Alloy 617 displays a ductility dip during straining at exactly 1000˚C, leading to brittle fracture. A sudden decrease in ductility appearing during Gleeble hot ductility tests of Ni-based superalloys is a well-known phenomenon, while its cause is unknown. Many mechanisms have been established as possible contributors to the issue, and in later years not one, but the simultaneous presence of several of these mechanisms were confirmed as the cause. The ductility dip leads to solid state cracking and a specific solid state cracking phenomenon known as ductility dip cracking is specifically common in Ni-based superalloys. Ductility dip cracking is identified by intergranular cracks and the occurrence of specific precipitates, among other things. This work investigates the possibility that the decreased ductility is due to ductility dip cracking. Furthermore, other possible explanations are investigated. Visual examination was conducted through LOM, SEM and chemical analysis using EDS technique. Combined with thermodynamic calculations, the existence of Cr-rich M23C6 carbides, Ti(N,C) and Mo-rich particles, most likely M3B2, were confirmed. Further, it is established that the ductility dip is related to the lack of dynamic recrystallization at 1000˚C. It is not confirmed that the ductility dip in alloy 617 is due to ductility dip cracking. / Nickelbaslegeringen 617 uppvisar en minskning i duktilitet under Gleeble-dragprovning vid exakt 1000˚C vilket leder till sprött brott. En plötslig sänkning av duktiliteten vid varmdragning av Ni-baserade superlegeringar är ett välkänt fenomen, dock är orsaken inte fastställd. Många mekanismer har bekräftats som bidrag till problemet och under de senaste åren har den simultana närvaron av fler av dessa mekanismer bekräftats som orsaken. Sänkningen i duktilitet leder till sprickbildning i fast fas och en specifik typ av sprickbildning känd som ”ductility dip cracking” är speciellt förekommande i Ni-bas legeringar. Denna identifieras bland annat genom intergranulära sprickor och närvaron av specifika utskiljningar. Detta arbete undersöker möjligheten att duktilitetssänkningen beror på  ”ductility dip cracking”. Dessutom undersöks fler tänkbara förklaringar. Visuell granskning genomfördes via LOM och SEM och analys av sammansättningar via EDS-analys. I kombination med termodynamiska simuleringar blev förekomsten av Cr-rika M23C6 karbider, Ti(N,C) och Mo-rika partiklar, troligtvis M3B2, bekräftad. Fortsatt är det bekräftat att duktilitetssänkningen är relaterat till avsaknaden av rekristallisation vid 1000˚C. Det är inte bekräftat i detta arbete att duktilitetssänkningen i legering 617 beror av ”ductility dip cracking”.

No description available.

Die für technische Anwendungen attraktivsten Eigenschaften der Hochtemperatur-Supraleiter beruhen auf der Wechselwirkung der Materialien mit einem externen Magnetfeld. Für hochleistungsfähige Supraleiteranwendungen werden großvolumige Funktionselemente mit eindomänigem Magnetisierungsverhalten benötigt. Zur Vergrößerung der magnetischen Domäne schmelztexturierter YBa2Cu3O7-δ-Kompaktsupraleiter wurde anhand der Multi-Seeding-Technik, die Rekristallisation unter Verwendung mehrerer SmBa2Cu3O7-δ-Keimpräparate untersucht. Als Schlüsseltechnologie zur Herstellung anwendungsorientierter Supraleitererzeugnisse wurde zu Beginn der Arbeit die Keimkristallherstellung optimiert. Gemäß den Zielvorgaben stehen zukünftig quasi-einkristalline Keimkörper definierter Form und Orientierung in hoher Stückzahl zur Verfügung. Die Supraleiter betreffend ist es gelungen, für den wechselseitigen Abstand und die Ausrichtung der Keimpräparate ein Optimum zu finden sowie tolerierbare Winkel der Verschwenkung angrenzender Kristalle zu ermitteln. Es wurde festgestellt, dass das Auftreten isolierender Korngrenzeneinschlüsse mit den magnetischen Materialeigenschaften korreliert und vom Keimabstand und der Korngrenzenorientierung abhängig ist. Mit Einsatz von bis zu 16 Keimkristallen gelang es, eindomänige Supraleiterhalbzeuge mit Höchstmaßen von (79 x 39 x 20) mm3 und Remanenzflussdichten von bis zu 1,3 T zu erzeugen. Im Chargenprozess konnten abschließend Multi-Seeding-Funktionselemente mit anwendungskonformen geometrischen und magnetischen Materialeigenschaften zum Aufbau eines hochdynamischen Supraleitermotors reproduzierbar gefertigt werden. In Leistungstests wurde für die Dynamik des Motors mit 200.000 rpm/s ein Rekordwert erzielt – nun können die Motoren in der Anwendung erprobt werden.

No description available.

The present dissertation reports the findings of a study of cracking behavior of a newly developed superalloy, Allvac 718Plus during high power beam welding and post-weld heat treatment. Microstructures of the base alloy, heat affected zone (HAZ) and fusion zone (FZ) of welded and post-weld heat treated (PWHT) coupons were examined by the use of standard metallographic techniques involving optical microscopy, analytical scanning electron microscopy (SEM) and analytical transmission electron microscopy. Moreover, grain boundary segregation behavior of boron atoms during pre-weld heat treatments was evaluated using secondary ion mass spectroscopic system. In the first phase of the research, 718Plus was welded using a low and high heat input CO2 laser to assess its weld cracking response. Detailed examination of the welds by analytical electron microscopic technique revealed the occurrence of cracking in the HAZ of low heat input welds, while their FZ was crack free. However, both the FZ and HAZ of high heat input welds were crack-free. Resolidified constituents were observed along the cracked grain boundaries of the lower heat input welds, which indicated that HAZ cracking in this newly developed superalloy was associated with grain boundary liquation. However, despite a more extensive liquation of grain boundaries and grain interior in the HAZ of high heat input welds, no cracking occurred. This was attributed to the combination of lower welding stresses generated during cooling, and relaxation of these stresses by thick intergranular liquid. Although HAZ cracking was prevented by welding with a high heat input laser, it resulted in a significant damage to the parent microstructure through its extensive liquation. Thus, the use of low heat input welding is desirable. However, this resulted in HAZ cracking which needs to be minimized or eliminated. Therefore, during the second phase of this research, the effects of pre-weld thermal processing on the cracking response of 718Plus were investigated. Results from the quantification of the cracking of the alloy showed that HAZ cracking may be significantly reduced or eliminated through an adequate selection of pre-weld thermal cycle. In the third stage of this research, crack-free welds of 718Plus were post-weld heat treated using standard thermal schedules. A significant solid state cracking of the alloy occurred during the PWHT. The cracking was attributed to the presence of embrittling phases on HAZ grain boundaries, coupled with aging contraction stresses that are generated by a considerable precipitation of gamma prime phase during aging.

The present dissertation reports the findings of a study of cracking behavior of a newly developed superalloy, Allvac 718Plus during high power beam welding and post-weld heat treatment. Microstructures of the base alloy, heat affected zone (HAZ) and fusion zone (FZ) of welded and post-weld heat treated (PWHT) coupons were examined by the use of standard metallographic techniques involving optical microscopy, analytical scanning electron microscopy (SEM) and analytical transmission electron microscopy. Moreover, grain boundary segregation behavior of boron atoms during pre-weld heat treatments was evaluated using secondary ion mass spectroscopic system. In the first phase of the research, 718Plus was welded using a low and high heat input CO2 laser to assess its weld cracking response. Detailed examination of the welds by analytical electron microscopic technique revealed the occurrence of cracking in the HAZ of low heat input welds, while their FZ was crack free. However, both the FZ and HAZ of high heat input welds were crack-free. Resolidified constituents were observed along the cracked grain boundaries of the lower heat input welds, which indicated that HAZ cracking in this newly developed superalloy was associated with grain boundary liquation. However, despite a more extensive liquation of grain boundaries and grain interior in the HAZ of high heat input welds, no cracking occurred. This was attributed to the combination of lower welding stresses generated during cooling, and relaxation of these stresses by thick intergranular liquid. Although HAZ cracking was prevented by welding with a high heat input laser, it resulted in a significant damage to the parent microstructure through its extensive liquation. Thus, the use of low heat input welding is desirable. However, this resulted in HAZ cracking which needs to be minimized or eliminated. Therefore, during the second phase of this research, the effects of pre-weld thermal processing on the cracking response of 718Plus were investigated. Results from the quantification of the cracking of the alloy showed that HAZ cracking may be significantly reduced or eliminated through an adequate selection of pre-weld thermal cycle. In the third stage of this research, crack-free welds of 718Plus were post-weld heat treated using standard thermal schedules. A significant solid state cracking of the alloy occurred during the PWHT. The cracking was attributed to the presence of embrittling phases on HAZ grain boundaries, coupled with aging contraction stresses that are generated by a considerable precipitation of gamma prime phase during aging.

L’intégrité des couches protectrices d’oxyde thermiques se développant à haute température à la surface des matériaux métalliques dépend des niveaux de contraintes générées et de leurs mécanismes de relaxation. Le comportement des films de chromine formés sur les alliages modèles NiCr et Fe47Cr a ici été étudié. Les contraintes résiduelles générées après oxydation des substrats à différentes températures (700°C-1000°C) et durées d’oxydation (3h et 18h) ont été déterminées par spectroscopie Raman. Ces contraintes évoluent avec les conditions d’oxydation de manière monotone (système Ni30Cr/Cr2O3) ou non (système Fe47Cr/Cr2O3). Les variations de déformation à l’échelle du grain ont aussi été suivies par AFM. Pour le premier système, relaxation non destructive par fluage de l’oxyde et délamination sont plus ou moins activées en bon accord avec l’évolution des contraintes résiduelles. Dans le second cas, un mode supplémentaire de relaxation des contraintes par fissuration doit également entrer en jeu. Les propriétés viscoplastiques des couches de chromine formées sur Ni30Cr et Ni28Cr ont pu être caractérisées par diffraction in situ à haute température sur rayonnement Synchrotron, en découplant les effets liés à l’activation thermique de ceux liés à la taille de grain. Le type de fluage intervenant dans la relaxation des contraintes générées dans les couches de chromine a pu être mis en évidence en confrontant les résultats obtenus à un modèle théorique de fluage diffusion. La valeur de l’énergie d’activation associée (130 kJ/mol) a montré, par comparaison avec les données de la littérature, que ce mode non destructeur de relaxation est gouverné par le transport des anions d’oxygène aux joints de grains de l’oxyde. L’ajout d’un élément réactif (Y ou Zr) au substrat Ni28Cr provoque, avec l’augmentation de la quantité introduite, un ralentissement croissant de la cinétique de formation des films de chromine. Cependant, cette quantité introduite ne semble exercer aucun effet significatif sur les niveaux de contraintes résiduelles. A l’échelle microscopique, on constate en général une diminution de la taille des grains avec la présence d’éléments réactifs, une double distribution ayant aussi été observée pour les quantités élevées. Les résultats issus des mesures par diffraction in situ et ceux obtenus par AFM (glissement aux joints de grains de l’oxyde) ont montré que la capacité des films de chromine à relaxer les contraintes grâce à leur comportement viscoplastique pourrait être retardée et/ou diminuée en présence des éléments yttrium et zirconium. Toutefois, ce mécanisme pourrait opérer pour des épaisseurs plus faibles des films de chromine. / Integrity of protective oxide scales developing at the metallic alloys surface at high temperature depends on the stress generation and their relaxation mechanisms. In this work, the behaviour of chromia scales formed on NiCr and Fe47Cr model alloys has been investigated. Raman spectroscopy was used to determine the residual stress level in chromia thin films after oxidation at different temperatures (700°C-1000°C) for 3 h and 18 h. A monotonous evolution of residual stresses with oxidation conditions was noted for the Ni30Cr/Cr2O3 system but not for the Fe47Cr/Cr2O3 one. The strain variations at microscopic scale was also determined by using atomic force microscopy. For the first studied system, non destructive relaxation by creep of the oxide and buckling can be more or less activated, in agreement with the residual stresses evolution. And a third additional stress release mode by intra film cracking could take place for the second system. In situ high temperature oxidation coupled with Synchrotron X-rays diffraction was also used to characterize the viscoplastic properties of chromia scales grown on Ni30Cr and Ni28Cr, with dissociating the effects related to thermal activation and grain size. The creep mechanism responsible of stress release in chromia scales has been evidenced by comparing experimental results with a diffusional creep model. Confrontation of the obtained activation energy (130 kJ.mol-1) with literature results has shown that this non destructive relaxation mode was likely governed by grain boundary transport of oxygen species. When a reactive element (Y or Zr) was added to the metallic substrate Ni28Cr, an important decrease of the oxidation rate was noted when increasing the amount of introduced element. No significant effect of this quantity on the residual stress level was however observed. At microscopic scale, a reduction of grain size has been also noted and two distinguished grains distribution appeared for the higher quantities. Results of in situ Synchrotron diffraction measurements and those of atomic force microscopy (grain boundary sliding) showed that the ability of chromia films to release stress thanks to their viscoplastic properties could be delayed and/or decreased with the presence of an active element. However, this mechanism could operate for smaller chromia films thicknesses.

L'objectif de ce travail est de caractériser et de modéliser le comportement mécanique des oxydes d'uranium (UO2) en situation d'Accident d'Injection de Réactivité (RIA). Les sollicitations vues par le combustible durant un RIA sont caractérisées par de fortes vitesses de déformation (jusqu'à 1/s) et de fortes températures (1000-2500°C). Deux lots de pastilles d'UO2 (de type industriel et à forte densité) ont donc fait l'objet d'une campagne d'essais de compression à vitesses de déplacements imposées (0,1-100 mm/min auxquelles correspondent des vitesses de déformations de 10−4-10−1/s) et à températures régulées (1100-1350-1550-1700°C). Les résultats expérimentaux obtenus (évolution de la géométrie, de la contrainte d'écoulement et de la microstructure) ont permis de définir un modèle de fluage en sinus hyperbolique ainsi qu'un critère de Drucker-Prager avec plasticité associée, modélisant la fragmentation des joints de grain à l'échelle macroscopique. Des simulations Éléments Finis de ces essais et de plus de 200 essais de fluage ont servi à valider la réponse du modèle sur une grande gamme de températures (1100°C-1700°C) et de vitesses de déformation (10−9-10−1/s). Enfin, une loi de comportement dite L3F (Loi Fluage Fissuration Fracturation des joints de grain) a été développée pour l'UO2 en ajoutant, au modèle précédent, le fluage d'irradiation et la fissuration macroscopique en traction. Cette loi a alors été utilisée dans le code crayon combustible ALCYONE-RIA pour simuler, à l'aide d'une modélisation 1,5D, les essais REP-Na effectués dans le réacteur expérimental CABRI. Les résultats de simulation sont en bon accord avec les observations post-essais. / The aim of this work is to characterize and model the mechanical behavior of uranium dioxide (UO2) during a Reactivity Initiated Accident (RIA). The fuel loading during a RIA is characterized by high strain rates (up to 1 /s) and high temperatures (1000°C - 2500°C). Two types of UO2 pellets (commercial and high density) were therefore tested in compression with prescribed displacement rates (0.1 to 100 mm / min corresponding to strain rates of 10-4 - 10-1 /s) and temperatures (1100°C - 1350°C - 1550°C et 1700°C). Experimental results (geometry, yield stress and microstructure) allowed us to define a hyperbolic sine creep law and a Drucker-Prager criterion with associated plasticity, in order to model grain boundaries fragmentation at the macroscopic scale. Finite Element Simulations of these tests and of more than 200 creep tests were used to assess the model response to a wide range of temperatures (1100°C - 1700°C) and strain rates (10-9 /s - 10-1 /s). Finally, a constitutive law called L3F was developed for UO2 by adding to the previous model irradiation creep and tensile macroscopic cracking. The L3F law was then introduced in the 1.5D scheme of the fuel performance code ALCYONE-RIA to simulate the REP-Na tests performed in the experimental reactor CABRI. Simulation results are in good agreement with post tests examinations.

Die für technische Anwendungen attraktivsten Eigenschaften der Hochtemperatur-Supraleiter beruhen auf der Wechselwirkung der Materialien mit einem externen Magnetfeld. Für hochleistungsfähige Supraleiteranwendungen werden großvolumige Funktionselemente mit eindomänigem Magnetisierungsverhalten benötigt. Zur Vergrößerung der magnetischen Domäne schmelztexturierter YBa2Cu3O7-δ-Kompaktsupraleiter wurde anhand der Multi-Seeding-Technik, die Rekristallisation unter Verwendung mehrerer SmBa2Cu3O7-δ-Keimpräparate untersucht. Als Schlüsseltechnologie zur Herstellung anwendungsorientierter Supraleitererzeugnisse wurde zu Beginn der Arbeit die Keimkristallherstellung optimiert. Gemäß den Zielvorgaben stehen zukünftig quasi-einkristalline Keimkörper definierter Form und Orientierung in hoher Stückzahl zur Verfügung. Die Supraleiter betreffend ist es gelungen, für den wechselseitigen Abstand und die Ausrichtung der Keimpräparate ein Optimum zu finden sowie tolerierbare Winkel der Verschwenkung angrenzender Kristalle zu ermitteln. Es wurde festgestellt, dass das Auftreten isolierender Korngrenzeneinschlüsse mit den magnetischen Materialeigenschaften korreliert und vom Keimabstand und der Korngrenzenorientierung abhängig ist. Mit Einsatz von bis zu 16 Keimkristallen gelang es, eindomänige Supraleiterhalbzeuge mit Höchstmaßen von (79 x 39 x 20) mm3 und Remanenzflussdichten von bis zu 1,3 T zu erzeugen. Im Chargenprozess konnten abschließend Multi-Seeding-Funktionselemente mit anwendungskonformen geometrischen und magnetischen Materialeigenschaften zum Aufbau eines hochdynamischen Supraleitermotors reproduzierbar gefertigt werden. In Leistungstests wurde für die Dynamik des Motors mit 200.000 rpm/s ein Rekordwert erzielt – nun können die Motoren in der Anwendung erprobt werden.

Microstructure and micro-mechanical characterization of as-built and heat-treated samples of Hastelloy X produced by laser powder bed fusion (LPBF) process has been carried out in this study. As-built LPBF blocks were solution heat-treated at 1177°C and 1220°C followed by fast cooling. The microstructure of as-built and heat-treated samples were studied by light optical microscopy, scanning electron microscopy, and electron backscatter diffraction. Instrumented indentation micro Vickers testing was performed to obtain microhardness and elastic modulus of asbuilt and heat-treated samples. Microtensile samples from as-built and heat-treated blocks were prepared and polished for mechanical characterization. Microtensile testing inside the scanning electron microscope was performed to evaluate the mechanical properties and to get information about the microstructural changes during plastic deformation. Microstructure characterization revealed disrupted epitaxial grain growth for the as-built samples whereas the two heated-treated Hastelloy X samples exhibited equiaxed grains with varying twin fractions. As-built Hastelloy X samples exhibited higher mean hardness than heat-treated samples. The yield strength of as-built samples reveals higher values as compared to conventional wrought Hastelloy X samples, whereas lower yield strength and higher elongation were observed for heat-treated samples as compared to as-built samples. Higher elongation and lower yield strength values were observed for the samples solution heat-treated at 1220°C compared to the solution heat-treated at 1177°C. Microstructural evaluation at different plastic strains during in-situ microtensile testing reveals a clear difference in dislocation density for as-built and heat-treated samples.