Les aciers ferritiques/martensitiques renforcés par dispersion d’oxydes (ODS) sont envisagés pour le gainage combustible des réacteurs à neutrons rapides à caloporteur sodium de quatrième génération. Les nano-oxydes étant à l’origine de la très bonne tenue en fluage à haute température de ces matériaux, il est nécessaire de s’assurer de leur stabilité pour les conditions extrêmes d’irradiation (jusqu’à 200 dpa) et de température (400-700°C) envisagées en service. Ainsi, l’objectif de ces travaux est d’étudier le comportement de ces nano-renforts sous irradiation. Une approche analytique par des irradiations aux ions in-situ et ex-situ est appliquée aux matériaux ODS Fe18Cr1W0,4Ti +0,3 Y2O3 et Fe18Cr1W0,4Ti + 0.3 MgO. Les résultats obtenus montrent notamment que les nano-renforts Y-Ti-O sont capables de résister à de très fortes doses d’irradiation (237 dpa, 500°C) et également que la cohérence des interfaces oxyde/matrice pourrait jouer un rôle important sur le comportement des renforts sous irradiation (stabilité et recombinaison des défauts ponctuels). / Oxide Dispersion Strengthened (ODS) Ferritic-Martensitic (FM) alloys are expected to play an important role as cladding material in Generation IV sodium fast reactors operating in extreme temperature (400-500°C) and irradiation conditions (up to 200 dpa). Since nano-oxides give ODS steels their high-temperature strength, the stability of these particles is an important issue. The present study evaluate the radiation response of nano-oxides by the use of in-situ and ex-situ ion irradiations performed on both Fe18Cr1W0,4Ti +0,3 Y2O3 and Fe18Cr1W0,4Ti + 0.3 MgO ODS steels. In particular, the results showed that Y-Ti-O nano-oxides are quite stable under very high dose irradiation, namely 237 dpa at 500°C and, that the oxide interfacial structures are likely playing an important role on the behavior under irradiation (oxide stability and point defect recombination).

Les matériaux ODS (Oxide Dispersion Strengthened), mis au point par métallurgie des poudres, sont la solution de référence pour le gainage du combustible nucléaire des nouveaux réacteurs de génération IV à fort taux de combustion. Ils présentent une résistance au gonflement sous irradiation augmentée par rapport aux aciers austénitiques et une grande stabilité dimensionnelle en fluage induite par une dispersion homogène de nano-particules stables à haute température. Après co-broyage de la poudre d'alliage maître avec une poudre d'oxydes d'yttrium, le matériau est consolidé par filage à chaud, puis mis en forme à froid par laminage à pas de pèlerin. Les matériaux ODS sont caractérisés par une faible ductilité et une dureté élevée à température ambiante. Les passes de laminage doivent être entrecoupées par des traitements thermiques intermédiaires afin de restaurer le tube et éviter tout endommagement pendant la gamme de transformation.Cette étude vise à identifier les points clés pour la maîtrise de la gamme de transformation à froid de deux nuances ODS : une nuance ferritique Fe-14Cr-1W et une nuance martensitique Fe-9Cr-1W. Les relations entre les traitements thermomécaniques et la microstructure sont étudiées à partir de caractérisations multi-échelles. La compréhension des mécanismes d'évolution de la microstructure permet de proposer, pour chaque nuance, une gamme de transformation à froid robuste. Pour la nuance ferritique Fe-14Cr-1W, la déformabilité est assurée par une croissance des grains à haute température suivant un mécanisme de type Strain Induced Boundary Migration (SIBM). Des optimisations s'appuyant sur une recristallisation primaire sont envisagées. Pour la nuance martensitique Fe-9Cr-1W, la gamme mise en œuvre permet d'obtenir un matériau dont la déformabilité et les caractéristiques mécaniques à chaud sont équivalentes voire meilleures que celles des nuances de la littérature. Des évolutions des gammes et de la composition chimique sont proposées pour améliorer la résistance à la corrosion et au fluage. / Oxide dispersion strengthened steels, elaborated by powder metallurgy, are considered as reference materials for high burn up cladding tubes for future Sodium Cooled Fast reactors. They present superior radiation resistance compared with austenitic steels and high creep strength due to reinforcement by the homogeneous dispersion of hard nano-sized particles. After mechanical alloying of the matrix powder and the yttrium oxides, ODS steels are consolidated by hot extrusion and manufactured by using cold pilgerin process. ODS steels are usually characterized by a low ductility and a high hardness at room temperature. The cold-rolling passes have to be punctuated by intermediate heat treatments in order to soften the raw tube and avoid any damage in the course of manufacturing.The aim of this study is to identify the key points for the control of the manufacturing of two grades: a Fe-14Cr-1W ferritic grade and a Fe-9Cr-1W martensitic grade. The relationship between thermomechanical treatments and microstructure is studied by multi-scale characterizations. The understanding of the microstructure evolution permits the determination of robust fabrication routes for both grades. The deformability of the ODS Fe-14Cr-1W ferritic grade is ensured by grain growth at high temperature following a Strain Induced Boundary Migration (SIBM) mechanism. Optimizations through primary recrystallization are proposed. Fabrication route of ODS Fe-9Cr-1W martensitic grade permits to obtain a material characterized by deformability and high temperature mechanical properties similar or even better than those of literature grades. Fabrication routes evolutions and chemical composition optimization are proposed to improve the corrosion and thermal creep resistance.

O crescente interesse em novos métodos para a geração de energia limpa e sustentável contribui para o desenvolvimento de materiais avançados destinados a aplicações estruturais em reatores de fusão nuclear. Os principais resultados obtidos quanto à caracterização microestrutural de dois aços endurecidos por dispersão de óxidos, candidatos potenciais a este tipo de aplicação, são apresentados. Um dos aços contém 9%Cr e o outro 13%Cr (% em massa). Os aços foram laminados até 80% de redução e recozidos até temperaturas próximas a 0,9 Tf, onde Tf é o ponto de fusão. A cinética de amolecimento foi acompanhada por meio de medidas de dureza Vickers em função da temperatura de recozimento e do tempo. Amostras representativas foram caracterizadas via microscopia eletrônica de transmissão e de varredura e por difração de elétrons retroespalhados. As temperaturas das transformações de fases foram determinadas por técnicas como dilatometria e análise térmica diferencial. Curvas de magnetização em função do campo magnético aplicado até 15 kOe foram obtidas para o aço com 9%Cr. Medidas de difração de raios X para determinar a densidade de discordâncias também foram realizadas em amostras representativas do aço com 9%Cr. Os resultados até o momento mostram que o engrossamento microestrutural destes aços só se torna significativo quando o recozimento é feito em temperaturas acima de 0,8 Tf. Em temperaturas mais baixas, ainda no campo ferrítico, a recuperação prevalece e a fração recristalizada é baixa. A resistência destes materiais à recristalização se deve à presença das partículas de óxido de ítrio dispersas na matriz que dificultam a movimentação e o rearranjo das discordâncias e contornos durante sua migração. Por outro lado, partículas grosseiras como as dos carbonetos M23C6 estimulam a recristalização atuando como sítios preferenciais para a nucleação. O recozimento em temperaturas elevadas no campo austenítico resultou no aumento considerável na dureza Vickers e na densidade de discordâncias para o aço com 9%Cr devido à transformação martensítica. No aço com 13%Cr os resultados também sugerem a ocorrência da transformação martensítica. / There is an increasing interest in the development of new, sustainable, clean and safe sources of energy. In view of these requirements, the development of advanced materials for future nuclear fusion reactors becomes essential. This work investigates the annealing behavior and the microstructural stability of two oxide dispersion strengthened steels with 9%Cr and 13%Cr ODS steels. These materials are potential candidates for structural applications in future fusion reactors. The two ODS steels were cold rolled to 80% thickness reduction. Samples were annealed in vacuum at temperatures of about 0.9 Tm, where Tm is the melting point. The microstructural characterization was performed by Vickers hardness testing, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) performed by a highresolution SEM. Important temperatures related to the phase transformations were determined with aid of dilatometry and differential thermal analysis (DTA). Magnetization curves as a function of applied magnetic fields up to 15 kOe were obtained for 9%Cr ODSEurofer. X-ray diffraction experiments were also performed on 9%Cr steel to evaluate the dislocation density in several metallurgical conditions. Results show that microstructural coarsening becomes significant when annealing is performed above 0.8 Tm. Below 800°C, static recovery is the main softening mechanism of these steels and the volume fraction of recrystallized grains is quite low. The resistance of these steels to recrystallization can be explained by the strong interaction between boundaries and mobile dislocations with fine particles of Y-based oxides. Contrastingly, coarse M23C6 particles act as preferential nucleation sites through the well-known particle stimulated nucleation (PSN) mechanism. Samples annealed above 800oC (austenitic phase field) display larger dislocation densities in the 9%Cr ODS steel. Results concerning to 13%Cr steel suggest the occurrence of martensitic transformation.

O crescente interesse em novos métodos para a geração de energia limpa e sustentável contribui para o desenvolvimento de materiais avançados destinados a aplicações estruturais em reatores de fusão nuclear. Os principais resultados obtidos quanto à caracterização microestrutural de dois aços endurecidos por dispersão de óxidos, candidatos potenciais a este tipo de aplicação, são apresentados. Um dos aços contém 9%Cr e o outro 13%Cr (% em massa). Os aços foram laminados até 80% de redução e recozidos até temperaturas próximas a 0,9 Tf, onde Tf é o ponto de fusão. A cinética de amolecimento foi acompanhada por meio de medidas de dureza Vickers em função da temperatura de recozimento e do tempo. Amostras representativas foram caracterizadas via microscopia eletrônica de transmissão e de varredura e por difração de elétrons retroespalhados. As temperaturas das transformações de fases foram determinadas por técnicas como dilatometria e análise térmica diferencial. Curvas de magnetização em função do campo magnético aplicado até 15 kOe foram obtidas para o aço com 9%Cr. Medidas de difração de raios X para determinar a densidade de discordâncias também foram realizadas em amostras representativas do aço com 9%Cr. Os resultados até o momento mostram que o engrossamento microestrutural destes aços só se torna significativo quando o recozimento é feito em temperaturas acima de 0,8 Tf. Em temperaturas mais baixas, ainda no campo ferrítico, a recuperação prevalece e a fração recristalizada é baixa. A resistência destes materiais à recristalização se deve à presença das partículas de óxido de ítrio dispersas na matriz que dificultam a movimentação e o rearranjo das discordâncias e contornos durante sua migração. Por outro lado, partículas grosseiras como as dos carbonetos M23C6 estimulam a recristalização atuando como sítios preferenciais para a nucleação. O recozimento em temperaturas elevadas no campo austenítico resultou no aumento considerável na dureza Vickers e na densidade de discordâncias para o aço com 9%Cr devido à transformação martensítica. No aço com 13%Cr os resultados também sugerem a ocorrência da transformação martensítica. / There is an increasing interest in the development of new, sustainable, clean and safe sources of energy. In view of these requirements, the development of advanced materials for future nuclear fusion reactors becomes essential. This work investigates the annealing behavior and the microstructural stability of two oxide dispersion strengthened steels with 9%Cr and 13%Cr ODS steels. These materials are potential candidates for structural applications in future fusion reactors. The two ODS steels were cold rolled to 80% thickness reduction. Samples were annealed in vacuum at temperatures of about 0.9 Tm, where Tm is the melting point. The microstructural characterization was performed by Vickers hardness testing, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) performed by a highresolution SEM. Important temperatures related to the phase transformations were determined with aid of dilatometry and differential thermal analysis (DTA). Magnetization curves as a function of applied magnetic fields up to 15 kOe were obtained for 9%Cr ODSEurofer. X-ray diffraction experiments were also performed on 9%Cr steel to evaluate the dislocation density in several metallurgical conditions. Results show that microstructural coarsening becomes significant when annealing is performed above 0.8 Tm. Below 800°C, static recovery is the main softening mechanism of these steels and the volume fraction of recrystallized grains is quite low. The resistance of these steels to recrystallization can be explained by the strong interaction between boundaries and mobile dislocations with fine particles of Y-based oxides. Contrastingly, coarse M23C6 particles act as preferential nucleation sites through the well-known particle stimulated nucleation (PSN) mechanism. Samples annealed above 800oC (austenitic phase field) display larger dislocation densities in the 9%Cr ODS steel. Results concerning to 13%Cr steel suggest the occurrence of martensitic transformation.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / A necessidade de redução da emissão de poluentes, visando diminuir os sérios problemas de poluição atmosférica enfrentados atualmente, é hoje uma das principais preocupações mundiais, provocando o surgimento de leis mais rígidas, que restringem o teor de enxofre na gasolina e no diesel. Assim, o desenvolvimento de tecnologias mais eficazes na remoção de enxofre nestes combustíveis tem recebido atenção crescente. Estas tecnologias incluem a extração física com solvente, a adsorção seletiva, processos de redução/oxidação microbiológicos e a dessulfurização oxidativa (ODS). A dessulfurização oxidativa converte os compostos de enxofre em sulfonas que podem ser facilmente separadas por processos físicos. Portanto, a ODS apresenta grande potencial para tornar-se um processo complementar a processo de hidrodessulfurização tradicional na produção de combustíveis altamente dessulfurizados. Neste contexto, este trabalho visou o estudo do desempenho de catalisadores de V2O5 suportados em alumina, sílica e sílica-alumina frente à reação de ODS do dibenzotiofeno em presença do peróxido de hidrogênio, como oxidante, e da acetonitrila, como solvente polar aprótico. Os catalisadores foram preparados por impregnação ao ponto úmido e caracterizados por difração de raios-X (DRX), análise textural, redução à temperatura programada (TPR-H2), dessorção de amônia à temperatura programa (TPD-NH3) e espectroscopia Raman. O efeito de parâmetros reacionais como quantidade de solvente, relação O/S e concentração de catalisador foram investigados, utilizando a alumina como suporte, visando estabelecer as condições reacionais que levassem a maiores valores de conversão do dibenzotiofeno (DBT). Uma vez estabelecidas estas condições, foi analisado o efeito do teor de V2O5 presente no catalisador e, posteriormente, o efeito do suporte catalítico. Os resultados obtidos mostraram a 70 C razão molar H2O2/Sde 16,6, razão carga/solvente igual a 1:1 e 100 mg do catalisador 15 % V2O5/SiO2, a conversão obtida foi de 95% / The need to reduce the gaseous emissions which causes serious environmental problems is a worldwide concern nowadays. Therefore, stricter laws aiming at to reduce the sulfur content in gasoline and diesel are being adopted in different countries, among them Brazil. Thus, the development of more efficient technologies to remove sulfur in these fuels has received increasing attention. These technologies include the physical extraction with a solvent, selective adsorption, microbiological reduction/oxidation processes and oxidative desulphurization (ODS). The oxidative desulfurization (ODS) converts sulfur compounds into sulfones that can be easily separated by physical processes. Therefore, the ODS has a great potential to become a process complementary to traditional hydrodesulfurization in the production of highly desulfurized fuels. In this context, this work studied the performance of V2O5 catalysts supported on alumina, silica and silica-alumina toward ODS reaction of dibenzothiophene in the presence of hydrogen peroxide as the oxidant, and acetonitrile as polar aprotic solvent. The catalysts were prepared by incipient wetness impregnation and characterized by X-ray diffraction (XRD), textural analysis, temperature programmed reduction (TPR-H2), temperature programmed desorption (TPD-NH3) and Raman spectroscopy. The effect of experimental parameters such as amount of solvent, O/S ratio and catalyst concentration were investigated, using alumina as a support, aiming at establishing the conditions that could lead to the higher conversion of dibenzothiophene (DBT). Once established these conditions, the effect of V2O5 content was investigated and then the effect of catalytic support. The results showed that at 70 C, H2O2/S molar ratio of 16.6, solvent/diesel ratio equal to 1: 1 and 100 mg of 15% V2O5/SiO2 catalyst, the conversion obtained was 95%

Les aciers renforcés par une dispersion d’oxydes nanométriques (ODS : Oxide Dispersion Strengthened) sont connus pour leur bonne tenue en fluage à haute température et pour leur bonne résistance au gonflement sous irradiation. Ils sont envisagés comme matériaux potentiels pour le gainage combustible des réacteurs de quatrième génération (Réacteur à Neutrons Rapides refroidis au Sodium). Les aciers ferritiques ODS, généralement élaborés par filage à chaud, possèdent une microstructure complexe (texture morphologique et cristallographique, fine précipitation, forte densité de dislocations, différentes tailles de grains) rendant la compréhension de la relation entre la microstructure et les propriétés mécaniques délicate. Le travail de cette thèse a consisté à caractériser et à modéliser l’effet des différents composants de la microstructure sur le comportement mécanique d’aciers ferritiques Fe-14Cr ODS, ainsi que d’affiner la compréhension de leurs mécanismes de déformation. Pour cela, des matériaux modèles ont été élaborés par compaction isostatique à chaud puis caractérisés, dans lesquels les différents paramètres microstructuraux ont été variés de manière contrôlée. Leur microstructure a été déterminée à l’aide de diverses techniques de caractérisation avancées (MEB-EBSD, MET, DXPA, microsonde de Castaing, …). Ces différentes nuances ont été testées en traction sur une large gamme de température et en fluage à 650°C et 700°C. Les résultats ont mis en évidence l’effet de la taille et la fraction des oxydes, de la structure de grains, et de la présence du Titane, et ont servi de base pour proposer une modélisation. Des essais de déformation in situ au MET ainsi que des essais de traction à chaud avec mesure des champs de déformation locaux ont permis de mettre en évidence une transition entre mouvement saccadé de dislocations à basse température, et mécanismes de déformation à chaud, intragranulaires (vieillissement dynamique, mouvement de dislocations continu) et intergranulaires. A haute température, un fort endommagement au niveau des joints de grains est observé. / Oxide dispersion strengthened (ODS) ferritic steels are known for their good resistance both to high temperature creep and to swelling under irradiation. They are considered as potential materials for fuel cladding for the next generation of nuclear reactors (Sodium-cooled Fast Reactor). These materials, usually processed by hot extrusion, exhibit a complex microstructure (crystallographic and grain texture, nanometer precipitation, high dislocation density, poly-dispersed grain size), making it a real challenge to establish the microstructure / properties relationships. This thesis has aimed at characterizing and modeling the effect of the different components of the microstructure on the mechanical properties of ferritic Fe-14Cr ODS steels, as well as to improve the understanding of their deformation mechanisms. For this purpose, model materials have been elaborated by hot isostatic pressing and characterized, where the different microstructural parameters have been varied in a controlled manner. Their microstructure have been determined using a set of advanced characterization techniques (SEM-EBSD, TEM, SAXS, EPMA, …). These different materials have been tensile tested over a wide temperature range and creep tested at 650 and 700°C. The results have evidenced the effect of the size and fraction of oxide particles, of the grain size and of the presence of Ti, and have made it possible to model the mechanical behavior. In-situ tensile tests in the SEM, as well as strain field measurements during high temperature testing, have evidenced a transition between a jerky movement of dislocations at low temperature and the high temperature mechanisms, whether intra-granular (dynamic strain ageing, continuous dislocation movement) or inter-granular. At high temperature, severe damage is observed at the grain boundaries.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / A necessidade de redução da emissão de poluentes, visando diminuir os sérios problemas de poluição atmosférica enfrentados atualmente, é hoje uma das principais preocupações mundiais, provocando o surgimento de leis mais rígidas, que restringem o teor de enxofre na gasolina e no diesel. Assim, o desenvolvimento de tecnologias mais eficazes na remoção de enxofre nestes combustíveis tem recebido atenção crescente. Estas tecnologias incluem a extração física com solvente, a adsorção seletiva, processos de redução/oxidação microbiológicos e a dessulfurização oxidativa (ODS). A dessulfurização oxidativa converte os compostos de enxofre em sulfonas que podem ser facilmente separadas por processos físicos. Portanto, a ODS apresenta grande potencial para tornar-se um processo complementar a processo de hidrodessulfurização tradicional na produção de combustíveis altamente dessulfurizados. Neste contexto, este trabalho visou o estudo do desempenho de catalisadores de V2O5 suportados em alumina, sílica e sílica-alumina frente à reação de ODS do dibenzotiofeno em presença do peróxido de hidrogênio, como oxidante, e da acetonitrila, como solvente polar aprótico. Os catalisadores foram preparados por impregnação ao ponto úmido e caracterizados por difração de raios-X (DRX), análise textural, redução à temperatura programada (TPR-H2), dessorção de amônia à temperatura programa (TPD-NH3) e espectroscopia Raman. O efeito de parâmetros reacionais como quantidade de solvente, relação O/S e concentração de catalisador foram investigados, utilizando a alumina como suporte, visando estabelecer as condições reacionais que levassem a maiores valores de conversão do dibenzotiofeno (DBT). Uma vez estabelecidas estas condições, foi analisado o efeito do teor de V2O5 presente no catalisador e, posteriormente, o efeito do suporte catalítico. Os resultados obtidos mostraram a 70 C razão molar H2O2/Sde 16,6, razão carga/solvente igual a 1:1 e 100 mg do catalisador 15 % V2O5/SiO2, a conversão obtida foi de 95% / The need to reduce the gaseous emissions which causes serious environmental problems is a worldwide concern nowadays. Therefore, stricter laws aiming at to reduce the sulfur content in gasoline and diesel are being adopted in different countries, among them Brazil. Thus, the development of more efficient technologies to remove sulfur in these fuels has received increasing attention. These technologies include the physical extraction with a solvent, selective adsorption, microbiological reduction/oxidation processes and oxidative desulphurization (ODS). The oxidative desulfurization (ODS) converts sulfur compounds into sulfones that can be easily separated by physical processes. Therefore, the ODS has a great potential to become a process complementary to traditional hydrodesulfurization in the production of highly desulfurized fuels. In this context, this work studied the performance of V2O5 catalysts supported on alumina, silica and silica-alumina toward ODS reaction of dibenzothiophene in the presence of hydrogen peroxide as the oxidant, and acetonitrile as polar aprotic solvent. The catalysts were prepared by incipient wetness impregnation and characterized by X-ray diffraction (XRD), textural analysis, temperature programmed reduction (TPR-H2), temperature programmed desorption (TPD-NH3) and Raman spectroscopy. The effect of experimental parameters such as amount of solvent, O/S ratio and catalyst concentration were investigated, using alumina as a support, aiming at establishing the conditions that could lead to the higher conversion of dibenzothiophene (DBT). Once established these conditions, the effect of V2O5 content was investigated and then the effect of catalytic support. The results showed that at 70 C, H2O2/S molar ratio of 16.6, solvent/diesel ratio equal to 1: 1 and 100 mg of 15% V2O5/SiO2 catalyst, the conversion obtained was 95%

Les travaux présentés dans ce manuscrit sont consacrés à l'étudie du un petit instrument sophistiqué de mesure d'épaisseur optique : ODS (Optical Depth Sensor) a été conçu pour étudier l'atmosphère martienne et terrestre. L'une de ses principales missions consiste à fournir des mesures journalières de l'épaisseur optique des aérosols (AOD: Aerosol Optical Depth) et de détecter et caractériser les nuages optiquement minces à l'aube et au crépuscule. Les méthodes d'analyses sont basées sur l'utilisation de tables d'intensité reproduisant les signaux observés ODS en fonction de différents paramètres clés. Ces tables ont été réalisées à l'aide d'un code de transfert radiatif dans une géométrie en plans parallèles pour l'estimation de l'opacité des poussières, tandis que les propriétés des nuages sont issues d'un modèle de type Monte-Carlo en géométrie sphérique. Le premier objectif de ce travail a consisté à développer les algorithmes d'analyses nécessaires à l'étude du signal d'ODS. / The work presented in this manuscript is devoted to the development of reliable retrieval procedures for a lightweight and sophisticated optical depth sensor (ODS) which measures alternatively scattered flux at zenith and the sum of the direct flux and the scattered flux in the blue and red wavelength ranges. The ODS sensor is dedicated to Mars and Earth atmosphere and its principal goals are perform measurements of the daily mean aerosol optical depth (AOD) and retrieve the altitude and optical depth of high altitude clouds at twilight. The retrieval procedure is based on the use of look-up tables of intensities reproducing the signals that should be observed by ODS, as a function of different key parameters. For the estimation of AOD, the look-up tables are obtained by using a plane-parallel radiative transfer code, while for the study of cloud properties a Monte-Carlo radiative transfer code in spherical geometry is used.

The main objective of present diploma thesis is to prepare three different classes of steels, differing by their content of chromium: 9Cr, 14Cr, 17Cr steels and their oxide dispersion strengthened variants. Steels were prepared from atomic and pre-alloyed powders by the mechanical alloying and compacted by the spark plasma sintering method. Used strengthening elements were yttrium, which is most commonly used, and aluminium. Preparation of oxide dispersion was done in two ways: direct adding of yttria and alumina and inner oxidation of aluminium and yttrium. In the experimental part has been found, that it is possible to make oxide dispersion by both ways, but aluminium strengthened steel has to be prepared by inner oxidation to ensure fine oxide dispersion.

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.