L’extraction réductrice liquide-liquide est une des voies pyrochimiques les plusprometteuses pour assurer le retraitement des déchets nucléaires. Cette techniqueconsiste à extraire à haute température des éléments initialement en solution dansun sel fondu sur une nappe métallique. Afin d’améliorer les transferts de masse,l’utilisation de forces électromagnétiques permettant de brasser sans contact matérielle coeur des bains et l’interface elle-même a été envisagée.Les cinétiques d’extraction de trois lanthanides (cérium, néodyme et samarium)ont été étudiées expérimentalement. Une étude préalable nous a conduit à travaillersur le couple fluorure de lithium/antimoine et à utiliser le lithium comme agentréducteur. Les investigations réalisées ont démontré que le mécanisme contrôlant lacinétique rapide des transferts est la diffusion des espèces réactives à l’interface.La simulation numérique du réacteur expérimental faisant intervenir de multiplescouplages a également été réalisée. Elle a permis de déterminer les écoulementsturbulents dans chacune des phases. Les transferts de masse simulés ont ensuiteété comparés aux mesures expérimentales. / Reductive extraction is one of the most promising pyroprocess for processing spentnuclear fuel. The extraction of elements from a molten salt to a liquid metal occurs athigh temperature. At the interface between the two immiscible flows mass transfersare ensured via a redox reaction. To increase these transfers, electromagnetic forcescan be used to stir the bulk of both phases and of the interface itself without materialcontact.The kinetic of extraction of three lanthanides (cerium, neodymium and samarium)has been experimentally studied. We worked on lithium fluoride/antimony system,the reducing agent being lithium. Theses experiments show that mass transfers arefast for all studied lanthanides and are controlled by diffusion of reactive species atthe interface.The numerical simulation of experimental reactor which involves many stronglycoupled phenomenon has been performed. Turbulent flows have been computed inboth phases. Mass transfers have then been deduced and compared to experimentalresults.

Ce travail se situé dans la perspective d'un contrôle de la structure de solidification des alliages métalliques sous l'effet de la convection naturelle et forcée afin d'améliorer à terme la maîtrise des microstructures de solidification grâce à un brassage électromagnétique efficace permettant d'avoir une homogénéisation du bain liquide qui par la suite peut améliorer la microstructure finale de l'alliage. La possibilité retenue dans ce travail est de réaliser ce brassage sans contact avec la solution liquide (alliage sous fusion) et sans pollution par d'autres éléments en utilisant un brassage par la force de Lorentz. L'objet de la thèse comporte une étude théorique à la fois expérimentale basée sur une installation expérimentale particulièrement documentée et instrumentée, développée au laboratoire SIMAP/EPM à Grenoble, nommée AFRODITE. Ce dispositif expérimental permet de fournir des données de quantitatives et qualitatives sur le processus de solidification des alliages métalliques. Ces données sont nécessaires à la contribution aux études menées sur la solidification des alliages métallique et enrichir la base des donnée des modèles numériques développés pour prédire les défauts liés à la solidification. L'alliage choisi dans notre travail est l'étain-plomb, vue sa basse température de fusion. Les expériences envisagées visent à étudier l'effet de deux modes de configuration dynamique sur la solidification de l'alliage Sn-Pb: la convection thermosolutale avec la variation de deux paramètres essentiels (la vitesse de refroidissement et la différence de température expérimentale) et la convection forcée par l'utilisation de plusieurs modes de brassage électromagnétique. Cette étude s'intéresse en particulier à la caractérisation des macrostructures et les défauts liés à la macroségrégation. L'originalité de l'étude vise à mesurer in situ les températures instantanées. Ceci nous a permis d'évaluer l'évolution du transfert thermique due à la convection naturelle/forcée, ainsi que leurs influence sur le processus de la solidification sous différents aspects. L'analyse post-mortem de l'alliage métallique, fournit la structure de solidification et la distribution des ségrégations à différentes échelles (mésoscopique et macroscopique). / This work is situated in the context of control of the solidification of metallic alloys structure under the effect of natural and forced convection to enhance control of solidification microstructures term through effective electromagnetic stirring to have a homogenizing the liquid which may subsequently improve the final microstructure of the alloy. The possibility considered in this work is to achieve this stirring without contacting the liquid solution (alloy in fusion) and pollution by other elements using a patch by the Lorentz force. The purpose of the thesis consists both a theoretical and experimental study based on an experimental setup particularly documented and instrumented developed / EPM SIMAP laboratory in Grenoble, named AFRODITE. The experimental device used to provide quantitative and qualitative data on the process of solidification of metallic alloys. These data are necessary for the contribution to studies on the solidification of metallic alloys and enrich the data base developed numerical models to predict defects related to solidification. The alloy selected from our work is tin-lead, for its low melting temperature. The proposed experiments are designed to study the effect of two types of dynamic configuration on the solidification of Sn-Pb alloy: the thermosolutal convection with the variation of two essential parameters (cooling rate and the difference in experimental temperature) and forced convection by the use of several modes of electromagnetic stirring. This study is particularly interested in the characterization of macrostructures and defects related to macrosegregation. The originality of this study is to measure in situ instantaneous temperatures. This allowed us to assess the evolution of the heat transfer due to natural / forced convection and their influence on the process of solidification in different aspects. The post-mortem analysis of the metal alloy provides the solidification structure and distribution of segregation at different scales (mesoscopic and macroscopic).

Ce travail porte sur l'optimisation de la géométrie de chambre réverbérante en s'inspirant du concept de cavité chaotique. Les chambres réverbérantes (RC) sont de plus en plus utilisées comme moyen de test de compatibilité électromagnétique. Elles sont utilisées au-delà d'une fréquence minimale à parti de laquelle les champs sont, dans le volume central de la cavité, statistiquement homogènes et isotropes ; l'obtention de ces propriétés statistiques nécessite l'utilisation d'un mécanisme de brassage, pouvant être mécanique ou électronique. Or, dans les cavités chaotiques, la plupart des modes sont associés à des champs statistiquement homogènes et isotropes, et ceci sans avoir recours à aucun brassage. C'est pourquoi un rapprochement entre chambres réverbérantes et cavités chaotiques a été fait dans ce travail.En premier lieu, nous nous intéressons à des cavités chaotiques 2D obtenues par des modifications successives d'une cavité rectangulaire. Les mesures effectuées dans ces cavités à l'aide d'une théorie perturbative, validées par des résultats de simulation, montrent qu'un champ électrique homogène est obtenu. Les principes retenus pour modifier la géométrie de la cavité rectangulaire seront repris dans les cavités 3D.Les propriétés de trois cavités 3D obtenues en modifiant une cavité parallélépipédique sont étudiées et comparées à celles d'une chambre réverbérante classique munie d'un brasseur de modes. Les modes propres et fréquences de résonance sont déterminés pour ces quatre cavités à l'aide du logiciel HFSS d'Ansoft, tout d'abord en considérant des cavités de géométrie figée, puis en y incluant un brassage mécanique.L'étude de l'homogénéité et de l'isotropie des modes propres montre clairement que les meilleures performances sont obtenues pour une des cavités chaotiques proposées, et ceci quels que soient les critères utilisés.Par ailleurs, il est montré que, dans la chambre réverbérante classique, un grand nombre de modes présente une forte localisation spatiale de l'énergie électrique, alors que ce phénomène ne se produit pas dans la cavité chaotique retenue. Ce phénomène, non détectable par les mesures classiquement effectuées en chambre réverbérante, est dommageable à l'obtention des propriétés d'homogénéité et d'isotropie requises dans le volume de travail.Enfin, l'étude de la distribution des écarts entre fréquences de résonance montre, comme prédit par la Théorie des Matrices Aléatoire, une concordance entre le suivi de la loi asymptotique prévue dans une cavité chaotique et les propriétés d'homogénéité et d'isotropie des champs. Ceci ouvre la voie vers l'utilisation de critères de caractérisation basés sur les fréquences de résonance et non plus uniquement sur les distributions des champs / This work deals with the optimization of the geometry of a reverberation chamber, drawing inspiration from the concept of chaotic cavity. Reverberation chambers, widely used for electromagnetic compatibility tests, are used above a minimal frequency from which the fields are statistically isotropic and uniform; however to respect these properties, a mode stirring process is necessary, that can be mechanical or electronic. As, in chaotic cavities, most modes are isotropic and uniform without the help of any stirring process, we take advantage of the knowledge gained from the studies of chaotic cavities to optimize reverberation chamber behavior.We firstly consider 2D chaotic cavities obtained by modifying a rectangular cavity. Measurements besed on a perturbative approch, and validated by simulations, show uniformly distributed electric fields. Similar geometrical modifications are then proposed in 3D.Three 3D different geometries of cavities obtained from a 3D rectangular cavity are then studied, and their properties are compared with those of a classical reverberation chamber equipped witdh a mode stirrer. Eigenmodes and resonant frequencies are determined numerically using Ansoft HFSS software, first by considering fixed cavity geometries, then by moving the stirrer.Electric field uniformity and isotropy are studied using several criteria; all of them clearly show that the best performances are attained within one of the proposed chaotic cavities.Moreover, a strong energy localization effect appears for numerous modes in the classical reverberation chamber, whereas it is not observed in the proposed 3D chaotic cavity. This effect, never reported in reverberation chamber studies, affects the field uniformity and isotropy within the working volume.The cavities properties are also compared width respect to their eigenfrequency spacing distributions. As predicted by the Random matrix Theory, the best agrement width the asymptotic law associated to chaotic cavities corresponds to the best field properties in terms of uniformity and isotropy. It leads to the proposal of reverberation chamber characterization criteria based on resonant frequencies instead of field distributions

The control of non-metallic inclusions is very important for the improvement of performance during the application of tool steel. This present study was performed to see the effect of changing of some process parameters during the vacuum degassing of the melt and how these changing parameters affects the characteristics of inclusions in tool steel. The main parameters that were changed during the vacuum degassing were the change of induction stirring, argon flow rate from both the plug 1 and 2 and different ladle ages for different heat. Electrolytic extraction method was used to observe the morphology and characteristics of inclusions as a 3 dimensional view in tool steel. Four lollipop samples from four different heats were used for the experiment and all the samples were after vacuum (AV) degassing. In this study four different types of inclusions were found and they are classified as type 1, 2, 3 and 4. Of them type 1 inclusion was the major one with mostly spherical shaped. This study shows that among the three parameters, induction stirring has the biggest effect for the total number of inclusions per volume in the sample than the other two parameters Heat 4A showed the lowest number of inclusions per volume comparing with the other heats. The main reason behind this can be said that the induction stirring was the lowest comparing with the other heats with moderate argon flow and ladle age of 12. Extreme value analysis was used in this study to predict the probability of getting largest size inclusions in a certain volume of the metal. For the prediction of the largest inclusion size, both the electrolytic extraction (3D) and cross-sectional (2D) method was used. Later in this study comparison was done to determine the accuracy of both the methods and it is concluded that for the type 1 inclusions electrolytic extraction method shows almost similar trend with cross-sectional method and electrolytic extraction method shows better accuracy for the prediction of largest size inclusions than the cross-sectional method. Electrolytic Extraction method is also applicable for the prediction of largest size inclusions for multiple types of inclusions.

It is well known that inclusions affect the properties of steels and alloys. Therefore, it is important to understand what type of inclusions that exist and how they behave and especially with a focus on large size inclusions. Thus, the large size non-metallic inclusions in ferroalloy FeTi70R were investigated in two dimensions (2D) by using scanning electron microscopy (SEM) in combination with an energy dispersive technique (EDS). It was found that the FeTi70R ferroalloy contain complex oxide inclusions consisting mostly of CaO, SiO2 and TiOx. Furthermore, experimental trials were performed to investigate how these inclusions behaved when entering a melt. More specifically, a comparison between pure Fe and an Alloy 825 grade were made. These results determined the parameters effect on the transformation of the inclusions in the melt. The large size non-metallic inclusions in Alloy 825 during the ladle treatment were investigated during industrial trials by using both two dimensional (2D) and three dimensional (3D) microscopic investigations. The results showed that inclusions consisted of spherical oxides and clusters made up of oxides and nitrides. Further investigations found that the spherical inclusions were transformed from existing NMI in the FeTi70R ferroalloy and slag particles. As for the clusters, they originate from deoxidation products. Furthermore, small inclusions precipitated in the local zones around the added FeTi70R ferroalloy and titanium nitrides. Investigations also found that only Al2O3-MgO and TiN clusters exist after casting. Industrial trials were performed during the last period of the ladle treatment and using a combined electromagnetic (EMS) and gas (GS) stirring. The purpose to investigate the effect of different EMS directions on the agglomeration and on the removal of Al2O3-MgO and TiN clusters. The investigations were then performed in 3D after an electrolytic extraction of the metal samples. The results show that electromagnetic stirring in the upwards direction is best for the agglomeration of the Al2O3-MgO and TiN clusters. However, electromagnetic stirring in the downwards direction is more effective to remove clusters from the melt. This is in agreement with the theoretical predictions based on Stokes’, Brownian and Turbulent collisions. Also, the calculations showed that for Al2O3-MgO clusters with sizes &lt;20 μm the Turbulent collision is the defining factor for agglomeration. However, both Stokes’ and Turbulent collisions are dominant for larger inclusions. For the TiN clusters, turbulent collisions is the dominant factor. Further investigations with more heats and stirring modes were done by using 2D microscopic investigations. More specifically, the number, size, composition and morphology of different inclusions were determined by using SEM in combination with EDS and Inca Feature analyses. The results show that the EMS in downwards direction with a 0.04 m3 min-1 gas flow rate promotes a general removal of Al2O3-MgO and TiN inclusions. Furthermore, that the upwards EMS direction promotes a drastically increase of inclusions having an equivalent size smaller than 11.2 μm. Moreover, the stirring with a 0.02 m3 min-1 gas flow rate has a better removal rate for both downwards and upwards stirring directions compared to the stirring with a 0.04 m3 min-1 gas flow rate. However, no influence on the inclusion composition and morphology could be seen from the different stirring modes. / Det är välkänt att inneslutningar påverkar egenskaperna i stål och legeringar. Därför är det viktigt att förstå vilken sorts inneslutningar som existerar samt hur de beter sig, särskilt stora inneslutningar. Således undersöktes de stora icke-metalliska inneslutningarna i ferrolegeringen FeTi70R i två dimensioner (2D) genom att använda svepelektronmikroskopi (SEM) i kombination med energidispersionsteknik (EDS). Det visade sig att ferrolegeringen FeTi70R innehåller komplexa oxidinneslutningar bestående huvudsakligen av CaO, Si02 och TiOx. Vidare utfördes laborativa försök för att undersöka hur dessa inneslutningar uppträder när de kommer ner i det smälta stålet. Mer specifikt så gjordes en jämförelse mellan rent Fe och Alloy 825 legeringen. Dessa resultat fastställde hur olika parametrar påverkade inneslutningarnas omvandling i smältan. De stora icke-metalliska inneslutningarna i Alloy 825 legeringen under skänkugnsbehandlingen undersöktes vid industriella försök med hjälp av både tvådimensionella (2D) och tredimensionella (3D) mikroskopiska undersökningar. Resultaten visade att inneslutningarna bestod av sfäriska oxider och kluster uppbyggda av oxider och nitrider. Ytterligare undersökningar visade att de sfäriska inneslutningarna omvandlades från befintliga icke-metalliska inneslutningar i ferrolegeringen FeTi70R och slaggpartiklar. När det gäller kluster härrör de från desoxidationsprodukter. Vidare så bildades små inneslutningar i de lokala zonerna kring den tillsatta FeTi70R legeringen och kring titanitriderna. Undersökningarna fann också att endast Al2O3-MgO och TiN-kluster existerar efter gjutning. De industriella försöken utfördes under den sista perioden av skänkugnsbehandlingen och med en kombinerad elektromagnetisk (EMS) och gas (GS) omröring. Syftet med detta var att undersöka effekten av olika riktningar på EMS omrörningen på agglomerationen och avskiljningen av Al2O3-MgO- och TiN klustren. Undersökningarna utfördes sedan i 3D efter en elektrolytisk extraktion av metallproverna. Resultaten visar att en uppåtriktad elektromagnetisk omröring är bäst för agglomereringen av Al2O3-MgO inneslutningar och TiN kluster. Emellertid så är en nedåtriktad elektromagnetisk omröring effektivare för att avlägsna kluster från smältan. Dessa resultat överensstämmer med de teoretiska förutsägelserna baserade på Stokes, Brownian och Turbulent kollisionsvolymer. Dessutom visade beräkningarna att för Al2O3-MgO kluster med storlekar &lt;20 μm är det turbulenta kollisioner som är den avgörande faktorn för agglomerering. Dock är det både Stokes och de Turbulenta kollisionerna som dominerar för större inneslutningar. För TiN klustren är det de turbulenta kollisionerna som är den dominerande faktorn. Ytterligare undersökningar med fler charger av Alloy 825 och olika omrörningsmetoder gjordes baserade på 2D mikroskopiska undersökningar. Mer specifikt så bestämdes antalet, storleken, sammansättningen och morfologin för olika inneslutningar med användning av SEM i kombination med EDS och Inca Feature analyser. Resultaten visar att en nedåtriktad EMS i kombination med ett gasflöde på 0,04 m3 min-1 främjar ett generellt avlägsnande av Al2O3-MgO och TiN inneslutningar. Vidare främjar den uppåtriktade EMS omrörningen en drastisk ökning av inneslutningar med en ekvivalent storlek av 11,2 μm eller mindre. Vidare har omröringen med ett gasflöde på 0,02 m3 min-1 en bättre avskiljningshastighet för inneslutningar i både nedåt och uppåtgående omrörningsriktningar jämfört med omrörningen med ett gasflöde på 0,04 m3 min-1. Emellertid kunde inget inflytande på sammansättningen och morfologin ses från de olika omrörningssätten. / <p>QC 20171122</p>

It is well known that inclusions affect the properties of steels and alloys. Therefore, it is important to understand what type of inclusions that exist and how they behave and especially with a focus on large size inclusions. Thus, the large size non-metallic inclusions in ferroalloy FeTi70R were investigated in two dimensions (2D) by using scanning electron microscopy (SEM) in combination with an energy dispersive technique (EDS). It was found that the FeTi70R ferroalloy contain complex oxide inclusions consisting mostly of CaO, SiO2 and TiOx. Furthermore, experimental trials were performed to investigate how these inclusions behaved when entering a melt. More specifically, a comparison between pure Fe and an Alloy 825 grade were made. These results determined the parameters effect on the transformation of the inclusions in the melt. The large size non-metallic inclusions in Alloy 825 during the ladle treatment were investigated during industrial trials by using both two dimensional (2D) and three dimensional (3D) microscopic investigations. The results showed that inclusions consisted of spherical oxides and clusters made up of oxides and nitrides. Further investigations found that the spherical inclusions were transformed from existing NMI in the FeTi70R ferroalloy and slag particles. As for the clusters, they originate from deoxidation products. Furthermore, small inclusions precipitated in the local zones around the added FeTi70R ferroalloy and titanium nitrides. Investigations also found that only Al2O3-MgO and TiN clusters exist after casting. Industrial trials were performed during the last period of the ladle treatment and using a combined electromagnetic (EMS) and gas (GS) stirring. The purpose to investigate the effect of different EMS directions on the agglomeration and on the removal of Al2O3-MgO and TiN clusters. The investigations were then performed in 3D after an electrolytic extraction of the metal samples. The results show that electromagnetic stirring in the upwards direction is best for the agglomeration of the Al2O3-MgO and TiN clusters. However, electromagnetic stirring in the downwards direction is more effective to remove clusters from the melt. This is in agreement with the theoretical predictions based on Stokes’, Brownian and Turbulent collisions. Also, the calculations showed that for Al2O3-MgO clusters with sizes &lt;20 μm the Turbulent collision is the defining factor for agglomeration. However, both Stokes’ and Turbulent collisions are dominant for larger inclusions. For the TiN clusters, turbulent collisions is the dominant factor. Further investigations with more heats and stirring modes were done by using 2D microscopic investigations. More specifically, the number, size, composition and morphology of different inclusions were determined by using SEM in combination with EDS and Inca Feature analyses. The results show that the EMS in downwards direction with a 0.04 m3 min-1 gas flow rate promotes a general removal of Al2O3-MgO and TiN inclusions. Furthermore, that the upwards EMS direction promotes a drastically increase of inclusions having an equivalent size smaller than 11.2 μm. Moreover, the stirring with a 0.02 m3 min-1 gas flow rate has a better removal rate for both downwards and upwards stirring directions compared to the stirring with a 0.04 m3 min-1 gas flow rate. However, no influence on the inclusion composition and morphology could be seen from the different stirring modes. / Det är välkänt att inneslutningar påverkar egenskaperna i stål och legeringar. Därför är det viktigt att förstå vilken sorts inneslutningar som existerar samt hur de beter sig, särskilt stora inneslutningar. Således undersöktes de stora icke-metalliska inneslutningarna i ferrolegeringen FeTi70R i två dimensioner (2D) genom att använda svepelektronmikroskopi (SEM) i kombination med energidispersionsteknik (EDS). Det visade sig att ferrolegeringen FeTi70R innehåller komplexa oxidinneslutningar bestående huvudsakligen av CaO, Si02 och TiOx. Vidare utfördes laborativa försök för att undersöka hur dessa inneslutningar uppträder när de kommer ner i det smälta stålet. Mer specifikt så gjordes en jämförelse mellan rent Fe och Alloy 825 legeringen. Dessa resultat fastställde hur olika parametrar påverkade inneslutningarnas omvandling i smältan. De stora icke-metalliska inneslutningarna i Alloy 825 legeringen under skänkugnsbehandlingen undersöktes vid industriella försök med hjälp av både tvådimensionella (2D) och tredimensionella (3D) mikroskopiska undersökningar. Resultaten visade att inneslutningarna bestod av sfäriska oxider och kluster uppbyggda av oxider och nitrider. Ytterligare undersökningar visade att de sfäriska inneslutningarna omvandlades från befintliga icke-metalliska inneslutningar i ferrolegeringen FeTi70R och slaggpartiklar. När det gäller kluster härrör de från desoxidationsprodukter. Vidare så bildades små inneslutningar i de lokala zonerna kring den tillsatta FeTi70R legeringen och kring titanitriderna. Undersökningarna fann också att endast Al2O3-MgO och TiN-kluster existerar efter gjutning. De industriella försöken utfördes under den sista perioden av skänkugnsbehandlingen och med en kombinerad elektromagnetisk (EMS) och gas (GS) omröring. Syftet med detta var att undersöka effekten av olika riktningar på EMS omrörningen på agglomerationen och avskiljningen av Al2O3-MgO- och TiN klustren. Undersökningarna utfördes sedan i 3D efter en elektrolytisk extraktion av metallproverna. Resultaten visar att en uppåtriktad elektromagnetisk omröring är bäst för agglomereringen av Al2O3-MgO inneslutningar och TiN kluster. Emellertid så är en nedåtriktad elektromagnetisk omröring effektivare för att avlägsna kluster från smältan. Dessa resultat överensstämmer med de teoretiska förutsägelserna baserade på Stokes, Brownian och Turbulent kollisionsvolymer. Dessutom visade beräkningarna att för Al2O3-MgO kluster med storlekar &lt;20 μm är det turbulenta kollisioner som är den avgörande faktorn för agglomerering. Dock är det både Stokes och de Turbulenta kollisionerna som dominerar för större inneslutningar. För TiN klustren är det de turbulenta kollisionerna som är den dominerande faktorn. Ytterligare undersökningar med fler charger av Alloy 825 och olika omrörningsmetoder gjordes baserade på 2D mikroskopiska undersökningar. Mer specifikt så bestämdes antalet, storleken, sammansättningen och morfologin för olika inneslutningar med användning av SEM i kombination med EDS och Inca Feature analyser. Resultaten visar att en nedåtriktad EMS i kombination med ett gasflöde på 0,04 m3 min-1 främjar ett generellt avlägsnande av Al2O3-MgO och TiN inneslutningar. Vidare främjar den uppåtriktade EMS omrörningen en drastisk ökning av inneslutningar med en ekvivalent storlek av 11,2 μm eller mindre. Vidare har omröringen med ett gasflöde på 0,02 m3 min-1 en bättre avskiljningshastighet för inneslutningar i både nedåt och uppåtgående omrörningsriktningar jämfört med omrörningen med ett gasflöde på 0,04 m3 min-1. Emellertid kunde inget inflytande på sammansättningen och morfologin ses från de olika omrörningssätten.

Τα κριτήρια σχεδιασμού στις σύγχρονες κατασκευές και κυρίως στην αεροναυπηγική και ναυπηγική βιομηχανία, στοχεύουν στην παραγωγή δομικών στοιχείων με μειωμένο βάρος και χαμηλότερο κόστος, ενώ ταυτόχρονα, απαιτείται να παρουσιάζουν υψηλότερες επιδόσεις και ικανοποιητική δομική ασφάλεια. Οι στόχοι αυτοί έχουν διαμορφώσει μια σχεδιαστική τάση η οποία οδηγεί στην αντικατάσταση των ‘παραδοσιακών’ διαφορικών δομών (differential structures) με ‘σύγχρονες’ ολοκληρωμένες δομές (integral structures). Η τάση αυτή βρίσκει εφαρμογή κατά κύριο λόγο στην αεροναυπηγική, όπου η μείωση του βάρους χωρίς υποβάθμιση της ασφαλούς λειτουργίας αποτελεί βασικό και μόνιμο στόχο. Η αυξημένη παραγωγή δομικών στοιχείων ολοκληρωμένων δομών έχει οδηγήσει σε συνεχή αύξηση της εφαρμογής διεργασιών συνένωσης με έμφαση στις προηγμένες διεργασίες συγκόλλησης. Οι διεργασίας συγκόλλησης οι οποίες, λόγω των πλεονεκτημάτων τους, βρίσκονται στην αιχμή της τεχνολογίας είναι η Συγκόλληση με Τριβή και Ανάμιξη (Friction Stir Welding – FSW) και η Συγκόλληση με Ακτίνα Λέιζερ (Laser Beam Welding – LBW). Η εφαρμογή συγκολλήσεων στην παραγωγή ολοκληρωμένων δομών έχει πολλά τεχνολογικά πλεονεκτήματα έναντι των άλλων τύπων σύνδεσης, ωστόσο, συνοδεύονται από την ανάπτυξη Παραμενουσών Τάσεων και στρεβλώσεων στο τελικό προϊόν, κάτι το οποίο, ανάλογα με την εφαρμογή, μπορεί να προκαλέσει σημαντικά προβλήματα. Συγκεκριμένα, οι στρεβλώσεις επηρεάζουν τη λειτουργικότητα του δομικού στοιχείου, αφού μεταβάλλουν την γεωμετρία του, ενώ οι παραμένουσες τάσεις, αναπροσαρμόζοντας το εσωτερικό εντατικό πεδίο, επιδρούν στη δομική τους ακεραιότητα. Όπως είναι γνωστό με κατάλληλη επιλογή των παραμέτρων της διεργασίας (π.χ. ταχύτητα συγκόλλησης, ισχύς κτλ) μπορεί να επιτευχθεί μείωση των αναπτυσσόμενων παραμενουσών τάσεων και στρεβλώσεων. Επίσης, τα τελευταία χρόνια έχει αποδειχθεί ότι η προσομοίωση μιας διεργασίας συγκόλλησης μπορεί να βοηθήσει σημαντικά στην επιλογή του βέλτιστου συνδυασμού των παραμέτρων της. Για το λόγο αυτό, μεγάλο μέρος της ερευνητικής δραστηριότητας στην περιοχή των προηγμένων διεργασιών συγκόλλησης έχει στραφεί προς την ανάπτυξη αξιόπιστων μεθοδολογιών προσομοίωσης, οι οποίες με δεδομένο (input data) τις παραμέτρους της διεργασίας μπορούν να δώσουν σαν αποτέλεσμα (output data) κρίσιμες απαντήσεις όσον αφορά στις τεχνολογικές ιδιότητες της συγκόλλησης. Βάσει των ανωτέρω, σκοπός της παρούσης διατριβής είναι η ανάπτυξη ολοκληρωμένων μεθόδων θερμομηχανικής προσομοίωσης των προηγμένων διεργασιών συγκόλλησης FSW και LBW με κύριο στόχο την πρόβλεψη των παραμενουσών τάσεων και των στρεβλώσεων καθώς και τη μελέτη της επίδρασης τους στη δομική ακεραιότητα των παραγόμενων δομικών στοιχείων. Ένα από τα σημαντικότερα και ίσως το κρισιμότερο στάδιο κατά την προσομοίωση μιας θερμομηχανικής διεργασίας είναι η εξομοίωση της θερμικής πηγής και ο υπολογισμός του θερμικού φορτίου, γιατί μια εσφαλμένη εκτίμηση του θερμικού φορτίου προκαλεί λανθασμένη πρόβλεψη της θερμοκρασιακής κατανομής και κατά συνέπεια εισάγει σφάλματα στον υπολογισμό των παραμενουσών τάσεων και των στρεβλώσεων. Στη βάση αυτή, τόσο για την περίπτωση της FSW όσο και για την LBW αναπτύχθηκαν μεθοδολογίες για τον προσδιορισμό των θερμικών πηγών τους και συνοδεύτηκαν από θερμικά μοντέλα για την πρόβλεψη του θερμοκρασιακού ιστορικού. Ακολούθως, το θερμοκρασιακό ιστορικό ασκείται υπό τη μορφή εξωτερικού φορτίου σε ένα θερμομηχανικό μοντέλο από όπου υπολογίζονται οι παραμένουσες τάσεις και οι στρεβλώσεις της διεργασίας. Τέλος, η εσωτερική εντατική κατάσταση του συγκολλημένου δομικού στοιχείου συνυπολογίζεται στο εντατικό πεδίο λόγω της φόρτισης λειτουργίας της κατασκευής και γίνεται πρόβλεψη των συντελεστών έντασης τάσης (Stress Intensity Factors - SIFs ) έτσι ώστε να εκτιμηθεί η επίδρασης της συγκόλλησης στη δομική ακεραιότητα. Τόσο το θερμομηχανικό όσο και το θραυστομηχανικό μοντέλο μπορούν να προσαρμοσθούν σε πολλούς διαφορετικούς τύπους σύνδεσης και ρηγμάτωσης, αντίστοιχα. / The design criteria in modern structures aim to the production of components with reduced weight and low cost, as well as, with higher performance and increased safety. The above goals lead to a tendency of replacing traditional differential structures with more modern integral structure, mainly in aeronautic sector where the weight and cost reduction, without decrease of safety, comprises the main target of the current research effort. The production of integral structures requires the adaptation of existing forming processes as well as the development and optimization of advanced welding processes. The most promising welding processes in aeronautics and maritime industries currently are the Friction Stir Welding–FSW and Laser Beam Welding-LBW. Despite of the many technological advantages of FSW and LBW process, their application in the production of integral structures leads to the development of Residual Stress (RS) and distortion fields which can cause significant problems. Specifically, distortions can effect on the components assembly, while, RS affect the structural integrity. However, an appropriate selection of process parameters can significantly reduce the RS and distortions levels. The usual way to optimize process parameters is experimental trial and error approach; recently, process simulation has been proven efficient, too. The present work aims to the development of efficient methodologies for the thermomechanical simulation of FSW and LBW processes in order to predict temperature history, as wells as RS and distortion fields. Consequently, the RS field is used for the determination of the welding effects on the structural integrity of the welded component. Generally, the reliability of a simulation methodology of any thermo-mechanical process, such as welding, is seriously affected by many parameters; two of them are very base, namely, the accurate determination of the heat input introduced to the material (thermal load) and the accurate representation of thermal and mechanical boundary conditions. As the boundary conditions determined by the welder and it is usually easy to transfer in a numerical model, one of the most difficult simulation issues is the appropriate determination of the heat input which will lead to an accurate prediction of the material temperature history. For this reason, one of the main objectives of the present work is to develop methodologies for the accurate thermal load calculation in both FSW and LBW processes. After the validation of the developed methodologies with respect to experimental measurements, the defined heat sources are used in global thermal models in order to predict the temperature histories which, thereinafter, are introduced in the thermo-mechanical models to predict the developed RS and distortion fields. Finally, the structural integrity of the welded component, under the effect of both RS field and service loading is studied; different possible ‘fracture scenarios’ are investigated based on the Stress Intensity Factor concept and the Elastic Fracture Mechanics principles.

La production d’éthanol à partir de biomasse lignocellulosique est reconnue comme une des voies possibles de réduction des émissions de gaz à effet de serre et de remplacement partiel des énergies fossiles. Pour être compétitif, la production d'enzymes à bas coûts est nécessaire. Ces enzymes sont produites par le champignon filamenteux Trichoderma reesei, qui présente, à forte concentration, un comportement fortement rhéofluidifiant pouvant entrainer des limitations de mélange et de transfert de matière lors du changement d'échelle. Dans ce travail, il est proposé de compléter les données de la littérature concernant le temps de mélange, la puissance dissipée et le transfert de matière gaz-liquide (global et local) par des mesures à plusieurs échelles dans des fluides modèles de rhéologie similaire aux milieux biologiques visés. Les modèles et corrélations développés qui en résultent sont directement exploitables pour le design des fermenteurs industriels. Afin d’étudier plus en détail le mélange, le taux de cisaillement et la turbulence, une étude par PIV a été menée sur des milieux transparents. La caractérisation fine de l'hydrodynamique repose sur la dissociation des différentes composantes du mouvement à l’aide de la POD. L'évolution des grandeurs mesurées avec les conditions opératoires permet de fournir des indications précieuses pour l'extrapolation des fermenteurs mettant en œuvre des micro-organismes potentiellement sensibles au cisaillement / Ethanol made from cellulosic biomass is recognized as a promising substitute for fossil fuel and thus as a way to reduce greenhouse gas emissions. To be competitive, low cost cellulosic enzymes produced by the filamentous fungus Trichoderma reesei are required. At high biomass concentration, the culture broth becomes so highly shear-thinning that mixing and mass transfer limitations may be encountered when the process is scaled up.In this study, we propose to complete data available in the literature for mixing times, power draw, and mass transfer (local and global) with measurements at several scales in model fluids (shear thinning) that mimic the rheology of biological media. Models and correlations that derive from this work can be used directly for industrial fermentor design. In order to study mixing, local shear rate and turbulence in detail, PIV is performed in transparent model fluids. The refined hydrodynamic characterisation relies on the dissociation of instantaneous velocity by means of the POD method. The change of key parameters with operating conditions gives relevant information for the scale-up of shear-sensitive micro-organisms.

It is an established fact that segregation during casting affects the physical properties of carbon-based ferro alloys; this motivates the study of the segregation behaviour of carbon and carbide-forming solute elements. In this context, this thesis investigates two different situations: the effects of cooling rate and turbulence on the precipitation behaviour of the graphite nodules in nodular cast iron; the nature of carbide precipitation in a bearing steel grade and the effects of subsequent soaking on these carbides. The structures of boiling water reactor inserts cast by the uphill and downhill casting of nodular cast iron were examined. The samples were taken from representative locations in the top, middle and bottom cross sections of the castings. It was observed that in uphill-cast inserts the nodules were larger but fewer in number the bottom section, whereas in downhill-cast inserts the nodules in the bottom section were smaller, but greater in number. Variation in volume fraction of the graphite nodules across the inserts was also observed. The probable cause of this variation was the difference in cooling rate in different sections of the insert. Between the steel tubes located at the central part of the casting, the fraction of graphite was lower, which could be the result of carburization of the steel tubes. To study the effects of melt stirring during the solidification of nodular cast iron, several experiments were conducted at variable cooling rates and for different stirring times. Examination of the microstructure was conducted using Light Optical Microscope (LOM) and Scanning Electron Microscope (SEM). It was observed that during stirring the melt oxidized and oxide nuclei were formed. The number of nucleation sites for the precipitation of graphite nodules increased, which raised the nodule count and the fraction of the graphite precipitated. The matrix transformed from pearlite to ferrite, which could be due to the fact that more carbon had diffused out of the matrix. The segregation behaviour in hypereutectoid bearing steel produced by ingot casting was also studied. The effects of soaking on micro and macro segregation was investigated in samples taken from as cast and soaked ingots; emphasis was laid on the bulk matrix and A-segregation channels. Samples were also taken from ingots which were soaked and then hot worked. The micro and macro examination of the microstructure was conducted using LOM and SEM. Quantitative and qualitative composition analysis was performed using Energy-dispersive X-ray spectroscopy (EDX) and an electron micro probe analyzer (EMPA). It was observed that M3C, M2C and M6C had precipitated. The carbide morphology in the bulk matrix was different to that in the A-segregation channels. All the primary carbides in the bulk matrix were found to have dissolved after 4 hours of soaking at 1200oC. / Det är ett faktum att segringar som uppstår under gjutning påverkar materialegenskaperna hos kolbaserade järnlegeringar; detta utgör motivationen till studien av segringsuppträdandet hos kol och karbidbildande ämnen. Denna avhandling behandlar två olika aspekter inom ramen för detta ämne: påverkan av kylningshastighet och turbulens på kärnbildningen av grafitnoduler i nodulärt gjutjärn samt karbidbildning i kullagerstål och dess påverkan på den efterföljande värmebehandlingen av dessa karbider. Strukturen hos rör till vattenkokare som tillverkats av nodulärt gjutjärn som gjutits med fyllning från botten eller från toppen undersöktes. Prover togs från representativa tvärsnittspositioner från toppen, mitten och botten av de gjutna ämnena. Resultaten visade att användandet av bottenfyllda kokiller gav upphov till större men färre karbider i nedre delen av ämnet, medans användandet av toppfyllda kokiller gav upphov till mindre men fler karbider i nedre delen av ämnet. Variationer av volymfraktionen av grafitnoduler längs tvärsnitten observerades också. Den mest sannolika orsaken till denna variation var skillnaden i kylhastighet i de olika områdena av tvärsnitten. Hos rör tillverkade av det centrala delen av ämnet så var fraktionen grafit lägre, vilket kan bero på en uppkolning av rören. Ett flertal experiment utfördes med varierande kylningshastigheter och olika omrörningstider för att studera inverkan av omrörning av smältan på stelningen av nodulärt gjutjärn. Studier av mikrostrukturen genomfördes med ljusoptisk mikroskopi och svepelektronmikroskopi. Resultaten visade att smältan oxiderades under omrörningen, vilket resulterade i bildandet av oxider. Detta ledde till en ökning av kärnbildningsområden för grafitnoduler, vilket ledde till en ökning av antalet noduler samt fraktionen av grafit som fälldes ut. Strukturen omvandlades från perlit till ferrit, vilket troligen orsakades av att kol hade diffunderat ut från strukturen. Segringsbeteendet hos hypereutektoida kullagerstål tillverkade genom götgjutning undersöktes också. Effekten av värmebehandling på mikro- och makrosegringar undersöktes i prover tagna från gjutna och värmebehandlade ämnen. Fokus var på att studera strukturen i ämnena samt A-segringar. Dessutom togs prover från ämnen som först värmebehandlats och därefter varmbearbetats. Både mikro- och makroundersökningar av mikrostrukturen utfördes med ljusoptisk mikroskopi och svepelektronmikroskopi. Dessutom så genomfördes kvantitativa sammansättningsbestämningar med energidispersiv röntgenspektroskopi och elektronmikroprobsanalys. Resultaten visade att M3C, M2C och M6C karbider hade fällts ut. Karbidmorfologin i huvuddelen av strukturen skiljde sig från den som återfanns i A-segringar. Samtliga primära karbider i huvuddelen av strukturen hade lösts upp efter 4 timmars värmebehandling vid 1200oC. / <p>QC 20180523</p>

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