Les pièces métalliques constituant le circuit primaire des installations nucléaires sont élaborées par forgeage à chaud. Pendant ce procédé, les transformations microstructurales induites par la déformation et les recuits déterminent une partie des propriétés mécaniques des produits finaux. L’orientation de la microstructure lors du processus de fabrication nécessite une connaissance précise des mécanismes physiques qui opèrent dans le matériau. Dans le cas de la déformation à chaud de l’acier austénitique 304L, ces modifications microstructurales dépendent de la recristallisation dynamique discontinue (DDRX) et de la recristallisation post-dynamique (PDRX). L’objet de ce projet est : (i) l’étude de la DDRX et de la PDRX dans les conditions de déformation du procédé de forgeage, (ii) l’étude de l’influence d’un ajout de niobium sur ces mécanismes, (iii) la modélisation de ces mécanismes afin de prédire les caractéristiques de la microstructure (moyenne et distribution de la taille des grains) à l’issue d’un procédé multipasses. Dans le cadre de l’étude, les conditions de déformation rencontrées lors du forgeage à chaud sont reproduites à l’aide d’essais de torsion sur des matériaux modèles contenant des teneurs en niobium différentes. La caractérisation et la modélisation des microstructures a permis de comprendre les effets respectifs de la température, de la vitesse de déformation ainsi que de l’ajout de niobium sur les mécanismes de la DDRX et de la PDRX. Dans cette étude, une nouvelle approche semi-topologique de l’hypothèse champs moyens est développée afin de permettre la prédiction de distributions de la taille de grain cohérentes avec les données expérimentales. / Cooling system of nuclear power plants is constituted of metallic parts obtained by hot forging. Thus during the manufacturing process, the microstructural trans- formations induced by the deformation and annealing process define partially the mechanical properties of the final products. A sharp knowledge of the physical mechanisms generated within the material is required to handle the microstructure. In the case of hot deformation of 304L austenitic stainless steel, the microstructural modifications depend on the discontinuous dynamic recrystallization (DDRX) and the post-dynamic recrystallization (PDRX). The aim of this project is: (i) the study of the DDRX and the PDRX under the conditions of deformation inherent in the forging process, (ii) the study of the influence of niobium addition on these mechanisms, (iii) the modeling of these me- chanisms in order to predict the microstructure characteristics (mean grain size and distribution) following a multipass process. As part of the research, the deformation conditions experienced during the hot forging process are replicated through torsion tests with model materials containing various niobium concentrations. Characterization and modeling of microstructures enable to understand the respective e ects of temperature, strain rate as well as niobium addittion on the DDRX and PDRX mechanisms. In this study, a new topological approach of mean-field hypothesis is developed in order to allow the prediction of realistic grain size distributions.

No description available.

[pt] Sintetizar Bi-2223 por decomposição peritética com posterior recristalização para estudar a cristalinidade e o efeito da fase líquida na formação de amorfo é de suma importância em pesquisas de fitas supercondutoras 1G (1ª geração) de Bi-2223. Tal rota de tratamento de fitas 1G de fase Bi-2223 já foi demonstrada, mas ainda há desafios devido à sua estreita região de estabilidade, lenta formação e a volatilização de chumbo durante a decomposição. No presente trabalho, amostras de (Bi, Pb)-2223 com 6 porcento de fração de PbO (adicionados aos reagentes) foram aquecidas a temperaturas acima da decomposição peritética e resfriadas lentamente. Empregaram-se análises de DTA/TGA, MEV/EDS, DRX e Análise quantitativa (com uso do método de Rietveld, V(I) e R(T). Os resultados mostram que o balanço de fases e a microestrutura dependem da temperatura de decomposição para fita comercial e caseira e da fração de PbO somente para a fita caseira. Uma investigação sistemática por DRX foi realizada, a fim de elucidar tal processo. Foi observada uma recuperação parcial de Bi-2223 nas fitas estudadas e os resultados indicaram que a decomposição e a recristalização da fase Bi-2223, fase amorfa e fases secundárias geraram mudanças na microestrutura e nas propriedades elétricas da fita 1G seja monofilamentar ou multifilamentar. / [en] Synthesize Bi-2223 by peritectic decomposition with subsequent recrystallization to study the crystallinity and the effect of the liquid phase in the formation of amorphous is very important in research of superconducting tapes 1G Bi-2223. Such a route of treatment tapes 1G phase Bi-2223 has been demonstrated, but there are still challenges due to its narrow region of stability, and slow formation of lead volatilization during decomposition. In this work, samples of (Bi, Pb) -2223 with 6 percent PbO fraction (added to the reactants) were heated to temperatures above the peritectic decomposition and cooled slowly. Analyzes were employed DTA / TGA, SEM / EDS and DRX Quantitative analysis (using the Rietveld method, V (I) and R (T). Results show that the balance of phases and microstructure depend on the decomposition temperature for commercial and homemade ribbon and the fraction of PbO only homemade tape. a systematic investigation by DRX was performed in order to elucidate this process. was observed a partial recovery of Bi-2223 and studied the tapes results indicate that the decomposition and recrystallization of the phase Bi-2223 phase amorphous and secondary phases generate changes in microstructure and electrical properties of the tape 1G be monofilament or multifilament.

In this study polycrystalline NiAl has been subjected to torsion deformation. Torsion has been used because of its characteristics. By this deformation mode high shear strains (gamma = 18 in this study) can be imposed on the sample. The deformation conditions are well-defined because of the local deformation mode, which is simple shear. Due to the monoclinic sample symmetry one half of the pole figure is needed in order to obtain the complete texture information, which is more than is needed e.g. by extrusion or rolling. Therefore, texture analysis might be more sensitive with respect to texture components. Furthermore, torsion deformation is characterized by being inhomogeneous in terms of the amount of shear strain and shear strain rate along the sample radius. The shear strain gradient makes the analysis of different stages of deformation on the same sample (i.e. under the same deformation conditions) possible. Another characteristic being special for torsion is that samples change their length, although no axial stress is applied. This effect is known as Swift effect and will be analyzed in detail. The deformation, microstructure and texture development subject to the shear strain are studied by different techniques (Electron Back-Scatter and High Energy Synchrotron Radiation). Beside the development of microstructure and texture with shear strain, the effect of an initial texture as well as the deformation temperature on the development of texture and microstructure constitute an important part of this study. Therefore, samples with three different initial textures were deformed in the temperature range T = 700K – 1300K. The development of the microstructure is characterized by two different regimes depending on the deformation temperature T. For T up to 1000K, continuous dynamic recrystallization (CDRX) takes place. This mechanism leads to the deformation-induced dislocations forming low angle grain boundaries (LAGBs) or being incorporated into them and the successive transformation of these boundaries into high angle grain boundaries (HAGBs) by a further increase of their misorientation. The predictions of this model were compared with the experimental results. The shear stress – shear strain curves are characterized by a peak at low strains, which is followed by softening and a steady state at high strains. This condition is fulfilled for a number of samples, but especially <111> oriented samples do not show a softening stage at low temperatures. Grain refinement takes place for all samples and the average grain size decreases with temperature. The predicted LAGB decrease is in best agreement with the experiments at the lowest temperatures (T = 700K and 800K). Deviations from the model can be explained by the temperature dependence of the grain boundary mobility. For temperatures T > 1000K, discontinuous dynamic recrystallization (DDRX) occurs, by which new grains form by nucleation and subsequent growth. The texture is characterized by two components, {100}<100> (cube, C) and {110}<100> (Goss, G). The intensity of G increases with temperature, while that of C decreases independent of the initial orientation. Both components have their maximum deviated about the 1 axis. The deviation is larger for grains containing the C component and decreases with temperature. Grains containing the G component have the smaller deviation, which decreases with temperature and strain. Texture simulations based on the full constraint Taylor model under the assumption of {110}<100> and {110}<110> slip were done with the experimental <110> and <111> fibres as well as a theoretical <100> fibre and a {100}<100> single orientation (ideal as well as rotated about the torsion axis). The G component is predicted by the simulations and is therefore a deformation texture. However the C component does not appear in the simulation. It therefore must originate by different mechanisms. For the non-<100> oriented samples, possibly nucleation is responsible for the formation of C oriented nuclei. Simulations with single orientations lead to the conclusion, that the ideal C orientation rotates about the 1 axis, while other C orientations, which are rotated about the torsion axis, increasingly converge towards the G component with strain. A single G orientation on the other hand is stable against such a rotation and is therefore the most likely steady state texture. Based on these results it is proposed, that ideally C oriented nuclei rotate until an orientation is reached into which they grow. These new grains are further rotated up to a critical angle, at which a part of them disappears either by adjacent grains or new C oriented nuclei. The recrystallization texture for T > 1000K is most likely the C component as well. Torsional creep of NiAl is characterized by a stress exponent, which depends on temperature and an activation energy, which is stress dependent. A model incorporating both dependencies is proposed and applied to the creep data. It is shown that these equations are able to describe the experimental findings. Thus creep of NiAl based on this model is dominated by non-diffusional processes such as cross slip of <100> screw dislocations for T  1000K. For T > 1000K the stress exponent and the activation energy are in a region, which according to previous reports is rather dominated by dislocation-climb controlled creep. The Swift effect, due to which samples change their axial dimension during torsion without applied axial stress, is observed for NiAl. It is strongly related to the texture development and in the case of NiAl the C component is identified as being responsible for shortening, whereas the G component leads to lengthening as long as it is not aligned with the shear system. Both tendencies can be explained based on the active slip systems. Simulations fail to predict the experimental observation, because the C component is not present. HESR and EBSD were compared with respect to local texture measurements. It was concluded depending on the average grain size HESR has an advantage in terms of grain statistics. For DDRX samples however, both methods are limited. Local texture inhomogeneities can be better detected using EBSD, whereas for an overall local texture information HESR is better suited.

No description available.

The current study focus on investigating a relationship between processing variables and microstructure evolution mechanism in 304L stainless steel subjected to hot torsion. The Gleeble 3800 with Mobile Torsion Unit (MTU) is utilized in the current study to conduct hot torsion test of 304L stainless steel. Samples are rotated at 1100℃ in the shear strain rate range of 0.02s-1 to 4.70s-1 and the shear strain range of 0.5 to 4. Orientation imaging microscopy (OIM) technique is used to collect and analyze the microstructure. At low strains (≤1) and strain rate (0.02s-1), average grain size remains relatively constant, but the lengths of DSs and LABs increase within grains. These are characteristics of the dynamic recovery (DRV). With increasing strain and strain rate, the lengths of DSs, LABs and HABs increase, accompanied by the decrease of average grain size. Subgrains with HAB segments are observed. These are characteristics of continuous dynamic recrystallization (CDRX). At strain rates greater than or equal to 0.94s-1, the fraction of deformation texture is about 3 times higher than that of rotated cube texture. The average grain size increases relative to that at a strain rate of 0.20s-1, accompanied by the increase of twin length per area. This indicates that grain growth take place after CDRX. Sigma phase is not observed in the current study due to the lack of static recrystallization (SRX) and the higher cooling rate.

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”.

В настоящей работе объектом исследования является магнитомягкий аморфный сплав системы Fe-Si-Nb-Cu-Mo-B из группы материалов Finemet. Образец выполнен в виде ленты толщиной 20…30 мкм методом быстрой закалки (спиннингованием). Для определения температурных интервалов фазовых и структурных превращений в исходно аморфном сплаве были использованы методы калориметрии, дилатометрии, терморентгеновского фазового анализа. При скоростях нагрева 0,3…0,5 o/сек установлен температурный диапазон существования данного сплава в нанокристаллическом состоянии. / The research object in that work is magnetically soft amorphous Fe-Si-Nb-Cu-Mo-B alloy. That and same alloy systems was named as Finemet material. The sample is an amorphous ribbon, which has thickness of 20…30 μm, it was producing by melt spinning method. The samples were studied using methods of calorimetry, dilatometry and non-ambient x-ray diffraction analysis. The alloy was heat treated. Data about thermal effects, changes in geometric dimensions, changes in the phase composition, and about critical points are obtained. Interval of nanocrystallic state existence for heating rate 0.3…0.5 o/sec was determined.

Nous avons observé une augmentation ‘’transient’’du taux de cristallisation interfacique de l’a-Si lorsqu’on réimplante du Si à proximité de l’interface amorphe/cristal. Après amorphisation et traitement thermique à 650°C pendant 5s de la couche a-Si crée par implantation ionique, une partie a été réimplantée. Les défauts produits par auto-réimplantation à 0.7MeV se trouvent à (302±9) nm de l’interface initiale. Cela nous a permis d’étudier d’avantage la variation initiale de la vitesse SPE (Épitaxie en phase solide). Avec des recuit identiques de 4h à 500°C, nous avons déterminé les positions successives des interfaces et en déduit les taux de cristallisation SPE. La cristallisation débute à l’interface et continue graduellement vers la surface. Après le premier recuit, (252±11) nm s’est recristallisé dans la zone réimplantée soit un avancement SPE de 1.26x10^18at./cm2. Cette valeur est environ 1.50 fois plus importante que celle dans l’état relaxé. Nous suggérons que la présence de défauts à proximité de l’interface a stimulé la vitesse initiale. Avec le nombre de recuit, l’écart entre les vitesses diminue, les deux régions se cristallisent presque à la même vitesse. Les mesures Raman prises avant le SPE et après chaque recuit ont permis de quantifier l’état de relaxation de l’a-Si et le transfert de l’état dé-relaxé à relaxé. / We observed a ‘’transient’’ increase of planar crystallization rate of a-Si when one reimplanted Si near the interface amorphous / crystal. After amorphization and heat treatment at 650°C for 5s, one part has been re-implanted. The defects produced at 0.7 MeV by self-re-implantation are located at (302±9) nm of the initial interface. This allows us to better study the initial variation of SPE speed (solid phase epitaxy). With recrystallisation anneals at 500±4°C for 4h, we have determined the successive positions of the interfaces and have deduced the SPE recrystallization rate. Crystallization began at the interface and continues gradually to the surface. After the first annealing, (252±11)nm was recrystallized in the re-implanted state. That means 1.26x10^18at./cm2 SPE enhancement. This value is approximately 1.50 times greater than that in the relaxed state. We suggest that the presence of defects near the interface stimulate the speed. Raman measurements taken after each annealing allowed us to know the transfer of the un-relaxed state to the relaxed state. After the number of anneals treatments, both areas progress almost at the same speed / Dans ce travail nous avons étudié le phénomène de diffusion du cuivre et de l’argent dans a-Si en présence de l’hydrogène à la température de la pièce et de recuit. Une couche amorphe de 0.9μm d’épaisseur a été produite par implantation de 28Si+ à 500 keV sur le c-Si (100). Après celle-ci, on procède à l’implantation du Cu et de l’Ag. Un traitement thermique a produit une distribution uniforme des impuretés dans la couche amorphe et la relaxation de défauts substantiels. Certains défauts dans a-Si sont de type lacune peuvent agir comme des pièges pour la mobilité du Cu et de l’Ag. L’hydrogène implanté après traitement thermique sert à dé-piéger les impuretés métalliques dans certaines conditions. Nous n’avons détecté aucune diffusion à la température de la pièce au bout d’un an, par contre un an après à la température de recuit (1h à 450°C) on observe la diffusion de ces métaux. Ce qui impliquerait qu’à la température de la pièce, même si l’hydrogène a dé-piégé les métaux mais ces derniers n’ont pas pu franchir une barrière d’énergie nécessaire pour migrer dans le réseau. / In this work we studied the diffusion phenomenon of copper and silver in a-Si in the presence of hydrogen at room temperature and annealing temperature. The 0.9 μm -thick a-Si layers were formed by ion implantation 28Si + at 500 keV on c-Si (100). After this Cu ions and Ag ions were implanted at 90keV.The heat treatment produces a uniform distribution of impurities in the amorphous layer and the relaxation of substantial defects. Vacancies defects in a-Si can act as traps for the mobility of Cu and Ag. Hydrogen implanted is used to de-trap metal impurities such as Cu and Ag. However we did not detect any diffusion at room temperature during 1 year, but after one year at the annealing temperature (450°C for 1h) we observe the distribution of these metals. Implying that the room at temperature, although the hydrogen de-trapping metals but they could not crossed an energy barrier required to migrate in the network.

PhD thesis focuses the field of textile application of modern functional materials, namely metallic shape memory alloys with unique thermomechanical properties deriving from martensitic transformation in solid state. Particularly, it deals with the development of a nonconventional thermomechanical treatment of thin NiTi filaments via Joule heating by electric current and related basic research involving thermomechanical testing and modeling of functional properties of the filaments, investigation of martensitic transformations and deformation processes in NiTi and investigation of the fast recovery and recrystallization processes in metals heated by short pulses of controlled electric power. The method was developed and called FTMT-EC. In contrast to conventional heat treatment of metallic filaments in environmental furnaces, this method allows for precise control of the raise of the filament temperature and filament stress during the fast heating (rate ~50 000 °C/s). As a consequence, it is possible to precisely control the progress of the fast recovery and recrystallization processes in heat treated filaments. In this way it is possible to prepare filaments with desired nanostructured microstructure and related functional properties. A prototype equipment for application of the method for heat treatment of continuous SMA filaments during respooling in textile processing was designed and built. Comparing to the conventional heat treatment of SMA filaments in tubular environmental furnaces, this approach is faster, saves energy and allows for preparation of filaments with special functional properties. International patent application was filed on the method. It is currently utilized in the research and development of smart textiles for medical applications.