Les aciers renforcés par dispersion d’oxydes (ODS) sont envisagés comme matériaux de gainage pour les réacteurs à neutrons rapides au sodium. Ils présentent de très bonnes propriétés mécaniques, notamment en fluage, du fait de la présence des nano-renforts ainsi qu’une résistance au gonflement élevée de par leur matrice ferrito-martensitique. La gamme de fabrication des ODS ferritiques est complexe et génère une forte texture morphologique et cristallographique. Les microstructures doivent donc être recristallisées mais cette recristallisation est très souvent hétérogène et difficile à maitriser. Cette étude vise à améliorer la compréhension des mécanismes de recristallisation qui dépend fortement du taux de renforts incorporé et de la déformation appliquée. Dans ce but, l’élaboration de nuances modèles avec différents taux de renforts a été réalisée et des caractérisations multi-échelles (EBSD, DNPA, DSC) ont été effectuées. Il est apparu que la nature chimique des nano-oxydes influence fortement la stabilité des microstructures et leur capacité à restaurer après consolidation. Ces travaux ont également permis de mettre en évidence l’étroite relation entre le chemin de déformation à froid, la distribution de l’énergie stockée et la microstructure après recristallisation. Lorsque le traitement thermomécanique est optimal, des microstructures recristallisées homogènes et peu texturées peuvent être obtenues. Il est aussi apparu que la diminution du taux de renforts ne permet pas de faciliter clairement la recristallisation des ODS. Le développement d’un modèle numérique Monte Carlo pour simuler la croissance de grains et la recristallisation en présence de particules a permis d’aider à la compréhension des mécanismes. De plus, une analyse des propriétés en traction des différents états métallurgiques a montré que la recristallisation améliorait nettement la ductilité à chaud sans diminuer significativement les résistances mécaniques. Les résultats obtenus sur matériaux modèles ont permis de mieux comprendre les mécanismes mis en jeu lors de la recristallisation des ODS et d’analyser les gammes de fabrication actuelles des tubes ODS. Diverses optimisations possibles sont discutées à la lumière des résultats obtenus. / Oxide dispersion strengthened steels are considered as cladding materials for Sodium Fast Reactor. Due to the nano-precipitates incorporated within the microstructure, their mechanical properties are very high, especially under creep loading. Moreover, the ferritic-martensitic lattice gives ODS steels a remarkable swelling resistance under radiation. The manufacturing route of ferritic ODS steels is complex and induces a strong morphologic and crystallographic texture. The microstructure needs to be recrystallized but this recrystallization is often heterogeneous and difficult to control. In this framework, this investigation aims at achieving a better understanding of the recrystallization mechanisms in ODS steels that strongly rely both on the nano-oxydes concentration and the applied deformation. Thereby, several model grades with various concentrations of oxydes were elaborated and characterized at different scales (EBSD, SANS, DSC). It appears that the chemical composition of the nano-oxydes strongly influence the microstructure stability and its ability to recover after consolidation. Throughout this study, the strong relationship between the cold-deformation path, the stored energy distribution and the recrystallized microstructure has been highlighted. When the thermo-mechanical treatment is optimal, homogeneous recrystallized microstructures weakly textured can be achieved. Experiments also showed that decreasing the nano-oxydes concentration does not clearly favor recrystallization. Monte Carlo modelling was performed to simulate grain growth and recrystallization in the presence of second phase particles and the simulations helped to identify the mechanisms that occur experimentally. Furthermore, the tensile properties of different metallurgical states were investigated and it came out that the recrystallization notably increases the ductility at high temperature without significantly affecting the yield strength. The results obtained on model materials allowed to achieve a better understanding of the mechanisms implied in the recrystallization process of ODS steels. Several possible optimizations to the current manufacturing route are discussed from the conclusions of this study.

Les alliages ferritiques Fe—14Cr renforcés par une dispersion d'oxydes (ODS) riches en Y, Ti et O sont envisagés comme matériaux de structure pour la prochaine génération de réacteurs nucléaires. Ils allient résistance à l’irradiation neutronique et excellentes propriétés mécaniques, notamment en fluage à hautes températures. Ce travail s'est positionné sur la compréhension des effets induits par de légères variations en oxygène et en yttrium autour d’une composition chimique de référence Fe—14Cr—1W—0,3Ti—0,3Y₂O₃. Nous avons montré que le paramètre crucial est la cinétique de précipitation des nanorenforts. Elle conditionne l’évolution de la microstructure globale que ce soit avant, après filage ou sous traitement thermique. Cette cinétique est propre à la nature des phases précipitant, à leur structure cristallographique et aux relations d'orientations à l'interface particules/matrice. Ce dernier paramètre détermine la stabilité des nanorenforts et par voie de conséquence les mécanismes de recristallisation, et in fine les propriétés mécaniques. La variation des teneurs en oxygène et en yttrium peuvent induire des états consolidés à peu près équivalents en termes de nanodispersion et de propriétés mécaniques bien que les mécanismes inhérents soient différents. Les enrichissements en oxygène et en yttrium conduisent tous les deux à une recristallisation du matériau à 1300°C mais avec des mécanismes radicalement différents. Les résultats de cette étude permettent de proposer des valeurs seuil à ne pas dépasser, 0,3% de Fe₂O₃ et 0,7% d’yttrium, pour conserver de bonnes propriétés mécaniques. / Fe—14Cr ODS ferritic alloys reinforced by a dispersion of oxides rich in Y, Ti and O are considered suitable structural materials structural for the 4th generation of nuclear reactors. They combine neutron irradiation resistance and excellent mechanical properties, especially creep properties at high temperatures. This work is dedicated to the understanding of the effects induced by a small oxygen and yttrium variation around a reference chemical composition: Fe—14Cr—0,3Ti—0,3Y₂O₃. We showed that the crucial parameter is the precipitation kinetic of the nano-reinforcements which is responsible for the microstructure evolution before, after or during the thermal annealing. This kinetic is proper to the nature of the precipitating phases, their structure and to the orientation relationships at the particle/matrix interfaces. This last parameter determines the stability of the nano-reinforcements, hence the recrystallization mechanisms and their mechanical properties. The concentration variation of oxygen and yttrium can induce similar consolidated states in terms od nano-dispersion and mechanical properties even if the underlying mechanisms are different. Both the oxygen and yttrium enrichments lead to a recrystallization of the material at 1300°C by compltetly different mechanisms. This study allows to propose threshold values of 0,3% Fe₂O₃ and 0,7% yttrium, that should not be exceeded in order to maintain the quality of the mechanical properties.

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第18987号 / 工博第4029号 / 新制||工||1620(附属図書館) / 31938 / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 辻 伸泰, 教授 白井 泰治, 教授 松原 英一郎 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM

The present study develops a phenomenological adaptation to an internal state variable (ISV) model that incorporates the influence of dynamic recrystallization (DRX) in a material’s evolving microstructure and flow stress response. During metal forming and joining processes that promote internal heat distributions and large strains, microstructural processes often occur that result in a transformation of the evolving microstructure away from the base distribution. In an effort to lower the stored energy accumulated in the material’s lattice and grain structure, the deformed material may undergo a type of dynamic recovery process, such as DRX. In this study, the ISV model’s flow stress output is modified to include a phenomenological DRX softening and hardening term internal to the isotropic hardening rate ISV. The flow stress thus directly includes the influence of microstructure evolution. The evolving grain size is modeled such that an inverse relation exists between strain hardening and average grain size.

The present study focuses on the evolving microstructure of Mg alloy AZ31. The material is subjected to channel die compression at room temperature to simulate a reduction stage in the rolling process. Samples are annealed to provoke recovery, static recrystallization, and grain growth. Annealing is carried out at three temperatures for times ranging from 10s to 10,000s. The material’s response is exhibited through the use of data collection methods such as microhardness, optical microscopy, and electron backscatter diffraction (EBSD). Methodology behind experimentation and data collection techniques are documented in detail. Conclusions are made about the effects of the compression and annealing processes on the material’s microstructure. The Johnson-Mehl-Avrami-Kolmogorov (JMAK) model is introduced, and a simple recrystallization kinetics plot is attempted.

No description available.

The process optimization of continuous annealing furnace, RHF 125, for recrystallization annealing of two steel grades, Sandvik 13C26 and Sandvik 20C has been carried out. To recreate the continuous annealing process carried out in the roller hearth furnace in the industry, samples with different cold reduction rates were chosen from ongoing production lines. An experimental heat treatment model was chosen by the ‘Design of Experiments’ approach from MODDE (from U-Metrics). The annealing temperature was chosen below the austenitization temperature for both steel grades and soaking time of 30 seconds to 240 seconds were chosen. Microscopic estimation of fraction recrystallized was performed with the help of Electron Back Scattered Diffraction, accompanied by mechanical testing methods to measure the hardness and yield strength of the steel strips. The experimental output was used to create a model to correlate between the different cold reduction rates and annealing parameters to achieve a higher degree of recrystallization along with desirable mechanical properties. Also, a modified Johnson-Mehl-Avrami-Kolomogrov model, based on hardness values, to determine the transformation kinetics by tracking the progress of recrystallization was developed. The model was verified with EBSD measurements for Sandvik 13C26 strip steels. For 20C, inhomogeneous recrystallization was observed, thus limiting the model’s adaptability to steels which exhibit homogeneous recrystallization behavior and negligible change in precipitation and/or coarsening of secondary phases. / Processoptimering av en kontinuerlig glödgningsugn, RHF 125, för rekristallisationsglödgning av två Sandvik-stål, Sandvik 13C26 och Sandvik 20C, har genomförts. För att återskapa den kontinuerliga glödgningsprocessen som utförs den verkilga processen i valdes prover och olika kallreduktionshastigheter från pågående produktionslinjer. En experimentell värmebehandlingsmodell valdes med metoden 'Design of Experiments' med MODDE (från U-Metrics). Glödgningstemperaturen valdes till en temperatur under austeniseringstemperaturen för båda stålen och hålltider varierade från 30 s till 240 s. Mikroskopisk uppskattning av fraktionen rekristalliserat material utfördes med hjälp av Electron Back Scatter Diffraktion (EBSD), åtföljd av mekaniska testmetoder för att mäta hårdheten och sträckgränsen för stålproverna. De experimentella resultaten användes för att skapa en modell för att korrelera mellan de olika reduktionshastigheterna och glödgningsparametrarna för att uppnå högre grad av rekristallisation tillsammans med önskvärda mekaniska egenskaper. Dessutom utvecklades en modifierad Johnson-Mehl-Avrami-Kolomogrov-modell, baserad på hårdhetsvärden, för att bestämma transformationskinetiken genom att spåra evolutionen för rekristallisation. Modellen verifierades genom jämförelse med EBSD-mätningarna för Sandvik 13C26 bandstål. För 20 °C observerades inhomogen rekristallisation, vilket begränsade modellens användbarhet till stål som uppvisade homogent rekristallisationsbeteende och försumbar förändring i utskiljning och/eller förgrovning av sekundära faser.

Extended plasticity mechanisms (EPM) allow a metal to undergo extended plastic deformation without failure. These mechanisms are responsible for the extended plastic deformation characteristic of hot working processes. In this thesis it is shown that electron backscatter diffraction (EBSD) is capable of detecting EPM artifacts in the final microstructure of AISI 304L stainless steel (304L). Results also indicate that dislocation cells form in hot worked AISI 304L stainless steel. Additionally, in this study EBSD data collection and analysis is used with a design of experiments approach to model the presence of EPM artifacts in the final microstructure of friction stir welded 304L. Texture analysis of the welded material reveals a dominant shear deformation texture and a lack of the rotated cube texture. The shear deformation texture is characteristic of dynamic recovery (DRV) and continuous dynamic recrystallization (CDRX), while the rotated cube texture is characteristic of discontinuous dynamic recrystallization (DDRX). The texture analysis results indicate that dynamic recovery (DRV) and continuous dynamic recrystallization (CDRX) play a role in the final microstructure of the welded material, while DDRX does not. Design of experiments was used to find the relationships between the fraction of cell boundaries and spindle speed, travel speed, location in the stir zone, and tool temperature. The regression analyses reported that predicted fraction of cell boundaries were relatively high (approximately 0.70 or more) and changed by less that 20% in the stir zone and 10% in the TMAZ. The relatively high predictions indicate that in FSW 304L DRV dominates and limited CDRX occurs. The small changes in predictions across the experimental space indicate that the effects, while statistically significant, are not practically significant. Finally, an alternate tool temperature basis was developed, which provides a valid method for selecting welds which should have constant tool temperature.

No description available.

The hot working behavior of AISI 1018 steel was studied by hot-compression deformation tests on the Gleeble 1500 thermo-mechanical simulator at true strain values of -0.143 and -0.405, true strain rate values of 0.01 and 0.1, and working temperatures of 900°C and 1000°C. The tests show that a lower working temperature and lower true strain value results in a greater maximum compressive force. The apparent activation energy Qapp was calculated by using the Zener-Hollomon parameter combined with the low stress law. Qapp ­was calculated to be 311 kJ mol-1 K-1.