For many metal components the presence of hard, non-metallic inclusions such as oxides lowers the impact toughness by acting as fracture initiation points and easing crack propagation. In components produced by powder metallurgy hot isostatic pressing (PM HIP), oxides often form a continuous network of small, spherical inclusions after consolidation at the prior particle boundaries (PPB). It is therefore of great importance to reduce surface oxides before consolidation in order to improve mechanical properties. In this work, oxides were attempted to be reduced directly prior to the consolidation of one tool steel and one low-alloy steel by introducing H2 into sealed PM HIP capsules. The two H2-carriers were hollow glass microspheres and the compound ammonia borane (H3NBH3). The H2-carriers were placed separately from the metal powder. Microspheres were filled at 300 °C with a gas mixture at 675 bar resulting in a storage capacity of 0.16 wt%. Gaseous species released from the H2-carriers during heating were analysed by mass spectrometry. Results showed that the microspheres only release H2 while ammonia borane in addition releases other nitrogen and boron containing species. Impact testing as well as chemical and microstructural analysis were performed on the two consolidated materials with samples retrieved from different vertical and radial positions. Both H2-carriers had leaked into the material resulting in decreased impact toughness compared to the reference. Further from the source of the contaminants, oxygen content was reduced and impact toughness was improved. Microspheres showed overall better reduction ability even though they release less hydrogen compared to ammonia borane. Impact toughness was not improved as much with ammonia borane even though similar oxygen levels were achieved. Ammonia borane’s decomposition products likely obstruct the oxide reduction or introduce new inclusions lowering the impact toughness. / Det är för många metallkomponenter viktigt att så mycket som möjligt undvika hårda, icke metalliska inneslutningar. Detta eftersom de sänker slagsegheten genom sprickinitiering men även genom att underlätta spricktillväxt. Ytoxider i komponenter tillverkade genom pulvermetallurgisk het-isostatisk pressning (PM HIP) bildar ofta ett kontinuerligt nätverk av små, sfäriska inneslutningar efter konsolidering vid de tidigare partikelgränserna. Det är därför viktigt att reducera ytoxider före konsolidering för att förbättra de mekaniska egenskaperna av komponenter tillverkade genom PM HIP. I detta examensarbete har ytoxider reduceras direkt före konsolidering av ett låglegerat stål och ett verktygsstål genom att tillsätta H2 i de förseglade PM HIP kapslarna. Två vätgasbärare testades, ihåliga mikrosfärer av glas och ammoniak boran (H3NBH3). Vätgasbärarna var placerade i ett område avskilt från metallpulvret. Mikrosfärerna fylldes med en gasblandning vid 675 bar och 300 °C vilket resulterade i en lagringskapacitet på 0.16 vikt%. Gaser som frigjordes från vätgasbärarna vid uppvärmning analyserades med en masspektrometer. Resultatet visade att mikrosfärerna bara frigör H2 medan ammoniak boran också frigör andra ämnen innehållande kväve och bor. Slagprovning och analys av mikrostruktur samt syre- och kvävehalter utfördes på de två konsoliderade materialen med prover från olika vertikala och radiella positioner. Båda vätgasbärarna hade läckt in i materialet vilket resulterade i minskad slagseghet jämfört med referensmaterialet. Längre från vätgasbärarnas ursprungsposition var slagsegheten bättre och syrehalten lägre. De vätgasfyllda mikrosfärerna uppvisade överlag bättre förmåga att minska syrehalten trots att de innehöll mindre H2 jämfört med ammoniak boran. Slagsegheten förbättrades inte lika mycket med ammoniak boran trots att liknade syrenivåer uppmättes. Ammoniak boranets pyrolysprodukter förhindrar möjligtvis oxidreduktionen eller introducerar nya inneslutningar som resulterar i en försämrad slagseghet.

Metastable austenitic and duplex stainless steels are widely used materials in industrial anddomestic applications, owing to their attractive characteristics such as good corrosion resistanceand favorable mechanical properties. Both types of steel experience enhanced mechanicalproperties during plastic deformation due to the formation of the martensite phase from theparent austenite phase, this is called deformation-induced martensitic transformation (DIMT).It is therefore of technical interest to study the transformation mechanism and its impact onmechanical properties for a better understanding and ultimately for developing new materialswith improved performance in certain applications. In the present thesis, two austenitic stainless steels (201Cu, HyTens® 301) and two duplexstainless steels (FDX25®, FDX27®) were investigated. Samples were tensile tested during insitusynchrotron radiation experiments performed at the Cornell High Energy SynchrotronSource (CHESS), Ithaca, USA. Tests were performed at both room temperature and at elevatedtemperatures. The collected diffraction data were then processed by software such as Fit2D andMATLAB. Quantitative phase fraction analysis based on the direct comparison method wasperformed successfully. Microstructural analysis of samples before deformation and after thefull tensile testing was also performed using electron microscopy. The deformation induced martensitic transformation took place in HyTens 301, FDX25 andFDX27, but in 201Cu the austenite was stable during the tensile tests conducted here. The a’-martensite formed in a significantly higher fraction than the ε-martensite in all alloys. At roomtemperature, the critical stress levels for martensitic transformation were 490 MPa, 700 MPaand 700MPa for HyTens 301, FDX25 and FDX27, respectively.

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

Continuous caster moulds are the last and most important stage in the steelmaking process, where inclusions can either be generated or removed. With increasing casting speed using conventional immersion nozzles critical problems, such as unstable bulk mould flow have been noticed. Mould flux entrapment due to vortex and shearing action from the oscillating surface waves have become of particular concern. It is therefore necessary to have a calm inlet flow at the entrance of the mould. Recently, it has been acknowledged that a swirl blade placed at the upstream of the immersion nozzle effectively resolves the problems arising from unstable bulk mould flow. Therefore, to increase the knowledge of effect of swirling flow on the flow pattern in the mould, fundamental mathematical models of a billet mould equipped with a swirl blade in the nozzle have been developed. The model was used to study the effect of divergent angle of the immersion nozzle and mould aspect ratio on the flow field and temperature distribution inside billets moulds. Data from water model experiments were used to verify the mathematical model predictions. A fairly good agreement was found between physical modeling data and predictions, which ensured that the numerical model is reliable. Thereafter, the differences between square and round billet moulds were studied. Next, the effect of changing aspect ratio of the rectangular mould on the fluid flow and heat transfer, while keeping mould surface area constant, was studied. Two types of immersion nozzles, bottomless and conventional, were also analyzed during the research. The model moulds were changed gradually from a square billet with an aspect ratio of 1x1 to a rectangular billet with an aspect ratio of 3x1. First, the temperature and velocity distributions were calculated. Later, unsteady calculations were done to determine velocity fluctuations on the meniscus level for two types of nozzles and several moulds geometries. / <p>QC 20101110</p>

The focus of this thesis is to develop a simulation model for predicting ductile fractures during hot working at Alleima. The main fracture mechanism in these conditions is ductile fracture by void coalescence. The ductile fractures are caused by the linking of voids that appear when there is large plastic deformation near second-phase particles. The chosen method to simulate these was to use a Ductile Fracture Criterion (DFC), which builds on using FE models with a damage parameter. Two criteria were selected to be tested. The austenitic stainless-steel alloy 316L was selected as material for this work. Using the Gleeble 3500 system, hot tension and compression experiments were performed to gather data needed for the simulation models as well as inducing ductile fractures. Rupture occurred for all the hot tension samples and cracks were found for only one of the hot compression experiments. Using data from the Gleeble tests, a separate simulation model for each of the setups were created using the finite element software Marc/Mentat. A flow stress model for 316L was developed. Results from the simulations show that both selected DFCs can be used to predict ductile fractures. Particularly for hot tension. It was shown that it is important to model the temperature gradient in the sample accurately. For hot compression, it was difficult to conclude if the criterions were able to predict fracture since only one data point was available. The thesis concludes that there could be of interest with continued work using DFCs at Alleima.

During the pyrometallurgical extraction of copper, a significant part of the copper is lost with discard slag, which decreases profits, overall copper recovery, and efficiency of raw material usage. Smelting furnace slag usually has a copper content that is close to or higher than that of copper ores. The investigation of copper losses to slag is thus a task of practical significance, as the ore grades are depleting. Slag cleaning, e.g., a settling furnace, can reduce copper losses to slag as the mechanically suspended copper-containing droplets separate from slag under the action of gravity and can hence be recovered.  An industrial trial was conducted in an electric settling furnace with slag originating from an electric smelting furnace and processed in a zinc fuming furnace. The trial was conducted to increase the understanding of copper losses to slag and how the process parameters temperature and settling time influence the slag copper content. The obtained slag samples were also evaluated to gain better insights as to the settling mechanism and, if any, factors that hinder the copper phases from settling. Slag modification with CaO was also evaluated to investigate how the modification influences the settling of copper phases and, thus, the final slag copper content.  Samples collected during the industrial trial were the basis for the evaluation in the current work. The samples came from batches with varying temperatures, settling times, and CaO content collected at four different sample positions. Instrumental techniques, including XRF, FAAS, ICP-SFMS, and SEM-EDS, were used to analyze the chemical compositions of the samples and the appearance of copper and associated phases.  The results indicated that the copper content of outgoing slag increased with increasing temperature in the evaluated interval. The copper content was also concluded to be more strongly affected by the temperature compared to the settling time. Regulating the temperature to the lower temperature interval in the settling furnace could thus decrease the final slag copper content. During the slag characterization, it was found that suspended copper-containing phases were hindered from settling, due to the attachment to solid phases and gas bubbles in the slag. By controlling and minimizing the presence of the bottom buildup and thus solid phases in the slag, the copper content can be decreased. The results indicated that the CaO slag modification decreased the final slag copper content, and can thus be used as a modifier for increased settling.

The focus of this master’s thesis is on the heat treatment of Ni-base alloys, specifically the risk of intermetallic σ-phases during different stages of heat treatment. The alloy studied is Sanicro®28, a super-austenitic stainless steel produced by Alleima AB. The problem at hand is that the quench-annealing stage is in high demand at the manufacturing facility, and the goal is to investigate if it can be removed from the manufacturing route. During forging, the outer surface and bar-ends can reach low temperatures, posing a high risk of σ-phase precipitation. Additionally, a necklace structure with large grains surrounded by fine re-crystallization is often observed at the surface of forged superalloys/Ni-base alloys. Today, this forged structure is re-crystallized and σ-phase dissolved during the quench-annealing stage. An alternative to quench-annealing after forging is to re-heat the bar using a Car Wagon Furnace(CWF). The thesis includes two laboratory experiments simulating two stages of heat treatment, the CWF and induction furnaces/soaking. The samples subjected to simulated CWF treatment showed re-crystallization throughout the entire structure. Annealing in CWF removes the large grains in surface positions. The time in the CWF also showed to be sufficient to dissolve σ-phase present from forging. Samples heated to the induction furnace set temperature do not contain precipitates, while temperatures below the induction set temperature induce σ precipitation to varying degrees. The key findings of the thesis are as follows: • Re-heating in a CWF right after forging is enough to dissolve σ-phase at half-radius and surface locations. • Quench-annealing stage could be removed by changing the route to a CWF after forging. • If temperatures fall below the σ-maximum stability temperature during induction furnace heating cycles, σ-phase precipitation occurs.

Nickel-based superalloys and tool steels are well-known high-performance alloys due to their extensive use in many different industries. Nickel-based superalloys have found their way into aircraft, aerospace, marine, chemical, and petrochemical industries owing to their excellent high-temperature corrosion and oxidation resistance. On the other hand, tool steels could provide a combination of outstanding corrosion and wear resistance. They can play an important role in cutting and wear applications and manufacturing plastic extrusion and food processing components. Near-net shape manufacturing using powder metallurgy (PM) and hot isostatic pressing (HIP) can serve as an efficient manufacturing process to produce these alloys. This technology can successfully tackle conventional manufacturing challenges of highly alloyed materials i.e. segregation during the casting process or cracks during hot working processes of Ni-based superalloys, and carbide segregation and formation of large and irregularly shaped carbides in wrought and hot rolled tool steels. However, the presence of precipitates on prior particle boundaries (PPBs) in Ni-based superalloys, and metallurgical defects like non-metallic inclusions in both Ni-based superalloys and tool steels may affect the fatigue performance of these PM-HIPed products. This licentiate thesis aims to investigate the microstructure and fatigue behavior of two PM-HIPed alloys i.e. Inconel 625 and high-nitrogen tool steel. The results confirm precipitation along PPBs in PM-HIPed Inconel 625; however, no effect was detected in the fractography studies of the high cycle fatigue samples, and tensile properties were comparable with wrought materials reported in the literature. On the other hand, the microstructure of PM-HIPed high-nitrogen tool steel displayed dispersed precipitates and no traces of PPBs. Moreover, in both cases, i.e. very high cycle fatigue of PM-HIPed high-nitrogen tool steel and high cycle fatigue of PM-HIPed Inconel 625, fatigue crack initiation was attributed to the presence of non-metallic inclusions, either individually or agglomerated with precipitates. This underscores the significance of the manufacturing process in fatigue performance. / Near-net shape manufacturing using powder metallurgy (PM) and hot isostatic pressing (HIP) can serve as an efficient manufacturing process to produce high-performance alloys. Among the variety of engineering alloys, Nickel-based superalloys and tool steels stand out as well-known high-performance alloys, widely employed across diverse industries. PM-HIP technology can successfully address conventional manufacturing challenges associated with highly alloyed materials, such as segregation during the casting process or cracks during hot working processes of Ni-based superalloys, and carbide segregation and the formation of large and irregularly shaped carbides in wrought and hot rolled tool steels. However, the presence of precipitates on prior particle boundaries in Ni-based superalloys, and metallurgical defects like non-metallic inclusions in both alloys, may affect the fatigue performance of these PM-HIPed products. The present study aims to assess two PM-HIPed alloys, namely Inconel 625 and high-nitrogen tool steel, with a comprehensive examination of their microstructure and fatigue properties. The objectives include examining the microstructural features introduced by the PM-HIP process and understanding how they influence fatigue failure mechanisms in these alloys.

Gas atomization is regarded as a reliable method for creating high-quality metal powders from molten metal. The liquid metal is fed into the chamber as a free-falling stream through a nozzle, where it is impinged by high-velocity gas jets, causing degeneration and production of metal droplets, which solidify to create metal powders. As the metal droplets fall lower towards the collection hoopers, the solidification process begins. As a result, having a strong handle on the process parameters helps to produce metal powders that are fine, spheroidized, and have good characteristics. A free fall atomizer with twelve discrete nozzles, having a cylindrical internal profile, arranged in two different levels has been employed to introduce high-velocity gas jets into the chamber, for the current study. A cross-sectional sketch created by Uddeholm AB provided the geometric dimensions, and CFD was used to generate a simulation experiment for the system. Fluent setup input values were derived from literature data. The primary objective of the study is to analyze the influence of varying inlet pressure and the number of discrete gas jet nozzles, on the flow behavior of the atomizing gas. Additionally, the Discrete Phase Model approach was adopted to study the interaction of particles with the gas flow. The simulation model was validated by carrying out the visualization experiment, Schlieren imaging. From the study, it was realized that the results of the numerical model showed a mismatch relative to the experimental value. This can be attributed to the discretization technique, input parameters and the numerical model employed in this study. However, the parametric study provided a qualitative analysis regarding the influence of input parameters on flow behavior. It was studied that with increasing the inlet pressure and number of discrete nozzles there is a subsequent increase in the maximum velocity attained by the atomizing gas, resulting in a decrease in velocity of melt introduced into the system. Additionally, a radial pressure gradient was observed to be present that increased in accordance with the parameters, resulting in reduction of the melt film thickness produced during pre-filming mechanism. However, the Discrete Phase Model provided evidence that with increment in the gas to melt ratio, the number of particles that get dispersed to make collision with the domain wall increased. Thus, a subsequent increase in downstream velocity was required to maintain the particles within the domain walls as the study parameters were increased. / Gasatomisering betraktas vara en tillförlitlig metod för att skapa högkvalitativt metallpulver från smält metall. Den flytande metallen matas in i en kammare som en fri fallande ström genom ett munstycke, där den trycks in av höghastighetsstrålar. Vilket skapar en degeneration och en bildandet av metalldroppar som stelnar till att metallpulver kan skapas. Stelningsprocessen börjar när metalldropparna faller emot uppsamlingsbågarna. Ett fint och sfärisk metall metallpulver med goda egenskaper kan produceras genom att ha en god kontroll på processparametrarna. I denna studie har en ”Free Fall Atomizer” med tolv diskreta munstycken med en cylindrisk profil arrangerade i två olika nivåer använts för att introducera höghastighetsstrålar i kammaren. De geometriska dimensionerna var försedda från en ritning i tvärsnitt skapad av Uddeholms AB och samt användes en CFD för att generera ett simulationsexperiment av systemet. Ingångsvärden för inställningarna av flödena härleddes från litteraturdata. Huvudsyftet med studien var att studera flödesbeteendet av den atomiserande gasen genom att analysera inflytandet av att variera ingångstrycket och antalet diskreta gasstrålmunstycken. Dessutom togs det till en diskret fasmodell för att studera partiklarnas interaktion med gasflödet. Simulationsmodellen validerades genom att utföra ett visualiseringsexperiment genom Schlierenfotografering. Det framgick i studien att den numeriska modellens resultat inte stämde överens med det experimentella värdet. Detta kan attribueras till diskretiseringstekniken, inmatningsparametrarna och den numeriska modellen som användes i studien. Hur som helst försedde den parametriska studien en kvalitativ analys angående inflytandet av inmatningsparametrarna på flödesbeteendet. Det framgick att en ökning av ingångstrycket och av antalet av diskreta munstycken gav en påföljande ökning i den maximala hastigheten som den atomiserande gasen kan erhålla. Vilket resulterar till en sänkning av hastigheten av smältan som introduceras till systemet. Dessutom observerades en radiell tryckgradient vara närvarande som ökade i enlighet med parametrarna. Det resulterade i en reduktion av smältfilmtjockleken som producerades under förfilmingsmekaniskmen. Trots det visade den diskreta fasmodellen att en ökning av gas till smältförhållandet också ökade antalet partiklar som sprids vidare för att kollidera med domänväggen. Således krävdes en påföljande ökning av nedströmningshastigheten för att bibehålla partiklarna inom domänväggar när studiens parametrar ökade.

Additive manufacturing (AM) has experienced significant growth and development in recent years, owing to the ability to produce complex parts using a wide range of materials with relative ease. Powder bed-based metal AM has been at the forefront of this growth, even reaching the point where parts can be manufactured for end-use applications. Binder jetting (BJ) is one such technique where a liquid binder is selectively deposited on powder layers to create a green body which is then densified using sintering. The aim of this work was to use binder jetting to produce parts using Vanadis 4 Extra, a highly alloyed cold-work tool steel produced by Uddeholm AB for applications involving high demand on abrasive wear. Optimization of the densification parameters, which included debinding atmosphere, debinding temperature, sintering atmosphere, sintering temperature, and sintering time, to achieve full density parts was carried out as the first phase. It was found that the sintering atmosphere and time had the most significant impact on the density of the samples while the debinding atmosphere heavily impacted the C residue from the binder. In the second phase, samples were produced using the optimized parameters for mechanical analysis, which included analyses of the surface roughness and the wear resistance of the binder jetted samples against the conventionally produced samples. The surface roughness was in line with the data presented in literature for binder jetted samples. The binder jetted samples produced during this work exhibited better wear resistance than the conventionally produced samples, with the samples post-processed using hot isostatic pressing showing even better wear resistance. One possible explanation is the diffusion of N from the sintering atmosphere into the samples, leading to the conversion of carbides to carbonitrides and even nitrides. However, further investigation is needed in order to confirm this theory.