Ziel der vorliegenden Arbeit ist es, die Herstellung von Grünkörpern mit vereinzelt unter Zentrifugalkraft sedimentierenden Partikeln und kontinuierlicher Partikelzufuhr zu untersuchen und ihre Eignung als neue Herstellungsvariante für metallische Grünteilhalbzeuge zur weiteren Verarbeitung mittels CNC-Zerspanung zu bewerten. Zur umfassenden Einordnung der Herstellungsmethode untergliedert sich die Zielstellung zum einen in die Beleuchtung des Einflusses des Ausgangspulvers auf die Packungscharakteristik der Sedimente. Dabei sollen vorteilhafte Partikelgrößenverteilungen identifiziert und typische Packungsphänomene bei der vereinzelten Sedimentation aufgedeckt werden. Zum anderen richtet sich der Fokus auf die Untersuchung prozessbedingter Einflüsse. Ziel ist hier die Ermittlung von Prozessgrenzen und erreichbaren Gründichten sowie die Identifikation potentieller Defektquellen. Alle Untersuchungsschwerpunkte werden im Hinblick auf den Sinterschritt bewertet. / The aim of the present work is to investigate the production of green bodies with particles sedimenting individually under centrifugal force and continuous particle feeding and to evaluate their suitability as a new manufacturing variant for metallic semi-finished green parts for further processing by means of CNC machining. For a comprehensive classification of the manufacturing method, the objective is subdivided on the one hand into the examination of the influence of the starting powder on the packing characteristics of the sediments. In this context, advantageous particle size distributions are to be identified and typical packing phenomena in isolated sedimentation are to be revealed. On the other hand, the focus is on the investigation of process-related influences. The aim here is to determine process limits and achievable green densities as well as to identify potential defect sources. All investigation foci will be evaluated with respect to the sintering step.

Amorphous and nanostructured Al-based alloys have attracted significant interest owing to their promising properties, including high strength combined with low density. Unfortunately, the production of these advanced materials is limited to powders or ribbons with thickness of less than 100 micrometers due to the reduced glass forming ability of the Al-based alloys. Powder metallurgy through pressure-assisted sintering is a good solution to overcome the size limitation of these materials. In this thesis, Al84Gd6Ni7Co3 glassy powders were consolidated into high-strength bulk materials by hot pressing. The sintering behavior and the microstructural evolution during hot pressing were analyzed as a function of temperature. The results reveal that, through the careful control of the sintering temperature, the combined devitrification and consolidation of the amorphous Al84Gd6Ni7Co3 powders can be achieved, leading to bulk samples with the desired hybrid microstructure and with excellent room temperature mechanical properties. Beside the sintering temperature, the microstructural state of the starting material is critical in order to obtain bulk samples with the desired microstructure and related properties. Consequently, the variation of the initial structural state of the powders as well as of their thermal stability and phase evolution during heating may be used for further tuning the mechanical performance of the hot pressed Al84Gd6Ni7Co3 samples. In order to analyze this aspect, ball milling was used to vary the crystallization behavior of the gas-atomized Al84Gd6Ni7Co3 glassy powder. The influence of milling on microstructure and thermal stability was investigated as a function of the milling time. The results show that the traces of crystalline phases present in the as-atomized powder decrease gradually with increasing the milling time. The thermal stability of the fcc-Al primary phase increases while the thermal stability of the intermetallic phases decreases with increasing milling. Moreover, significant improvement in hardness occurs after milling, which is attributed to the amorphization of the residual crystalline phases present in the as-atomized powder. These finding demonstrate that milling is an effective way to change the initial structural state of the powders and to control the thermal stability of the material. The effect of the microstructural state of the starting material on the mechanical properties of the consolidated samples was investigated in detail. For this, the milled Al84Gd6Ni7Co3 glassy powders were consolidated into bulk specimens by hot pressing. These materials exhibit superior mechanical properties than the samples produced from the as-atomized powder: record high yield strength of 1.7 GPa and fracture strength exceeding 1.8 GPa. This is combined with a plastic strain of about 4 %, Young’s modulus of 120 GPa and density of 3.75 g/cm3. A bimodal microstructure consisting of coarse grained and fine grained regions was achieved in the hot pressed samples by properly controlling the milling process. The exceptionally high strength is attributed to the increased volume fraction of the fine regions, whereas the plastic deformation is favored by the coarse regions, which are able to hinder crack propagation during loading. In addition, the fracture toughness is also improved by the existence of the coarse regions. The tribological properties of the Al84Gd6Ni7Co3 bulk samples were also evaluated. The wear resistance of the bulk samples produced from the milled powder is enhanced with respect to the specimens fabricated from the as-atomized powder, and both alloys exhibit improved wear properties compared to pure aluminum and Al88Si12. Abrasive wear is the main mechanism for these alloys. Finally, the corrosion resistance of these alloys was studied. The results indicate that the Al84Gd6Ni7Co3 bulk material produced from the as-atomized powder has better corrosion resistance than the samples obtained from the milled powder. The main corrosion behavior for these alloys is pit corrosion, intermetallic particle etchout and the corrosion of the Al-rich inter-particle areas. These results clearly demonstrate that, by the proper selection of the sintering temperature and through the appropriate choice of the initial structural state of the powders, the combined devitrification and consolidation of amorphous precursors can be successfully used to produce bulk amorphous/nanostructured Al-based materials with tunable physical and mechanical properties. This expands the known boundaries of Al alloys and offers a new route for the development of novel and innovative high-performance Al-based materials capable to meet specific requirements.

Die exzellenten Eigenschaften einer Keramik beziehen sich auf den hohen Schmelzpunkt, die gute Hochtemperaturfestigkeit sowie hohe Elastizitätsmodul- und Härtewerte. Weiterhin zeichnen sich die anorganisch-nichtmetallischen Werkstoffebesonders durch ihre gute Korrosions- und Verschleißbeständigkeit aus.Bedingt durch die erschwerte Versetzungsbewegung weisen keramische Werkstoffeeine höhere Sprödigkeit auf. Metallische Werkstoffedagegen sind in der Regel duktil und zeigen meist ein duktiles Bruchverhalten. Lokale Spannungsspitzen können durch plastische Verformung abgebaut werden.Das Ziel dieser Arbeit ist es, das grundsätzlich unterschiedliche Werkstofferhalten einer Keramik und eines Metalls miteinander zu kombinieren, um die Bruchzähigkeit des Keramik-Metall-Verbundwerkstoffes zu erhöhenDie fein verteilten Metalle sollen die Rissausbreitung behindern. Es können unterschiedliche Mechanismen wirken. Im Vergleich zur unverstärkten Keramik ist eine höhere Bruchenergie aufzubringen, um den Riss voran zu treiben. Die Erhöhung der Bruchenergie spiegelt sich in einer höheren Bruchzähigkeit wieder.Um eine duktile Phase in einer spröden Zirkoniumdioxidmatrix zu erzeugen, werden für die Untersuchungen unterschiedliche Metalle eingebracht. Dadurch soll die Bruchzähigkeit als Schadenstoleranz gegenüber dem Totalversagen erhöht werden. Die resultierenden Eigenschaften der Keramik-Metall-Verbundwerkstoffewerden analysiert und charakterisiert.Die Untersuchungen umfassen das pulvermetallurgische Einbringen von metallischen Pulvern mit verschiedenen Teilchengrößen sowie die chemische Einbringung von Präkursoren, die in nanokristalline Metallpartikel umgewandelt werden. Dabei kommen verschiedene Metalle mit unterschiedlichen Wechselwirkungen und Spannungen durch thermische Fehlpassungen in der Matrix zur Anwendung. Zusätzlich wird die Auswirkung der Variation der Verstärkungsform (Partikel/Faser) und des Metallgehaltes untersucht.

Dans le cadre du développement de matériaux de gainage combustible pour les réacteurs à neutrons rapides refroidis au sodium (RNR-Na), cette étude s’intéresse au développement d’un procédé innovant d’élaboration d’aciers renforcés par dispersion d’oxyde (aciers ODS) par mécanosynthèse qui doit éviter l’apparition de précipités de tailles micrométriques indésirables dont la présence dégrade drastiquement les propriétés mécaniques. Ce nouveau procédé consiste à introduire directement des nanoparticules d’oxydes de structure pyrochlore Y2Ti2O7 dans une poudre métallique Fe-Cr via un broyage. Pour cela, un procédé de synthèse des oxydes de structure pyrochlore Y2Ti2O7 par co-broyage des poudres nanométriques Y2O3 et TiO2 a d’abord été mis en place au laboratoire. L’optimisation des conditions de broyage a permis d’obtenir une poudre nanostructurée de nature voulue et de grande pureté. Grâce au produit obtenu, la gamme de fabrication innovante d’aciers ODS proposée a pu être développée puis validé, à petite échelle puis à l’échelle semi-industrielle. Ce nouveau procédé a été utilisé pour étudier l’impact des conditions de broyage et de la composition chimique sur les caractéristiques des matériaux produits, et a permis d’établir le lien entre conditions d’élaboration, microstructure et propriétés mécaniques. Cette étude permet d’abord de valider le mode d’introduction des renforts sous la forme Y2Ti2O7 comme une méthode efficace pour l’obtention d’aciers ODS performants. De plus, elle révèle l’importance des conditions d’élaboration, et en particulier du broyage, sur la microstructure et les propriétés mécaniques des aciers ODS. Les résultats mis en avant ouvrent des perspectives prometteuses en ce qui concerne l’optimisation des conditions d’élaboration des aciers ODS. / This study concerns the development of an innovative manufacturing process for oxidedispersion strengthened steel (hereafter referred to as “ODS”) by mechanosynthesis. As part of materials development for Sodium-cooled Fast Reactors (SFR), the aim is to prevent the growth of undesirable micrometric precipitates which can drastically degrade steel’s mechanical properties. This new process introduces Y2Ti2O7 pyrochlore oxide nanoparticles directly into Fe-Cr metallic powder through mechanical milling. To achieve this, a process has been set up to synthesize Y2Ti2O7 pyrochlore oxides via mechanical alloying of nanosized Y2O3 and TiO2 powders. Optimization of the milling parameters enabled the production of a pure nanostructured powder of the desired nature. Thereafter, the innovative ODS steel manufacturing process was validated on a small and then semiindustrial scale. This new process was used to study the impact of milling parameters and chemical composition on the produced material’s features and enabled the establishment of a link between milling conditions, microstructure and mechanical properties. This study first enables the validation of the method of introducing precipitates in the form of Y2Ti2O7 oxides as an efficient way to obtain competitive ODS steel. Moreover, it reveals the importance of the features of the manufacturing process, particularly milling conditions, on the microstructure and mechanical properties of ODS steel. The results reveal promising perspectives concerning the features of ODS steel manufacturing.

The thesis deals with the high-temperature embrittlement of 14%Cr ODS ferritic steel in liquid lead environment. The 14%Cr ferritic ODS steel ODM401 manufactured by powder metallurgy technology was used as an experimental material. The effect of the long-term annealing, surface corrosion attack in the melt Pb and Pb-Bi on the microstructure and mechanical properties was described. The subsequent microstructural changes were evaluated by means of scanning electron microscopy and transmission electron microscopy The mechanical behaviour of the experimental material was proven by means of microhardness test, impact test and static tensile test. The fractographical evaluation of fracture surfaces were performed on all samples. The surface attack and outstanding microstructural ganges were found after the long-time exposition of the steel in Pb/Pb-Bi melts at temperature 550°C/1000h and 500°C/1000h respectively. The embrittlement of the steel after exposition in Pb/Pb-Bi melts was comparable to the embrittlement after high-temperature annealing of the steel at temperature 650°C/1000h.

The muffle furnace main purpose is to anneal the rough sponge iron powder transported through it, which is done by burning natural gas. Heat is absorbed by the muffle and is transferred to the bed of sponge iron powder. In order to reduce the consumptions of fossil fuel, some companies of the industry aims to exchange the natural gas in their muffle furnace’s burners to syngas, produced from biomass. This will however affect the performance of the furnace in the heating aspect. For this work, it is assumed that the effect will be negative. Thus the aim of this study is to investigate how to compensate the loss of effect from the burners, by examining which other parameters have influence on the furnace heating performance of the sponge iron powder transported through the furnace. The investigation is executed by simulating a 1 meter of the furnace in COMSOL multiphysics for 10 min, not including the combustion chambers. The investigated parameters are the packing degree of the powder, surface emissivity of the muffle, process gas velocity, conveyor belt velocity and the heat transfer rate coefficient to muffle from the combustion chambers. Alas, the process gas velocity and conveyor belt velocity only have minor influence on the final result, according to this simulation. However, the simulation exhibited that the surface emissivity of the muffle and the packing degree of the powder has great impact on the heating of the powder and could compensate some of the lost effect from the burners. This could be obtained by using an unpolished and oxidized muffle surface, and use densely packed powder sample.

No description available.

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.

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.

No description available.