Internal fatigue crack propagation in a Ti-6Al-4V alloy: An in situ study

Fatigue specimens of a Ti-6Al-4V alloy containing internal artificial defects with controlled and reproducible size and shape have been produced. These defects systematically led to the initiation of a fatigue crack which propagation has been monitored in situ by synchrotron X-ray tomography during R=0.1 uniaxial fatigue tests at 20 Hz. The crack growth curves of the internal cracks have been obtained for 6 samples. Ex situ fatigue tests have been performed on samples submitted to a supplementary heat treatment or containing a defect put into contact with air. The results obtained tend to support the fact that internal fatigue cracks grow from the notch in a vacuum environment. On the fracture surfaces of samples containing an artificial defect not connected to air, two regions have been observed. They correspond to the Rough Area and the Fish Eye regions observed for internal cracks initiated from natural defects. The transition between those two regions takes place when the plastic radius size is equivalent to the grain size

Consolidation rapide à haute température d'aciers renforcés par dispersion d'oxydes (ODS) : Procédé, microstructure, précipitation, propriétés mécaniques

This work aims to lighten the understanding of the behavior of a class of metallic materials called Oxide-Dispersion Strengthened (ODS) ferritic steels. ODS steels are produced by powder metallurgy with various steps including atomization, mechanical alloying and high-temperature consolidation. The consolidation involves the formation of nanoparticles in the steel and various evolutions of the microstructure of the material that are not fully understood. In this thesis, a novel consolidation technique assisted by electric field called "Spark Plasma Sintering" (SPS) or "Field-Assisted Sintering Technique" (FAST) was assessed. Excellent mechanical properties were obtained by SPS, comparable to those of conventional hot isostatic pressed (HIP) materials but with much shorter processing time. Also, a broad range of microstructures and thus of tensile strength and ductility were obtained by performing SPS on either milled or atomized powder at different temperatures. However, SPS consolidation failed to avoid heterogeneous microstructure composed of ultrafine-grained regions surrounded by micronic grains despite of the rapid consolidation kinetics. A multiscale characterization allowed to understand and model the evolution of this complex microstructure. An analytical evaluation of the contributing mechanisms can explain the appearance of the complex grain structure and its thermal stability during further heat treatments. Inhomogeneous distribution of plastic deformation in the powder is argued to be the major cause of heterogeneous recrystallization and further grain growth during hot consolidation. Even if increasing the solute content of yttrium, titanium and oxygen does not impede abnormal growth, it permits to control the fraction and the size of the retained ultrafine grains, which is a key-factor to tailor the mechanical properties. Since precipitation through grain boundary pinning plays a significant role on grain growth, a careful characterization of the precipitation state was performed on consolidated ODS steels. The experimental data obtained by transmission electron microscopy, small angle neutron scattering and atom-probe tomography evidenced the presence of dense and nanosized particles in SPS ODS steels, similarly to what is observed in conventional ODS steels. This is of great importance since it proves that the precipitation is very rapid and mainly occurs during the heating stage of the consolidation process. Using a thermodynamic model, the precipitation kinetics of Y2O3 and Y2Ti2O7 were successfully reproduced at various consolidation temperatures. Both experimental and numerical findings agree with the rapid precipitation of nanoparticles that are then extremely stable, even at high temperature. Consequently, this model can be an efficient tool to design ODS steelsby the optimization of the precipitation state.Ce travail vise à améliorer la compréhension de la microstructure d’aciers ferritiques appelés aciers ODS. Ils sont fabriqués par métallurgie des poudres, ce qui inclut le cobroyage d’une poudre ferritique avec une fine poudre d’oxydes, suivi d'une consolidation à haute température. La consolidation permet de former un matériau dense renforcé par des particules nanométriques qui sont responsables des bonnes propriétés mécaniques à haute température. Cependant, les procédés conventionnels, notamment la Compaction Isostatique à Chaud, provoquent des microstructures hétérogènes qui étaient jusqu’à ce jour mal comprises. Ainsi, la technique rapide de consolidation assistée par courant électrique appelée "Spark Plasma Sintering" (SPS), a été testée afin d’étudier la microstructure. Pour la première fois, on montre que d’excellentes propriétés mécaniques peuvent être obtenues par SPS, comparables à celles des matériaux ODS obtenus classiquement par Compaction Isostatique à Chaud, mais avec un temps de procédé largement réduit. Cependant, la consolidation par SPS échoue quand il s’agit d’obtenir une micro-structure ferritique homogène. En effet, malgré la cinétique rapide de consolidation, on obtient des grains dits ultrafins (D 10 μm). Une caractérisation microstructurale poussée a permis de comprendre l’évolution du matériau durant la consolidation. Un modèle d’évolution microstructurale a été proposé. Le calcul des pressions gouvernant la mobilité des interfaces souligne l’importance de la déformation plastique hétérogène issue du cobroyage des poudres. Par ailleurs, il est montré que la précipitation des particules d’oxydes ancre les joints de grains et stabilise la microstructure hétérogène, même à très haute température. On montre aussi qu’augmenter la teneur en renforts n’empêche pas la croissance anormale mais permet de contrôler la fraction et la taille de grains ultrafins, et donc les propriétés mécaniques des ODS. Parce que les particules jouent un rôle primordial dans la croissance des grains, une caractérisation fine de l’état de précipitation a été réalisée sur les matériaux consolidés par SPS. L’étude par Microscopie Electronique en Transmission, Diffusion des Neutrons et Sonde Atomique révèle une grande densité d’oxydes qui varient en taille et en composition chimique. Un modèle thermodynamique de type germination/croissance/coalescence a été développé pour simuler les cinétiques de précipitation des phases Y2O3 et Y2Ti2O7 durant les étapes de consolidation non isothermes. Tant les résultats expérimentaux que numériques démontrent la précipitation rapide des nano-particules qui sont ensuite extrêmement stables durant les recuits. Ce modèle permet de mieux comprendre la spécificité des microstructures et de la précipitation dans les ODS, de la formation rapide de particules nanométriques à la précipitation grossière d’oxydes de titane aux interfaces

Dual Beam microfocus high-energy tomography: Towards multimodal and faster laboratory experiments

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Modelling of delta ferrite to austenite phase transformation kinetics in martensitic steels: application to rapid cooling in additive manufacturing

International audienceIn this paper, the high temperature transformation kinetics of delta ferrite to austenite (δ → γ) phase transformation is modeled by thermodynamic and diffusion calculations. It appears that, in martensitic steels, the δ → γ transformation is very fast (a few nanoseconds) as soon as the first austenite nuclei appears. Classically the austenitic phase will thus systematically be observed in the material during conventional elaboration processes. However, in powder metallurgy and additive manufacturing, it is possible to obtain sufficiently high quenching rates (up to 106 °C/s) so that the γ phase does not have time to appear. The calculations presented here allow to rationalize the understanding of the microstructures of powders and different additive manufacturing materials. They enable to understand why ferrite or martensite is sometimes obtained in the final microstructure. From the calculations made, an original CCT (Continuous Cooling Transformations) diagram starting from the δ phase is proposed. It allows to set up a strategy of grade design or process definition according to the final microstructure targeted

Laser Beam Direct Energy Deposition of graded austenitic-to-martensitic steel junctions compared to dissimilar Electron Beam welding

International audienceThis article presents the Direct Metal Deposition (DMD) process as a method to build a graded austenitic-to-martensitic steel. Builds are obtained by varying the ratio of the two powders upon DMD processing. Samples with gradual transitions were successfully obtained thanks to the use of a high dilution rate from a layer to another. Long austenitic grains are observed on 316L side when martensitic grains are observed on Fe-9Cr-1Mo side. In the transition zone, the microstructure is mainly martensitic.Characterizations were performed after building and after a tempering heat treatment at 630°C during 8h and compared to dissimilar Electron Beam welds. Before heat treatment, DMD graded area has high hardness values (around 430 HV) due to fresh martensite formed during building. Tempering heat treatment allows reducing hardness in this area to 300 HV. EDS measurements indicate that the chemical gradient between 316L and Fe-9Cr-1Mo obtained by DMD is smoother than the chemical change obtained in Electron Beam (EB) welds. Microstructures in DMD are quite different from those obtained by EB welding. Hardness measurements in DMD samples and in welds exhibit similar behaviours: the weld metal and the Fe-9Cr-1Mo heat affected zone are relatively hard after welding because of fresh martensite, such as the DMD transition zone. These areas are all softened by the tempering heat treatment

Nitrogen-induced hardening in an austenitic CrFeMnNi high-entropy alloy (HEA)

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Influence of oxide volume fraction on abnormal growth of nanostructured ferritic steels during non-isothermal treatments: An in situ study

International audienceNanostructured ferritic steels were mechanically alloyed with various contents of oxide-forming yttrium and titanium (0, 0.05, 0.3 and 1 wt%). The microstructure evolution of the milled powders during non-isothermal annealing treatments was studied using in situ synchrotron X-ray diffraction. Recrystallization and grain growth were quantified upon heating up to 1100 degrees C, which is the typical consolidation temperature for nanostructured ferritic steels. The temperature where abnormal grain growth occurs is observed to increase with the volume fraction of oxide nanoparticles. This demonstrates the interest of increasing the amount of alloying elements to limit the formation of the bi-modal grain microstructure. Using the nanoscale characterization of the precipitation state, the size of retained ultrafine grains (UFG) in the bimodal microstructure was found to be in agreement with the modified Zener theory demonstrating that the microstructure of ultrafine-grained steels can be tailored by the amount and size of second-phase particle