beskrivning av volframpartitionering stämmer dåligt för nickelbaslegeringar. I detta arbete undersöktes den termodynamiska beskrivningen av vissa lägre system, dvs Ni-W, Al-Ni-W och Cr-Ni-W genom att utföra nyckelförsök på tre binära Ni-W-legeringar och två ternära legeringar (Al-Ni-W och Cr-Ni-W). Experimentvid fyra temperaturer utfördes i vilka legeringarna homogeniserades,jämviktsbehandlades, släcktes och undersöktes för att bestämma sammansättning för jämvikt fast fas/smälta. De erhållna experimentella resultaten användes för att validera den termodynamiska beskrivningen av smältan och fcc-fasen. Till skillnad från ternära Al-Ni-W ochCr-Ni-W, reproducerade den experimentella informationen den binära Ni-W-beskrivningen tillfredsställande. Ternära parametrar för fcc justerades efter de experimentella resultaten från detta arbete. Resultaten visar att de ternära parametrarna för fcc i Al-Ni-W och Cr-Ni-W systemen signifikant påverkar volframs fördelning mellan fast fas och smälta i nickelbaslegeringar.

The aim of this work was to systematically study how the microstructure evolution is affected by the carbon activity in WC-Ni cemented carbides. Seven WC-9.59at%Ni alloys with different carbon activity were sintered at 1500 °C. From investigating these alloys, the carbon window has been experimentally evaluated using light optical microscopy and compared to theoretical carbon window calculated using Thermo-Calc. The overall microstructure of cross sections and raw surfaces have been investigated using scanning electron microscopy. Finally, the WC grain size and distribution have been evaluated using electron backscatter diffraction. It was found that the experimental carbon window was slightly wider than the theoretical carbon window. The WC grain size increased and the grain size distribution got wider with increasing carbon activity. In addition, the largest WC grains showed the largest grain growth by increasing carbon activity. By comparing the present results of grain size and distribution of WC-Ni to previous results of WC-Co, it was found that the WC grain growth was more pronounced and more influenced by the carbon activity.

Tungsten (W) is listed among the European Union (EU) critical raw materials (CRMs) for its supply risk and economic importance. Primarily, tungsten is produced from scheelite and wolframite mineral ores with 0.08-1.5% tungsten trioxide (WO3) grade. However, as primary deposits for these resources are becoming less or lower in grade, alternative sources need to be explored. These alternative tungsten sources include scrap from end-of-life products, mine waste and rejects from the ore beneficiation processes (tailings). The latter alternative source is the focus within this thesis. Historical tailings repositories often pose environmental risks but may also become secondary sources of CRMs. This is because of relatively high minerals and metals content due to less efficient extraction methods and/or relatively low metal prices at the time of active mining. Therefore, reprocessing of such tailings is not only a supply risk-reducing measure but also an approach to remediation that contributes to the mining industry’s aim of moving towards a circular economy. The aim of this thesis has been to develop efficient methods for separating valuable minerals from the tailings in order to leave behind a stable and environmentally safe residue. Geometallurgical studies were conducted by collecting drill core samples from the Smaltjärnen tailings repository in Yxsjöberg, Sweden, for evaluating the potential of this repository for further processing. The tailings were originally produced from the ore that was mined by Yxsjö Mines while it was in operation from 1935 to 1963, with average ore grades of 0.3-0.4 wt.% WO3, 0.2 wt.% Cu and 5-6 wt.% fluorspar. The exploited minerals were scheelite for W, chalcopyrite for Cu and fluorspar. The tailings repository is estimated to have about 2.2 million tons of tailings covering an area of 26 hectares, with elemental concentrations of 1-2 wt.% S, 0.02-0.2 wt.% Cu, 0.02-0.3 wt.% W, 0.02-0.04 wt.% Sn and 0.02-0.03 wt.% Be. Sampling and characterization of the historical tailings were conducted based on geometallurgical units (i.e. a distinction between different layers and locations in the repository), followed by metallurgical test work. The tailings were characterized with regard to color and granulometry, particle size distribution, chemical composition, scheelite mineral occurrence, texture and mineral liberation, as well as mineralogical composition. Based on a comprehensive literature survey, tailings characteristics, and assessment of the earlier processes from which the Yxsjöberg tailings were produced, feasible separation methods were pre-selected involving dry low-intensity magnetic separation (LIMS) and high intensity magnetic separation (HIMS), enhanced gravity separation (EGS) using a Knelson concentrator, and batch froth flotation. The average WO3 and Cu concentration in these tailings based on the sampled locations was 0.15 % and 0.11 % respectively. Applying them to the estimated 2.2 million tons of tailings in this repository gives approximately 3300 tons of WO3 and 2512 tons of Cu. From the metallurgical test work, several feasible processing routes have been identified that need to be further assessed based on the economic and environmental criteria. / REMinE (Improve Resource Efficiency and Minimize Environmental Footprint)

Binderless tungsten carbide (BTC) ceramics are inherently difficult to process and very brittle. Most consolidation techniques for processing pure WC powder require long sintering times and intense energy consumption. High-T pressureless and pressure-assisted sintering processes often lead to low-quality and coarsened microstructures, thus limiting the use of WC ceramics to few niche applications. Field-assisted sintering techniques (FAST), like spark plasma sintering (SPS), significantly improve the densification of fine and ultrafine WC powders. However, SPS requires high current outputs and expensive apparatus. SPS ceramics still lack adequate toughness to extend the use of BTC components in heavy-duty applications requiring reliable load-bearing capability and/or resistance against rapid and unexpected impacts or temperature drops. This research work explored a new consolidation route capable of boosting the mass transport phenomena (accelerated sintering) and, simultaneously, introducing new microstructural features. The process called flash sintering (FS) offers great potential in accelerating diffusion phenomena and altering the crystallographic and/or the defect chemistry of the sintered ceramics. Many scientific studies reported structural alterations, enhanced plastic flow and material softening by introducing “out-of-equilibrium” characteristics. Currently, FS technology requires, for its activation, a negative dependence of the electrical resistivity with temperature (NTC) of the material to be sintered. This is a universal requirement for the flash event to occur thus theoretically inhibiting the flash sintering of conductive materials with a positive temperature coefficient for resistivity (PTC), like metals or WC. In the present work, we reported how during electrical resistance sintering (ERS) experiments conducted on pure WC nanopowders, a flash event was triggered during the first seconds of the process. This was demonstrated to occur thanks to the different evolution of the electrical properties of a granular compact with temperature. WC powders possess an initial NTC behaviour which can activate a transitory thermal runaway phenomenon which makes the activation of a flash event in these materials possible, intense enough to allow ultrafast densification in less than 10 s. This breakthrough allows to verify whether and how the flash event modifies the final sintered material. FS and SPS sintered ceramics were compared in their microstructural, physical and mechanical properties, thus pointing out how some peculiar modifications are exclusively present in the flash-sintered material. FS can stabilize the WC1-x metastable phase after cooling to room temperature, and this was demonstrated to alter the high-temperature deformation of WC micropillars during compression. In addition, FS BTC are inherently softer with respect to SPS ones, resulting in higher fracture toughness and slightly lower hardness. Even if not final, the results indicate how the flash sintering of WC can be explored further to process engineered BTC ceramics with an optimized hardness/toughness ratio and an enhanced deformability.

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Welding is used extensively in aerospace, automotive, chemical, manufacturing, electronic and power-generation industries. Thermally-induced residual stresses due to welding can significantly impair the performance and reliability of welded structures. Numerical simulation of weld pool dynamics is important as experimental measurements of velocities and temperature profiles are difficult due to the small size of the weld pool and the presence of the arc. From a structural integrity perspective of welded structures, it is necessary to have an accurate spatial and temporal thermal distribution in the welded structure before stress analysis is performed. Existing research on weld pool dynamics simulation has ignored the effect of fluid flow in the weld pool on the temperature field of the welded joint. Previous research has established that the weld pool depth/width (D/W) ratio and Heat Affected Zone (HAZ) are significantly altered by the weld pool dynamics. Hence, for a more accurate estimation of the thermally-induced stresses it is desired to incorporate the weld pool dynamics into the analysis. Moreover, the effects of microstructure evolution in the HAZ on the mechanical behavior of the structure need to be included in the analysis for better mechanical response prediction. In this study, a three-dimensional model for the thermo-mechanical analysis of Gas Tungsten Arc (GTA) welding of thin stainless steel butt-joint plates has been developed. The model incorporates the effects of thermal energy redistribution through weld pool dynamics into the structural behavior calculations. Through material modeling the effects of microstructure change/phase transformation are indirectly included in the model. The developed weld pool dynamics model includes the effects of current, arc length, and electrode angle on the heat flux and current density distributions. All the major weld pool driving forces are included, namely surface tension gradient, plasma drag force, electromagnetic force, and buoyancy. The weld D/W predictions are validated with experimental results. They agree well. The effects of welding parameters (like welding speed, current, arc length, etc.) on the weld D/W ratio are documented. The workpiece deformation and stress distributions are also highlighted. The transverse and longitudinal residual stress distribution plots across the weld bead and their variations with welding speed and current are also provided. The mathematical framework developed here serves as a robust tool for better prediction of weld D/W ratio and thermally-induced stress evolution and distribution in a welded structure by coupling the different fields in a welding process. / Ph. D.

Au cours de ce travail, un modèle physique et numérique 3D du procédé de soudage à l’arc TIG (Tungsten Inert Gas) a été développé dans l’objectif de prédire, en fonction des paramètres opératoires, les grandeurs utiles au concepteur d’assemblages soudés.Le modèle développé, à l’aide du code de calcul aux éléments finis Cast3M, traite les phénomènes physiques agissant dans la pièce et, plus particulièrement, dans le bain de soudage, l’arc étant traité comme une source. Pour ce faire, les équations non-linéaires de la thermohydraulique couplées à celles de l’électromagnétisme sont résolues en régime stationnaire avec un modèle prenant en compte la surface libre déformable du bain de soudage.Une première étape du développement a porté sur la modélisation des phénomènes électromagnétiques par deux méthodes numériques différentes, à comparer les résultats numériques obtenus avec ceux de la littérature. Ensuite, afin de valider le pouvoir prédictif du modèle, des simulations de différentes configurations de soudage d’intérêt ont été étudiées, en variant la composition chimique du matériau, la vitesse de défilement, la pression d’arc imposée et, plus particulièrement, la position de soudage. Des comparaisons avec des expériences et des modèles numériques de la littérature confirment les bonnes tendances obtenues. Enfin, une approche de la modélisation de l’apport de matière a été abordée et des résultats de cette approche ont été montrés. Notre modèle complet constitue donc une base solide pour le développement de modèles de simulation numérique du soudage (SNS) 3D totalement couplés avec l’arc dans le futur et sera intégré dans le logiciel métier WPROCESS. / In this work, we develop a 3D physical and numerical model of the GTA (gas tungsten arc) welding process in order to predict, for given welding parameters, useful quantities for the designer of welded assembly.The model is developed in the Cast3M finite element software and takes into account the main physical phenomena acting in the workpiece and particularly in the weld pool, subject to source terms modeling the arc part of the welding process. A steady solution of this model is thought for and involves the coupling of the nonlinear thermohydaulics and electromagnetic equations together with the displacement of the deformable free surface of the weld pool.A first step in the development consisted in modeling the electromagnetic phenomena with two different numerical methods, in comparing the numerical results obtained with those of the literature. Then, in order to assess the predictive capability of the model, simulations of various welding configurations are performed : variation in the chemical composition of the material, of the welding speed, of the prescribed arc pressure and of the welding positions, which is a focus of this work, are studied. A good agreement is obtained between the results of our model and other experimental and numerical results of the literature. Eventually, a model accounting for metal filling is proposed and its results are discussed. Thus, our complete model can be seen as a solid foundation towards future totally-coupled 3D welding models including the arc and it will be included in the WPROCESS software dedicated to the numerical simulation of welding.

An assessment of tin-skarn resources in the Erzgebirge, Germany, was conducted with the 3-Part Method. For this purpose a Grade-Tonnage Model for this deposit type was established. A literature review produced grade and tonnage data for 23 skarn deposits, of which 9 are in the assessment area. Based on an existing predictive map created with an AI algorithm, seven permissive tracts with a total area of 776 km² were defined. To estimate the number of undiscovered deposits a panel of five experts in the economic geology of the Erzgebirge was assembled. From the expert estimates and the newly developed Grade-Tonnage Model the undiscovered ore and metal tonnages in each permissive tract were evaluated. In four of the seven tracts the probability of the existence of at least one undiscovered deposit is estimated to be greater than 50%, in permissive tract 2 it is even greater than 90%. In each of these tracts, the median assessed undiscovered ore tonnages are several million tons and the tin resources exceed 10,000 tons. For the most perspective tract (Permissive tract 2) the median estimates are 40.6 Million tons of ore with a tin content of 114,000 tons. For tungsten (tonnages calculated as WO3) the numbers are slightly lower. The results verify the high resource potential of tin skarns in the Erzgebirge and can be used to guide future exploration activities to the most economically promising permissive tracts.