No presente trabalho, peças com gradiente funcional de Al2O3 com reforço de NbC foram planejadas com o intuito de obter um MGF (material com gradiente funcional) com uma alta dureza e boa tenacidade à fratura a partir de diferentes técnicas de sinterização. Os MGFs apresentam-se como uma excelente alternativa quando é necessária a união de materiais com propriedades térmicas ou mecânicas muito diferentes, já que possuem uma transição suave de propriedades ao longo do corpo, como consequência de uma mudança gradual do teor das fases. No planejamento dos MGFs foram utilizadas análises dilatométricas para compatibilizar o comportamento durante a sinterização de cada camada e assim minimizar as tensões que ocorrem durante a retração, responsáveis por trincas e delaminações. Nos ensaios de dilatometria observou-se que a diferença máxima de retração entre os compósitos de teor de NbC variando de 5 a 30 %p é de 4,85%, assim, foram projetados MGFs com um passo de 5% de NbC, reduzindo esta diferença para 2,73%. Compósitos monolíticos de Al2O3 com diferentes teores de NbC foram sinterizadas a 1500ºC num forno convencional sob atmosfera de grafite. As densidades das peças sinterizadas foram inferiores a 90% da densidade teórica (DT), o que comprometeu a dureza dos compósitos (10 a 14 GPa), inferiores que as durezas dos materiais originais. Uma das maiores dificuldades no processamento destes compósitos foi sua densificação, prejudicada devido à presença de partículas de alta refratariedade na matriz de alumina, pelo que foi realizado um estudo do efeito da nióbia (Nb2O5) como auxiliar de sinterização nos compósitos Al2O3-NbC. Utilizando 0,5 %mol deste aditivo foi possível melhorar as densidades dos compósitos que, segundo os resultados da microscopia eletrônica de varredura (MEV), devido a uma densificação em presença de fase líquida. No entanto, a melhora na densidade é efetiva para temperaturas inferiores a 1450°C devido provavelmente à sobrequeima. Devido às dificuldades para obter peças densas a partir desses compósitos, foi utilizado o processo de Spark Plasma Sintering (SPS), o qual foi bem sucedido para obter peças com gradiente funcional com boa densidade (> 98 %TD) e livres de trincas. O gradiente projetado foi mantido com sucesso após a sinterização e, graças à alta densidade das peças, foi possível atingir altas durezas (até 24,3 GPa) e tenacidade à fratura ~5 MPa.m1/2, fazendo com que estes materiais apresentem potencial de aplicação como ferramentas de corte. / In the present work, Al2O3/ NbC graded composites were designed in order to obtain a FGM with a high hardness and good fracture toughness from different sintering techniques. Functionally graded materials (FGM) present enormous potential on matching materials that have different mechanical and thermal properties via a gradual transition throughout the body, as a consequence of a gradual transition of the phase content. For designing of FGMs, a dilatometric analysis was used for matching the sintering behavior of each layer in order to minimize the thermal strains occurring during shrinkage and that are responsible for cracking and delamination. It was observed that the maximum difference in shrinkage between these composites is 4.85%, which could be reduced to 2.73% if a FGM with step of 5% NbC is produced. Monolithic composites of Al2O3 with different amounts of NbC were sintered at 1500°C in a conventional oven under an atmosphere of graphite, the density of the sintered pieces were less than 90 %TD, compromising the hardness of the composites (10 to 14 GPa) that were lower than the hardness of the original materials. Due to the fact that one of the greatest difficulties in processing these composites is a densification, which is impaired due to the presence of high refractory particles in the alumina matrix, a study of the effect of the niobia (Nb2O5) as a sintering aid in the composite Al2O3-NbC was conducted, with addition of 0.5 mol% was possible to improve the density of the composites, due to the liquid state sintering according to the SEM results. However, this effect is only effective until a temperature of 1450°C probably due to the overfiring. In order to obtain dense bodies from these composites, Spark plasma sintering (SPS) was used. This process was successful for producing functional graded bodies with good density (> 98% TD) and crack free. The designed gradient was successfully maintained after sintering and due to the high density of FGMs, it was possible to attain high hardness (up to 24.3 GPa) and a fracture toughness of ~ 5 MPa.m1/2, showing that these materials have a good potential application as cutting tools.

Ce travail se place dans le cadre des matériaux thermo-structuraux utilisés dans les applications aéronautiques et aérospatiales. Les composites HfB2-SiC et ZrB2-SiC se sont avérés très prometteurs pour ces domaines, dans la mesure où ceux-ci présentent de bonnes tenues à l’oxydation à très haute température. L’enjeu principal de ce travail réside dans l’amélioration de leurs performances (durée de vie, résistance aux attaques chimiques et aux chocs thermiques) ainsi que dans la compréhension des mécanismes d’oxydation impliqués dans deux environnements distincts (sous oxygène moléculaire, à pression atmosphérique, de 1450 K à 2000 K et sous oxygène dissocié, à faible pression partielle d’oxygène, de 1800 K à 2200 K). Pour cela, une première étape a consisté à élaborer, par Spark Plasma Sintering (SPS), plusieurs nuances de matériaux homogènes en termes de microstructure et de densité relative. Leur comportement dans ces deux environnements a ensuite été étudié grâce à l’utilisation de dispositifs d’oxydation adaptés (four solaire et analyseur thermogravimétrique) et de techniques de caractérisation complémentaires (microscopie électronique à balayage, diffraction des rayons X, spectroscopies Raman et de photo-électrons). / This work is part of thermo-structural materials used in the aeronautic and aerospace fields. HfB2-SiC and ZrB2-SiC composites turned out to be very promising for these areas insofar as they present good oxidation resistance at very high temperature. The main issue of this work consists in improving their performances (lifetime, chemical attacks and thermal shocks resistance) and in the understanding of the oxidation mechanisms involved in two different environments (under molecular oxygen, at atmospheric pressure, from 1450 K to 2000 K and under dissociated oxygen, at low oxygen partial pressure, from 1800 K to 2200 K). To this end, a first step consisted in synthesizing, by Spark Plasma Sintering (SPS), several compositions of homogeneous materials in terms of microstructure and relative density. Then, their behavior in both environments has been studied thanks to the use of adapted oxidation facilities (solar furnace and thermogravimetric analyzer) and complementary characterization techniques (scanning electron microscopy, X-ray diffraction, Raman and photo-electron spectroscopies).

L'incertitude de l'énergie mondiale avec l'augmentation constante de la demande d'énergie déclenche la recherche de technologies de conversion d'énergie à haut rendement. Les dispositifs thermoélectriques (TE) peuvent jouer un rôle très important dans la collecte et la valorisation de l'énergie car ils peuvent être employés pour récupérer la chaleur résiduelle. Par exemple, la quantité de chaleur émise sous forme de déchets par les différents moteurs thermiques est évaluée en centaines de millions de MWh /an.Cette thèse vise à démontrer la faisabilité de fabrication des systèmes de récupération de la chaleur issue des déchets à l'échelle industrielle en utilisant des générateurs thermoélectriques (TE). Les techniques de fabrication proposées sont basées sur l'utilisation de technologies avancées comme le frittage par spark plasma, le broyage, la fusion laser sélective et la technologie de projection thermique. Ces techniques rendent possible l'élaboration de revêtements de matériau thermoélectrique avec des performances thermoélectriques supérieures et une flexibilité forte liées aux choix multiples de tailles, de formes et de matériaux.Nous nous sommes intéressés à l'étude du matériau semi-conducteur ß-FeSi2 car il présente un coefficient de mérite fort dans une plage de température de 300-800oC qui est la température des gaz en sortie de moteur voiture.Les techniques de SLM (Selective Laser Melting), de broyage, de frittage et de frittage flash (SPS) ont été successivement utilisées pour aboutir à l'élaboration de l'alliage ¿-FeSi2. Les revêtements ont ensuite été obtenus par la technique de projection plasma sous basse pression.Concernant le revêtement formé à partir de l'alliage par procédé LPPS, la transformation de phase de la phase cubique -ferrosilicium et de la phase quadratique ¿-Fe2Si5 en phase orthorhombique ß-FeSi2 se produit en obéissant aux réactions péritectique et eutectique. Après recuit sous température et temps appropriés, les revêtements présentent une phase complète ß-FeSi2 sur le substrat céramique.En outre pour une application à grande échelle, il est nécessaire de déposer ce type de revêtement sur un substrat en acier inoxydable et il convient dans ce cas d'utiliser un masque approprié pour fabriquer le dispositif thermoélectrique. / The uncertainty in the global energy with the constant increase in energy demand triggers the search for energyconversion technologies with high efficiency. The thermoeletrical devices (TE) can play a relevant role in thecollection and recovery of energy because they can be used to recover waste heat. For example, the amount of heatemitted as waste by different ombustion engines is evaluated hundreds of millions of MWh / year.This thesis aims to demonstrate the feasibility of anufacturing heat recovery systems from waste on an industrialscale using thermoelectric generators (TE). The proposed manufacturing techniques are based on the use ofadvanced technologies such as spark plasma sintering, crushing, selective laser melting and thermal spraytechnology. These techniques make possible the development of thermoelectric material coatings with superiorthermoelectric performance and high flexibility related to multiple choices of sizes, shapes and materials.The study of semiconductor ß-FeSi2 material was conducted in this goal because it has a strong merit coefficient(ZT) in the temperature range of 300-800°C which is the temperature of the output gas of the cars.Selective Laser Melting, sintering and spark plasma sintering (SPS) were successively used to lead to themanufacture of ¿-FeSi2 alloy. The coatings were then obtained by low pressure plasma spraying.Concerning the coating formed from the alloy, the phase transformation of the cubic phase ¿-ferro-silicon and thetetragonal phase ¿-Fe2Si5 in the orthorhombic phase ß-FeSi2 is produced by obeying the eritectic and eutecticreactions. After annealing under suitable temperature and time, the coatings sprayed on the ceramic bstratepresent a complete phase ß-FeSi2.In view of a large-scale application, it is necessary to spray this type of coating on a stainless steel substrate and inthis case to use a suitable mask for making the appropriate thermoelectric device.

Il lavoro si apre con un’approfondita ricognizione delle principali scuole di pensiero attinenti alla sociologia ambientale, analisi che conduce alla scelta del paradigma della modernizzazione ecologica come modello di riferimento preferenziale. Lo studio empirico prende in esame tre siti di produzione elettrica italiani, riguardo ai quali sono stati ricostruiti anzitutto gli elementi istituzionali di scenario. Questa ricostruzione, che nel caso italiano sottopone a critica alcuni aspetti della stessa teoria della modernizzazione ecologica, mette in relazione un consistente dibattito nazionale con l’agire concreto – anche se meno conosciuto – di soggetti internazionali di grande rilievo. Un secondo obiettivo della tesi consiste in una critica dei recenti processi di liberalizzazione della produzione e distribuzione dell’energia in Italia: un tema che sta ai confini della sociologia economica, dando per assodato che anche l’agire economico è per sua natura agire sociale. Un’ulteriore finalità dello studio si ravvisa nell’analisi dei processi di comunicazione ambientale messi in atto dalle organizzazioni produttive dell’energia nei confronti delle pubbliche opinioni, in una fase di potenziale ridistribuzione del mercato tra i diversi competitori. Sono evidenti in questo caso gli aspetti attinenti alla sociologia della cultura e della comunicazione. Gli strumenti utilizzati per condurre l’indagine sono essenzialmente riconducibili a due categorie: a) l’analisi documentale della letteratura teorica, delle fonti statistiche, dei documenti ufficiali degli enti pubblici e degli elaborati delle organizzazione produttive dell’energia: b) una serie di interviste in profondità condotte con testimoni privilegiati (utilizzando griglie semistrutturate). / This work begins with an outline of the main theoretical trends in Environmental Sociology and, in particular, the Ecological Modernization Theory. The empirical research studies three Italian electric power plants and, concerning this issue, it analyses some of the most meaningful aspects of international scenario. This analysis expresses critics on some elements of the Ecological Modernization Theory, and it will be of use in debating the energetic sector development and the connection between the national policy debate and the international organisms’ concrete action. The second objective of this thesis is to provide an assessment of the impact of the market liberalization on the social process of production of electricity. Another purpose of the study is to examine the role of power plants in the communication of environmental issues and ideas, in this historical period of market fragmentation, which is often followed by the increase in the number of competitors. The instruments used in this research are: Secondary Analysis of energy market data; content analysis of official documents created by governments and main energy companies. Some interview in-person made with managers and employers working for electric companies.

自2005年以降，我國針對是否開放含萊克多巴胺畜產品進口之問題即屬多事之秋，其主因係在食品添加物專家委員會（Joint FAO/WHO Expert Committee on Food Additives，簡稱JECFA）所擬每日容許攝食量下，國際上之相關科學研究無法確切證明萊克多巴胺是否完全安全，抑或其可能對於人體造成之危害及程度，因此多數肉品出口國仍常於家畜飼養過程中添加萊克多巴胺於飼料中，藉以增加畜產品之瘦肉比例並提升經濟效率；另一方面，由於不肖業者違法使用乙型受體素（如克崙特羅、沙丁胺醇）導致人體中毒的案件時有所聞，影響民眾對於畜產品的消費意願及產業發展，是故雖然萊克多巴胺之毒性相較於其他乙型受體素為低，惟受他種毒素高出數倍的乙型受體素之累，在我國自2006年起亦屬禁用之列。在國際食品標準委員會（Codex Alimentarius Commission，簡稱Codex委員會）於去（2012）年以普通多數決之方式制定萊克多巴胺的國際標準後，我國遂修訂食品衛生管理法第11條（2013年新法第15條）、第17-1條 （新法第25條）及動物用藥殘留標準第3條，並公告農防字第1011473960號之行政命令，採行「安全容許、牛豬分離、強制標示、排除內臟」之檢疫政策，在牛肉（含脂肪）的部分採行與國際標準相同之檢疫標準；惟在豬肉及內臟的部分，則為兼顧「國人特殊膳食習慣」及「相關產業發展」，仍維持既有「零檢出」的檢疫政策，全面禁止含萊克多巴胺的畜產品進口。針對此我國特殊之管制作法，本文將以國際經貿法的觀點，依據WTO協定中與檢疫措施最密切相關的SPS協定規範、過往案例之判決及相關文獻，分析我國進口檢疫規定之適法性，藉以思考目前畜產品進口的議題，並判斷該措施將來是否存在遭非難之可能，希冀能對於我國日後檢疫政策走向提供一實質性之參考及展望。 / Since 2005, the issue of liberalizing the import of meat containing Ractopamine had sparked great controversy in Taiwan, resulting from the lack of clear and definite scientific evidences worldwide to prove the harmlessness toward human body under JECFA’s maximal residue level and acceptable daily intake. Owing to the abusing of other much more poisonous Beta-adrenergic agonist (e.g., Clenbuterol, Salbutamol) by some of illegal stockbreeders causing the vibration of meat market and industry, Taiwan’s government had decided to ban the residual of Beta-adrenergic agonist including Ractopamine contained in both domestic and import meat products since 2006. After Codex Alimentarius Commission finally voted through the international standard of Ractopamine in 2012, Taiwan’s Legislative Yuan amended former regulations, approving the import of beef which conformed to Codex’s international standard, while still remained the prohibition of pork containing Ractopamine. This essay staying with the view of international trade law, in particular the Agreement on the Application of Sanitary and Phytosanitary Measures under World Trade Organization, tries to analyze the consistency of Taiwan’s meat regulations with the SPS agreement in order to prospect Taiwan’s trade policy and meat regulations regarding Ractopamine in the future.

La presente ricerca focalizza l’attenzione ad un approccio sociologico alla resilienza ai disastri. Nello specifico si vuole esplorare le relazioni sociali, che si sviluppano in un contesto di disastro naturale fra la popolazione colpita e i volontari di protezione civile. Gli ambiti di ricerca sono costituti dagli ultimi tre drammatici terremoti italiani: Umbria – Marche (1997), Molise (2002) e Abruzzo (2009). Nella prima parte della tesi si presentano le definizioni dei concetti fondamentali della sociologia dei disastri, un’analisi della letteratura presente per la tematica della resilienza nell’ambito delle scienze umane e sociali e l’organizzazione del sistema di protezione civile e difesa civile in Italia. In riferimento alla parte empirica, sono state raccolte importanti ed interessanti informazioni circa il possibile legame sociale fra volontari di protezione civile e popolazione colpita dai terremoti attraverso differenti metodologie di ricerca come le interviste semi strutturate agli esperti di protezione civile, un questionario on line per tutti i volontari di protezione civile ed i racconti di vita per la popolazione colpita dal terremoto. La ricerca conduce a interessanti risultati per la resilienza ai disastri in ambito sociologico e a suoi possibili sviluppi futuri. / The present research focalizes the attention on a sociological approach to disaster resilience. Specifically it would explore the social relationships established in a context of natural disaster and between population affected by natural disaster and civil protection volunteers. The research fieldworks are represented by last three dramatic Italian earthquakes: Umbria – Marche (1997), Molise (2002) e Abruzzo (2009). In the first part of the thesis will be presented the definitions of the fundamental concepts for the sociology of disasters, a literature review about the topic of disaster resilient presents within human and social science context and the organization of civil protection system and civil defence in Italy. Referring to the empirical part, there were collected important and interesting information about the possible social tie between civil protection volunteers and population affected by earthquakes through different methodologies of research as semi structured interviews to the civil protection experts, an on line questionnaire for all civil protection volunteers and life stories for population affected by earthquake. The research guides for interesting findings for disaster resilience within a sociological context and for its future possible developments.

No presente trabalho, peças com gradiente funcional de Al2O3 com reforço de NbC foram planejadas com o intuito de obter um MGF (material com gradiente funcional) com uma alta dureza e boa tenacidade à fratura a partir de diferentes técnicas de sinterização. Os MGFs apresentam-se como uma excelente alternativa quando é necessária a união de materiais com propriedades térmicas ou mecânicas muito diferentes, já que possuem uma transição suave de propriedades ao longo do corpo, como consequência de uma mudança gradual do teor das fases. No planejamento dos MGFs foram utilizadas análises dilatométricas para compatibilizar o comportamento durante a sinterização de cada camada e assim minimizar as tensões que ocorrem durante a retração, responsáveis por trincas e delaminações. Nos ensaios de dilatometria observou-se que a diferença máxima de retração entre os compósitos de teor de NbC variando de 5 a 30 %p é de 4,85%, assim, foram projetados MGFs com um passo de 5% de NbC, reduzindo esta diferença para 2,73%. Compósitos monolíticos de Al2O3 com diferentes teores de NbC foram sinterizadas a 1500ºC num forno convencional sob atmosfera de grafite. As densidades das peças sinterizadas foram inferiores a 90% da densidade teórica (DT), o que comprometeu a dureza dos compósitos (10 a 14 GPa), inferiores que as durezas dos materiais originais. Uma das maiores dificuldades no processamento destes compósitos foi sua densificação, prejudicada devido à presença de partículas de alta refratariedade na matriz de alumina, pelo que foi realizado um estudo do efeito da nióbia (Nb2O5) como auxiliar de sinterização nos compósitos Al2O3-NbC. Utilizando 0,5 %mol deste aditivo foi possível melhorar as densidades dos compósitos que, segundo os resultados da microscopia eletrônica de varredura (MEV), devido a uma densificação em presença de fase líquida. No entanto, a melhora na densidade é efetiva para temperaturas inferiores a 1450°C devido provavelmente à sobrequeima. Devido às dificuldades para obter peças densas a partir desses compósitos, foi utilizado o processo de Spark Plasma Sintering (SPS), o qual foi bem sucedido para obter peças com gradiente funcional com boa densidade (> 98 %TD) e livres de trincas. O gradiente projetado foi mantido com sucesso após a sinterização e, graças à alta densidade das peças, foi possível atingir altas durezas (até 24,3 GPa) e tenacidade à fratura ~5 MPa.m1/2, fazendo com que estes materiais apresentem potencial de aplicação como ferramentas de corte. / In the present work, Al2O3/ NbC graded composites were designed in order to obtain a FGM with a high hardness and good fracture toughness from different sintering techniques. Functionally graded materials (FGM) present enormous potential on matching materials that have different mechanical and thermal properties via a gradual transition throughout the body, as a consequence of a gradual transition of the phase content. For designing of FGMs, a dilatometric analysis was used for matching the sintering behavior of each layer in order to minimize the thermal strains occurring during shrinkage and that are responsible for cracking and delamination. It was observed that the maximum difference in shrinkage between these composites is 4.85%, which could be reduced to 2.73% if a FGM with step of 5% NbC is produced. Monolithic composites of Al2O3 with different amounts of NbC were sintered at 1500°C in a conventional oven under an atmosphere of graphite, the density of the sintered pieces were less than 90 %TD, compromising the hardness of the composites (10 to 14 GPa) that were lower than the hardness of the original materials. Due to the fact that one of the greatest difficulties in processing these composites is a densification, which is impaired due to the presence of high refractory particles in the alumina matrix, a study of the effect of the niobia (Nb2O5) as a sintering aid in the composite Al2O3-NbC was conducted, with addition of 0.5 mol% was possible to improve the density of the composites, due to the liquid state sintering according to the SEM results. However, this effect is only effective until a temperature of 1450°C probably due to the overfiring. In order to obtain dense bodies from these composites, Spark plasma sintering (SPS) was used. This process was successful for producing functional graded bodies with good density (> 98% TD) and crack free. The designed gradient was successfully maintained after sintering and due to the high density of FGMs, it was possible to attain high hardness (up to 24.3 GPa) and a fracture toughness of ~ 5 MPa.m1/2, showing that these materials have a good potential application as cutting tools.

Ce travail porte sur l'évolution microstructurale d'un alliage TiAl lors du frittage par un procédé appelé Spark Plasma Sintering (SPS). Les poudres initiales, élaborées par atomisation, sont constituées principalement d'une phase métastable. Les transformations qui accompagnent le retour à l'équilibre de cette dernière durant un chauffage sont finement caractérisées par MEB, MET et EBSD. Ces transformations seront ensuite utilisées comme marqueur thermique lors de la densification SPS afin de mieux estimer les amplitudes des gradients thermiques et mécaniques du procédé de frittage. Les mécanismes de densification responsables de la formation des cous sont discutés, ainsi que les origines des hétérogénéités microstructurales des échantillons complètement densifiés. Un comparatif des mécanismes de densification et des microstructures finales entre une poudre broyée et une poudre non broyée est dressé. Enfin, l'influence de l'application d'une contrainte dynamique pendant la compaction au moyen d'un dispositif original est présentée / This work focuses on the microstructure evolution of a TiAl alloy during sintering by a process called Spark Plasma Sintering (SPS). The initial powders, elaborated by atomization, consist primarily of a metastable phase. The transformations of the return to equilibrium of the latter during heating are finely characterized using SEM, TEM and EBSD. These phase transformations are then used as a thermal indicator during the SPS densification to estimate the thermal and mechanical gradients. The densification mechanisms responsible for the neck formation and the origins of the microstructure heterogeneities of fully densified samples are discussed. A comparison between the densification mechanisms and the final microstructures of a milled powder and a no milled powder is showed. Finally, the effect of the application of a dynamic stress during the compaction using an original process is presented

En raison de la résistance élevée à l’irradiation de certaines compositions, les oxydes de structure pyrochlore A₂B₂O ₇ sont considérés comme des matrices potentielles d’immobilisation des actinides produits en réacteur nucléaire. Dans ce contexte, l’étude de la stabilité structurale sous irradiation de ces oxydes est particulièrement importante. Ce travail concerne donc l’étude de l’influence de la composition des pyrochlores et de leur microstructure sur leur comportement vis-à-vis de l’irradiation.Dans ce but, quatre compositions d’oxydes pyrochlores de formule générale A₂B₂O ₇ avec A = Gd, Nd et B = Zr, Ti ont tout d’abord été élaborées. Différentes voies de synthèse (réaction à l’état solide, chimie douce par la méthode Pechini) de poudres pyrochlores ont été explorées afin de maîtriser in fine la taille de grains des céramiques densifiées par frittage classique ou par frittage SPS. Les résultats obtenus par chimie douce sont prometteurs : des poudres fines (<100 nm) de structure pyrochlore ont été élaborées. Enfin, selon les conditions de frittage SPS choisies, des céramiques denses ont été obtenues, avec une taille de grains de 700 nm pour Y₂Ti₂O ₇ et de 300 nm pour Nd₂Zr₂O ₇ , ce qui, à notre connaissance, correspond aux plus petites tailles de grains pour ce type de composé.Afin d’étudier le comportement sous irradiation, les oxydes élaborés de compositions Gd₂Ti₂O ₇ , Y₂Ti₂O ₇ , Gd₂Zr₂O ₇ et Nd₂Zr₂O ₇ , ont été irradiés avec des ions lourds de basse énergie (Au 4MeV délivrés par l’installation JANNuS à Orsay) pour déterminer les modifications structurales produites par les effets nucléaires et par des ions lourds d’une centaine de MeV (ligne IRRSUD) ou de l’ordre du GeV (ligne SME) du GANIL à Caen afin d’étudier les effets induits par les excitations électroniques. Les transformations induites par irradiation ont été caractérisées par Diffraction des Rayons X (parfois in situ avec le dispositif ALIX du GANIL), Microscopie Electronique à Balayage et en Transmission (MEB, MET) et spectroscopie Raman. La spectroscopie d'absorption (XANES et EXAFS effectuées au synchrotron SOLEIL) a été utilisée pour caractériser l'ordre local dans la phase amorphe induite par irradiation dans les titanates. Dans le domaine du ralentissement nucléaire, les résultats principaux sont que les titanates s’amorphisent sous irradiation alors que seule une transition pyrochlore-fluorine est observée pour les zirconates. Dans le domaine du ralentissement électronique, les titanates s’amorphisent par un mécanisme d’impact direct et Gd₂Zr₂O ₇ subit uniquement une transition pyrochlore-fluorine. Par contre, contrairement à son comportement observé sous irradiation avec des ions de basse énergie, Nd₂Zr₂O ₇ s’amorphise avec des ions lourds de haute énergie, avec une cinétique d’endommagement complexe qui met en jeu des transitions pyrochlore-amorphe, pyrochlore-fluorine et fluorine-amorphe. La structure interne des traces induites par excitations électroniques a été étudiée par MET. Les analyses par spectroscopie Raman en coupe transverse des échantillons irradiés ont permis la détermination de l’épaisseur de la phase amorphe ainsi que du pouvoir d’arrêt électronique seuil pour la formation des traces. Les conductivités thermiques des échantillons irradiés sont plus faibles que celles obtenues dans les composés non irradiés. Enfin, l’étude de la restauration thermique des composés irradiés avec des ions lourds de haute énergie montre que les transformations de phases ainsi que les températures auxquelles se produisent ces transformations dépendent de la composition. / Due to the high resistance to irradiation of some compositions, pyrochlore-type oxides with A₂B₂O ₇ structure are considered as potential matrices for the immobilization of actinides produced in nuclear reactor. In this context, the study of the structural stability after irradiation of these oxides is particularly important and should be investigated. This work aims at studying the effects of both the composition and the microstructure on the behavior of pyrochlores upon irradiation. For this purpose, four compositions of pyrochlore oxides of general formula A₂B₂O ₇ (with A = Gd, Nd and B = Ti, Zr) were first elaborated. Powders were prepared using different routes (solid state reaction, soft chemistry with Pechini process) in order to control the grain size of the ceramics densified either by conventional sintering or by SPS. The results obtained by soft chemistry are promising: fine powders (<100 nm) with the pyrochlore structure were prepared. Finally, according to the selected SPS conditions, dense ceramics were obtained with a grain size of 700 nm for Y₂Ti₂O ₇ and 300 nm for Nd₂Zr₂O ₇ , which, to our knowledge, corresponds to the smaller grain size for these compositions. Pyrochlore oxides with the compositions Gd₂Ti₂O ₇ , Y₂Ti₂O ₇ , Gd₂Zr₂O ₇ and Nd₂Zr₂O ₇ were irradiated with low energy heavy ions (4 MeV Au ions delivered by the JANNuS platform in Orsay) to determine the structural modifications produced by nuclear collisions. The same ceramics were also irradiated with swift heavy ions (hundreds of MeV on the IRRSUD beamline or of the order of GeV on the SME beamline) at the GANIL accelerator in Caen to study the effects induced by electronic excitations. The transformations induced by irradiation were characterized by XRD (in situ with the ALIX set up of the GANIL or ex situ after irradiation), scanning and transmission electron microscopy (SEM, TEM) and Raman spectroscopy. Fine absorption spectroscopy (XANES and EXAFS performed at the synchrotron Soleil) was implemented in order to characterize the local order in the amorphous phase induced by irradiation in the titanates. In the ballistic process regime, the main results are the amorphization of the titanates, while only an anion-deficient fluorite phase is formed for zirconates. The phase transformations induced by electronic excitation show that titanates become amorphous by a direct impact mechanism whereas a pyrochlore-fluorite transition occurs for Gd₂Zr₂O ₇ . However, in contrast to the behavior observed upon irradiation with low energy ions, Nd₂Zr₂O ₇ becomes amorphous upon high energy ion irradiations, with a complex damage kinetics involving pyrochlore-amorphous, pyrochlore-fluorite and fluorite-amorphous phase transitions. The internal structure of tracks induced by electronic excitation was studied by TEM. Raman spectroscopy analyses performed on cross-sectioned irradiated samples allowed the determination of the amorphous phase thickness and the electronic stopping power threshold for the formation of tracks.The thermal conductivities of the irradiated samples are lower than those obtained for unirradiated compounds. Finally, a specific study concerning the thermal recovery of irradiated pyrochlores with swift heavy ions shows that the phase transitions and the temperature at which these transformations occur depend on the composition.

Les travaux de recherche documentés dans cette thèse s'inscrivent dans le cadre de la Collaboration UA9 au CERN. L'objectif principal de la collaboration est l'étude de la collimation et de l'extraction de faisceaux de particules de haute énergie. La thèse est principalement consacrée au développement des détecteurs et aux installations expérimentales correspondantes qui ont été mises en œuvre au SPS et au LHC au CERN. En ce qui concerne la nature de l'interaction des particules chargées avec une structure monocristalline, un cristal courbé peut être utilisé pour orienter le faisceau de particules de haute énergie au moyen de la canalisation de particules entre les plans atomiques du cristal. Un tel phénomène est étudié de manière approfondie par la Collaboration UA9. Un des principaux objectifs de la recherche présentée dans cette thèse est de développer des dispositifs sensibles pour mesurer le flux et les caractéristiques de faisceau des particules déviées par le cristal au SPS et au LHC. Pour cette thèse nous avons étudié les détecteurs Cherenkov (CpFM) et les détecteurs à pixel (Timepix). Depuis 2015, le CpFM (détecteur de Cherenkov pour la mesure du flux de protons) a été souvent modifié afin d'améliorer la précision pour le comptage des particules. La plage de fonctionnement du dispositif varie de 1 à 1000 particules par faisceau de particules (~3 ns) avec une résolution inférieure à 20% par proton. Fonctionnant dans le vide primaire de l’accélérateur et à des doses de rayonnement élevées, le détecteur a montré une grande stabilité et ayant la possibilité d’effectuer des études de contamination par faisceau. À son tour, le détecteur Timepix a été étalonné sur la ligne de faisceaux d'extraction de l'accélérateur SPS, fonctionnant dans le vide secondaire (Roman Pot). Une partie importante de la thèse est consacrée à la caractérisation et à l'étalonnage de ces détecteurs avec les développements des logiciels pour l'acquisition et l'analyse de données. Dans cette thèse, nous proposons également la mesure du moment dipolaire magnétique (MDM) de baryons à courte durée de vie. Le MDM est une caractéristique importante de l'interaction des particules avec un champ magnétique externe. Pour cette thèse, nous nous concentrons sur la mesure le MDM du baryon LambdaC+, qui pourrait fournir des informations sur le facteur gyromagnétique (g) du quark charme. Une valeur différente de g=2 indiquera une structure composite possible du c-quark et clairement la présence de physique au-delà du Modèle Standard (SM). Jusqu'ici, aucune mesure expérimentale du moment dipolaire magnétique des baryons avec des quarks lourds n'a été effectuée en raison d'une courte durée de désintégration de ces particules (environ 60 um). La proposition faite dans cette thèse est de produire des baryons charmés par interaction forte entre les protons extraits (à l’aide d’un premier cristal courbé) et une cible. Après la cible, un deuxième cristal courbé à grand angle (de plusieurs mrad) est utilisé pour canaliser les baryons et induire une rotation du vecteur de polarisation des baryons charmés. Cette configuration s'appelle une configuration à double cristal et l'expérience est proposée au LHC. Dans cette thèse, je me suis concentré principalement sur tous les tests et la validation nécessaires au SPS avant la mise en œuvre au LHC. Une configuration expérimentale possible pour les mesures MDM au niveau du SPS est également proposée avec une estimation de l'erreur absolue de la valeur mesurée du facteur g pour le baryon LambdaC+. / The research work documented in this thesis is done in a frame of the UA9 Collaboration at CERN. The main goal of the collaboration is the investigation of the high-energy particle beam collimation and extraction. The thesis is mainly devoted to the developments of detectors and the consequent experimental setups implemented at the SPS or LHC circulating machines at CERN. Regarding the nature of the charged particle interaction with a monocrystalline structure, a curved crystal can be used for the steering of the high-energy particle beam by means of the particle channeling between atomic planes of the crystal. Such a phenomenon is intensively studied by the UA9 Collaboration. Therefore, one of the main goals of the presented research is to develop sensitive devices for measuring the flux and the beam characteristics of the particles deflected by the crystal at the circulating machines. The detectors studied for this thesis are Cherenkov (CpFM) and pixel (Timepix). Since 2015, the CpFM (Cherenkov detector for proton Flux Measurement) has undergone various modifications to improve the particle counting characteristics. The range of the device operation varies from 1 to 1000 particles per bunch (~3 ns) with the particle resolution of less than 20% per single proton. Working in the primary vacuum of the accelerator and at high radiation doses, the detector showed high stability with the possibility to perform beam contamination studies. In turn, the Timepix detector has been calibrated at the extraction beamline and SPS accelerator, working in the secondary vacuum of the Roman Pot. A significant part of the thesis is devoted to the characterization and calibration of these detectors with the software developments for data acquisition and analysis. In this thesis, we also make a proposal for the measurement of the magnetic dipole moment (MDM) of short-lived baryons. The MDM is an important characteristic of the particle interaction with an external magnetic field. For the thesis, we concentrate on the measurement of the LambdaC+ MDM, which could provide information on the gyromagnetic (g) factor of the charm quark. Any discrepancy from g=2 will indicate a possible composite structure of the c-quark and clearly physics beyond the Standard Model (SM). So far, no experimental measurements of this value of baryons with heavy flavoured quarks have been carried out due to a short decay length of these particles (about 60 um). The proposal made in this thesis is to produce charm baryons by a strong interaction of the extracted proton beam (using a first bent crystal) impinging onto a target followed by the second large angle bent crystal (of several mrad) to channel the baryons and to rotate their polarization vector. This configuration is called a double-crystal setup and the experiment is proposed to take place at the LHC. In this thesis, I concentrate mainly on all the tests and validation needed at the SPS prior to the implementation at the LHC. A possible experimental configuration for the MDM measurements at the SPS is also proposed with an estimation of the absolute error of the measured g-factor value for the LambdaC+ baryon.