<p>The aim of this study is to synthesize a material with high thermal conductivity and a low coefficient of thermal expansion (CTE), useful as a heat sink. Carbon nanofibres (CNF) are first coated with copper by an electroless plating technique and then sintered to a solid sample by either spark plasma sintering (SPS) or hot pressing (HP). The final product is a carbon nanofibre reinforced copper composite. Two different fibre structures are considered: platlet (PL) and herringbone (HB). The influence of the amount of CNF reinforcement (6-24 %wt), on the thermal conductivity and CTE is studied. CNF has an excellent thermal conductivity in the direction along the fibre while it is poor in the transverse direction. The CTE is close to zero in the temperature range of interest. The adhesion of Cu to the CNF surface is in general poor and thus improving the the wetting of the copper by surface modifications of the fibres are of interest such that thermal gaps in the microstructure can be avoided. The poor wetting results in CNF agglomerates, resulting in an inhomogeneous microstructure. In this report a combination of three different types of surface modifications has been tested: (1) electroless deposition of copper was used to improve Cu impregnation of CNF; (2) heat treatment of CNF to improve wetting; and (3) introduction of a Cr buffer layer to further enhance wetting. The obtained composite microstructures are characterized in terms of chemical composition, grain size and degree of agglomeration. In addition their densities are also reported. The thermal properties were evaluated in terms of thermal diffusivity, thermal conductivity and CTE. Cr/Cu coated platelet fibres (6wt% of CNF reinforcement) sintered by SPS is the sample with the highest thermal conductivity, ~200 W/Km. The thermal conductivity is found to decrease with increasing content of CNFs.</p>

Ionic transport in metal oxides is crucial for the functioning of a broad range of different components, such as heat resistant alloys designed for high temperature applications and oxide electrolytes in solid oxide fuel cells. This thesis presents results from in situ electrochemical studies of properties related to ionic transport in metal oxides that are important for their applications as protective oxides and ionic conductors. Heat resistant alloys of alumina-former type are known to form an adherent, slowly growing and protective aluminium oxide (Al2O3) scale that protects metals from chemical degradation at high temperature. In situ impedance spectroscopy was used to study highly pure and dense samples of a-alumina in the temperature range 400 – 1000 °C. It was shown that surface conduction on the sample could severely distort the measurement below 700 °C. The magnitude of the distortions appeared to be sensitive to the type of electrodes used. The use of a so-called guard electrode was shown to effectively block the surface conduction in the measurements. By varying the grain size of the sintered alpha-alumina samples, the influence of grain size on the overall conductivity of the a-alumina was studied. It was shown that the activation energy for conductivity increased as the grain size decreased. Molecular dynamics calculations were performed in order to elucidate whether Al- or O ions are dominant in the ionic conductivity of the alpha-alumina. Comparing the calculation and experimental results, the dominating charge carrier was suggested to be oxygen ions. Moreover, the ionic transport in thermally grown alumina-like oxide scales formed on a FeCrAl alloy was studied in situ by impedance spectroscopy between 600 and 1000 °C. It was shown that the properties of these scales differ largely from those of pure and dense alpha-alumina. Furthermore, the conductivity is mainly electronic, due to the multiphase/multilayer microstructure and substantial incorporation of species from the base metal. However, the diffusivity obtained from the ionic conductivity was in line with diffusion data in literature obtained by other methods such as thermogravimetry. Besides, the initial stage of oxidation of a number of Fe-, Ni- and Co-based alloys at temperatures between 500 and 800 °C was studied in situ by high temperature cyclic voltammetry, in which the oxygen activity was changed over a wide range. From the resulting voltammograms the redox reactions occurring on the alloy surface could be identified. It was concluded that the base metal oxidized readily on these alloys before a protective chromia- or alumina-like scale is formed. The base metal oxide is most likely incorporated into the more protective oxide. Further, the oxygen ionic conductivity of highly pure and fully dense yttria-stabilized zirconia produced by spark plasma sintering was studied by impedance spectroscopy. The aim was to evaluate intrinsic blocking effects on the ionic conduction associated with the space charge layer in the grain boundary region. It was observed that the ionic conductivity of the spark plasma sintered oxides is equal or slightly higher than what has been achieved by conventional sintering methods. In addition, it was shown that the specific grain boundary conductivity increases with decreasing grain size, which can be explained by a decreasing Schottky barrier height (i.e., decreasing blocking effect). The quantitative results from this work verify the space charge model describing the influence of grain size on the ionic conductivity of yttria-stabilized zirconia through dopant segregation and oxygen vacancy depletion along the grain boundaries. / QC 20100825

The aim of this study is to synthesize a material with high thermal conductivity and a low coefficient of thermal expansion (CTE), useful as a heat sink. Carbon nanofibres (CNF) are first coated with copper by an electroless plating technique and then sintered to a solid sample by either spark plasma sintering (SPS) or hot pressing (HP). The final product is a carbon nanofibre reinforced copper composite. Two different fibre structures are considered: platlet (PL) and herringbone (HB). The influence of the amount of CNF reinforcement (6-24 %wt), on the thermal conductivity and CTE is studied. CNF has an excellent thermal conductivity in the direction along the fibre while it is poor in the transverse direction. The CTE is close to zero in the temperature range of interest. The adhesion of Cu to the CNF surface is in general poor and thus improving the the wetting of the copper by surface modifications of the fibres are of interest such that thermal gaps in the microstructure can be avoided. The poor wetting results in CNF agglomerates, resulting in an inhomogeneous microstructure. In this report a combination of three different types of surface modifications has been tested: (1) electroless deposition of copper was used to improve Cu impregnation of CNF; (2) heat treatment of CNF to improve wetting; and (3) introduction of a Cr buffer layer to further enhance wetting. The obtained composite microstructures are characterized in terms of chemical composition, grain size and degree of agglomeration. In addition their densities are also reported. The thermal properties were evaluated in terms of thermal diffusivity, thermal conductivity and CTE. Cr/Cu coated platelet fibres (6wt% of CNF reinforcement) sintered by SPS is the sample with the highest thermal conductivity, ~200 W/Km. The thermal conductivity is found to decrease with increasing content of CNFs.

Le développement des moteurs électromagnétiques nécessite des matériaux magnétiques possédant une forte induction à saturation, une perméabilité magnétique importante, ainsi que de faibles pertes magnétiques lorsque le matériau est utilisé à des fréquences allant jusqu’à 20 kHz.Pour réduire ces pertes, le matériau doit alors posséder une résistivité électrique la plus élevée possible. Les composites magnétiques doux ont été développés dans ce contexte, en associant du fer (ou un alliage) à un matériau isolant. Historiquement, ceux-ci étaient présents sous forme de couches laminées, mais des matériaux coeur-écorce se sont développés ces dernières années.Au cours de ces travaux, nous avons développé l’enrobage de particules de fer par un matériau isolant et magnétique : le ferrite NiZn. L’enrobage de ferrite a été réalisé par voie liquide. De cette manière, il a été possible de réaliser un enrobage homogène d’épaisseur contrôlée sur des particules de fer sphériques.L’étude de la mise en forme de ces particules coeur-écorce, par métallurgie des poudres, a montré qu’en frittant le matériau composite à une température supérieure à 580°C, une réaction d’oxydoréduction a lieu entre les deux composés. Cette réaction mène à la formation d’une phase type FexNi1-x et d’une solution solide FeO-FeZnO. Ces deux phases font alors chuter les propriétés magnétiques du matériau final.Pour éviter cette réaction d’oxydoréduction, nous avons montré qu’il est possible d’ajouter une barrière de diffusion : la silice, ou bien de fritter le matériau à l’aide de techniques type FAST. De cette manière, nous avons obtenu un matériau possédant des pertes magnétiques comparables à celles de poudres industrielles mais avec une perméabilité magnétique supérieure. / Magnetic materials with high saturation induction, high magnetic permeability and low magnetic losses, are necessary for the development of electromagnetic motors used at frequencies up to 20 kHz.The electric resistivity of these materials must be as high as possible to reduce iron losses. To increase the resistivity of ferromagnetic materials, soft magnetic composites (SMC) were developed combining a ferromagnetic material with an insulating one. Firstly, laminated steel sheets were developed but during the last years core-shell materials were investigated.In this work, we have studied the coating of iron particles by an insulating and a magnetic material: NiZn ferrite. These coatings were deposited by an aqueous solution to obtain a homogenous coating with a controlled thickness on spherical iron particles.A study of composite shaping by powder metallurgy shows a redox reaction between ferrite and iron at a sintering temperature above 580°C. This reaction leads to the formation of a FexNi1-x and a FeO-FeZnO solid solution. These two phases deteriorate the magnetic properties of the final material.To avoid this redox reaction, we have shown that a silica layer can be used as a diffusion barrier. Another solution is to sinter the composite with a Field Assisted Sintering Technique (FAST) as Spark Plasma Sintering. A material with properties similar to industrial material and with a superior magnetic permeability was obtained with Spark Plasma Sintering

Made available in DSpace on 2016-06-02T20:15:28Z (GMT). No. of bitstreams: 1 5160.pdf: 6005480 bytes, checksum: 6aae866e51fab054ffc455e4b0479f2f (MD5) Previous issue date: 2013-02-25 / Financiadora de Estudos e Projetos / Considering the search for miniaturization of electronic devices, the development of new methods and techniques for the production and characterization of nanostructured materials is fundamental, beyond understanding of the effect of grain size on the properties of materials in nanoscale. Therefore, it was proposed in this work the obtaining of nanostructured multiferroic materials, in bulk, with high density and microstructural control, with grains ranging from micrometer to nanometer scale. To achieve this goal, was developed a methodology for obtaining the powder of lead iron niobate, Pb(Fe1/2Nb1/2)O3 (PFN) and lead iron tungstate, Pb(Fe2/3W1/3)O3 (PFW), with average particle size around 150 nm, contamination-free, minimal agglomeration and with highly reproductive results using the micro-milling technique. Regarding consolidation materials, conventional sintering requires higher temperatures and long holding times for a satisfactory densification, resulting in a grain growth higher than the desired. Through the fast sintering technique, only high heating rates are not sufficient to ensure a satisfactory densification and also inhibit the growth of grains. The obtain nanostructured dense samples with average grain size of approximately 200 nm was only possible using spark plasma sintering technique (SPS), which allows sintering at temperatures corresponding to the intermediate sintering stage, inhibiting the grain growth. PFN and PFW samples obtained through the SPS technique showed high conductivity at room temperature due the extreme reduction suffers in the system plus the use of high current densities during sintering, being necessary the samples oxidation. Through the dielectric characterization, the decrease in grain size of micrometer to nanometer scale results in lower permittivity values in phase transition temperature, besides a peak broadening. Moreover, the SPS technique added to the oxidation process makes it possible to obtain PFW samples with high dielectric values (in order of 104) at room temperature, a motivation results with regard to the application. / Considerando a busca pela miniaturização dos dispositivos eletrônicos é fundamental o desenvolvimento de novos métodos e técnicas para a produção e caracterização de materiais nanoestruturados, além do entendimento do efeito do tamanho de grão sobre as propriedades dos materiais em escala nanométrica. Dessa forma, propôs-se neste trabalho a obtenção de materiais multiferróicos nanoestruturados, na forma de bulk com alta densidade e controle microestrutural, com grãos variando de escala micrométrica a nanométrica. Para alcançar este objetivo, foi desenvolvida uma metodologia para a obtenção de pós de niobato de ferro e chumbo, Pb(Fe1/2Nb1/2)O3 (PFN) e tungstanato de ferro e chumbo, Pb(Fe2/3W1/3)O3 (PFW), com tamanhos médios de partículas em torno de 150 nm, livre de contaminação, mínima aglomeração e com resultados altamente reprodutivos por meio da técnica de micromoagem. Em relação à consolidação dos materiais, o procedimento convencional requer altas temperaturas e longos tempos de patamar para uma densificação satisfatória, resultando em um crescimento de grão superior ao desejado. Por meio da técnica de sinterização rápida fast sintering , somente altas taxas de aquecimento não são suficientes para garantir uma densificação satisfatória bem como inibir o crescimento de grãos. A obtenção de amostras densas nanoestruturadas com tamanhos médio de grão de aproximadamente 200 nm só foi possível utilizando a técnica spark plasma sintering (SPS), que permite a sinterização a temperaturas correspondentes ao estágio intermediário de sinterização, inibindo o crescimento de grãos. As amostras de PFN e PFW obtidas por meio da técnica de SPS apresentaram alta condutividade à temperatura ambiente devido às condições extremas de redução que a amostra sofre somada ao uso de altas densidades de corrente durante a sinterização, sendo necessária a oxidação das mesmas. Através da caracterização dielétrica, verifica-se que a diminuição nos tamanhos de grãos de escala micrométrica para nanométrica resulta em menores valores de permissividade na temperatura de transição de fase, além de um alargamento dos picos. Contudo, a técnica de sinterização SPS somada ao processo de oxidação torna possível a obtenção de amostras de PFW com altos valores de constate dielétrica (na ordem de 104), a temperatura ambiente, resultado extremamente motivador no que diz respeito à aplicação.

La réparation des revêtements barrières thermiques endommagés par fissuration entraine des coûts de maintenance très élevés. Dans cette étude, qui s’inscrit dans le cadre du projet Européen FP7-SAMBA, il a été proposé d’utiliser des particules de MoSi2(B), revêtues d’une couche d’alumine, comme agent cicatrisant. L’oxydation de celles-ci doit entrainer la formation de silice amorphe qui s’écoule dans la fissure puis réagit avec la barrière thermique en zircone yttriée pour former du zircon. Cette étude traite dans un premier temps de l’élaboration par Spark Plasma Sintering (SPS) de composites modèles composés de zircone yttriée et de particules de MoSi2(B) non revêtues. Les propriétés mécaniques (ténacité, dureté, module d’Young) et thermiques (conductivité thermique, coefficient de dilatation) de ces composites ont été déterminées. Les travaux se sont ensuite orientés vers l’étude du comportement en oxydation cyclique à 1100 °C sous air de ces composites par thermogravimétrie cyclique. La modélisation de l’oxydation de ces composites mais aussi de systèmes multi-couches MoSi2(B)/YPSZ modèles a permis de déterminer les mécanismes et les cinétiques de formation de la silice et du zircon. Une augmentation significative des cinétiques de formation de ces oxydes a été observée lorsque le bore est ajouté dans le MoSi2 ce qui peut être potentiellement très bénéfique pour la cicatrisation des fissures. L'utilisation du procédé SPS a permis de réaliser des systèmes barrières thermiques auto-cicatrisants sur substrats en superalliages à base de nickel revêtus à partir de zircone yttriée et de particules de MoSi2(B) elles-mêmes revêtues d’une couche d’alumine. La pré-oxydation des substrats revêtus favorise la croissance d’une couche d’alumine qui empêche la formation de siliciures par réaction entre les particules et la sous-couche. Ces revêtements présentent une bonne résistance à l’endommagement en cyclage thermique. Les observations post-mortem de ces systèmes mettent en évidence la cicatrisation locale de fissures par formation de silice et de zircon. Bien qu’il ne soit pas possible aujourd’hui de dire si la présence de ces particules augmente ou non la durée de vie de la barrière thermique, par manque de systèmes de référence, ces observations très encourageantes démontrent expérimentalement la validité du concept d’auto-cicatrisation des barrières thermiques proposé dans le cadre de ce projet. / Repair of thermal barrier coatings (TBC) systems damaged by cracking leads to significant maintenance costs. In this project (FP7-SAMBA), it was proposed to use MoSi2(B) particles, coated with an alumina shell, as healing agent for TBCs. Healing particles intercepted by cracks will oxidize preferentially, leading to the formation of amorphous SiO2, which flows into cracks and subsequently reacts with the TBC leading to the formation of a load bearing ZrSiO4 phase. In this study model composite materials were prepared from mixtures of yttria partially stabilized zirconia (YPSZ) and uncoated MoSi2(B) particles by using Spark Plasma Sintering (SPS) technique. Mechanical (toughness, hardness, Young modulus) and thermal (conductivity, coefficient of thermal expansion) properties of these materials were determined. Then, cyclic thermogravimetry analysis (CTGA) was used to study the oxidation behavior of these materials at 1100 °C in air. Kinetics of silica and zircon formations were determined through modelling of the oxidation of composite materials but also the oxidation of multi-layer YPSZ/MoSi2(B) materials. Boron addition was shown to significantly increase silica and zircon formation rates which could be very beneficial for the healing of the cracks. Then, SPS technique was used to sinter self-healing thermal barrier coatings on bond coated Ni-based superalloys from mixtures of YPSZ and Al2O3-coated MoSi2(B) particles. The pre-oxidation of coated substrates was shown to prevent the detrimental formation of silicides by the reaction of MoSi2(B) particles and the bond coat. Good results were obtained upon thermal cycling and post-mortem observations highlight local healing of cracks. At this time, it is too early to quantify the potential effect of the particles on the TBC lifetime due to a lack of reference systems and statistics. However, these observations demonstrate, experimentally, the validity of the self-healing mechanism proposed in the framework of this project.

A obtenção da sílica vítrea pelo processo de sinterização por plasma pulsado (SPS), a partir de matérias-primas de diferentes estruturas (cristalina e amorfa) e diferentes granulometrias, foi investigada. Análises de difração de raios X, transmitância óptica, microscopia óptica e eletrônica de varredura, e medições de densidade foram realizadas nas amostras sinterizadas. Sílicas vítreas transparentes foram fabricadas a partir de pós de quartzo atingindo-se temperaturas finais entre 1450 e 1600°C, enquanto que nanopó e pó amorfo de sílica formaram consolidados transparentes com temperaturas máximas próximas de 1200° C. Taxas de aquecimento entre 40 e 150°C/min. foram utilizadas nas sinterizações, com tempos de processo menores que 40 minutos. As maiores taxas de aquecimento exigiram uma maior temperatura final para a fusão completa do material cristalino e causaram, de forma indireta, a presença de aglomerações de micro-bolhas nas amostras obtidas com o nanopó. Um gradiente radial de temperatura (decrescente do centro para as bordas) foi observado nos consolidados fabricados com os pós cristalinos, facilitando o processo de fechamento da porosidade aberta. A presença ou ausência de material não fundido e de bolhas nas amostras foram analisadas por difratogramas de raios X, microscopia óptica e medidas de densidade. A análise da transmitância indicou uma quantidade praticamente nula de grupos OH nos compactos sinterizados com os pós cristalinos e em torno de 20 ppm no caso dos sólidos fabricados com matéria-prima sol-gel. Amostras de nanopós de sílica dopada com titânia (~6% em massa) foram processadas com temperaturas finais de 1200 e 1400°C apresentando coloração azulada e negra, respectivamente, e aumento dos clusters de titânia para a temperatura mais elevada. A sinterização a uma temperatura em torno 1200°C mantida por apenas 4 minutos resultou na conversão completa da fase anatase para a fase rutilo da titânia. / The production of vitreous silica by the spark plasma sintering (SPS) process, starting from raw materials of different structures (crystalline and amorphous) and granulometry were investigated. Analysis of X-ray diffraction, optical transmittance, optical and scanning electron microscopy, and density measurements were performed on the sintered compacts. Transparent vitreous silica was fabricated from quartz powder at final temperatures ranging from 1450 and 1600°C while silica nanopowder and silica powder formed transparent compacts at temperatures around 1200°C. Heating rates between 40 and 150° C/min. were used in processes with durations smaller than 40 minutes. Higher heating rates demanded higher final temperatures to complete the fusion process and caused, indirectly, the formation of micro-bubbles agglomerations in the samples produced from the nanopowder. A radial gradient of temperature (decreasing from the center to the border) was observed at the compacts fabricated with the crystalline powders favoring the closure of the open porosity. The presence or the absence of non-fused material and bubbles in the samples was analyzed by X-ray diffraction, optical microscopy and density measurements. The transmittance analysis indicated an almost zero quantity of OH groups in the compacts sintered from crystalline powders and about 20 ppm in the solids fabricated from the sol-gel raw material. Nanopowder samples of silica titania (~6 wt % of titania) were processed with final temperatures of 1200°C and 1400°C presenting blue and black coloration, respectively, and an increase of the titania clusters for the highest temperature. The sintering at temperatures near 1200°C with a holding time of just 4 minutes caused the complete anatase-rutile conversion in titania.

Cerâmicas piezelétricas possibilitam posicionamento e sensoriamento de precisão ou captação de energia mecânica valendo-se do efeito piezelétrico, capaz de converter energia mecânica em elétrica ou o contrário. Para aprimorar ou estender as aplicações dessas cerâmicas, mecanismos flexíveis podem ser acoplados a elas, formando um Dispositivo Piezelétrico Flextensional (DPF). No projeto desse tipo de estrutura, o conceito de Material com Gradação Funcional (MGF) é interessante, já que esses materiais apresentam variações graduais de suas propriedades efetivas, permitindo a alternância entre um material mais flexível e um mais rígido de acordo com a intensidade de deslocamento desejada em cada região da estrutura. Assim, neste trabalho, implementa-se o Método de Otimização Topológica (MOT) no projeto de estruturas gradadas com o intuito de identificar as vantagens e desvantagens da utilização do conceito de MGF em DPF. Esse método combina algoritmos de otimização e o Métodos dos Elementos Finitos (MEF) para distribuir material dentro de um domínio fixo através de um modelo de material, que no presente caso é o de Material Isotrópico Sólido com Penalização (MISP) adaptado a MGF. Na fabricação desses dispositivos otimizados, utiliza-se a Sinterização por Jato de Plasma (SJP) para a obtenção de tarugos gradados que são submetidos a processos de eletro-erosão e de corte a laser. Por fim, para a verificação dos resultados numéricos, utiliza-se um vibrômetro para aferir os deslocamentos dos protótipos de atuadores fabricados. / Piezoelectric devices enable precision positioning and sensing or mechanical energy harvesting based on the piezoelectric effect. In flextensional piezoelectric devices, flexible coupling structures are attached to ceramics to improve or extend the application possibilities. On the design of this kind of structure, the concept of Functionally Graded Materials (FGM) can be interesting, since it allows gradual variations of its effective properties along some direction by mixing two or more materials. Thus, in order to identify the advantages and disadvantages of using FGM, graded flexible coupling structures that maximize the performance of piezoelectric devices are obtained by implementing the Topology Optimization Method (TOM). This method combines optimization algorithms and the Finite Element Method (FEM) to distribute material inside a fixed domain. In this work, the formulation is based on the Solid Isotropic Material with Penalization (SIMP) material model adapted for the FGM concept, which can represent continuous change in material properties along the domain. Resulting optimal graded topologies of coupling structures are presented and compared with homogeneous structures. Finally, graded devices are manufactured through Spark Plasma Sintering (SPS) technique in order to be characterized, validating numerical results. The numerical results demonstrate the TOM efficacy in designing functionally graded piezoelectric devices and show, by its implementation, significant gains in graded mechanisms performance when compared with analogous homogeneous. Furthermore, the feasibility of proposed manufacturing process is confirmed, allowing the fabrication of prototypes with expected behavior.

L'objectif de ce travail était d'élaborer un matériau à gradient de propriétés fonctionnelles (MGF) W/Cu afin de remplacer la couche de compliance (Cu-OFHC) dans les composants face au plasma des machines de fusion thermonucléaire de type ITER. La particularité de ce travail étant de réaliser ces matériaux sans dépasser la température de fusion du cuivre dans le but de contrôler la microstructure des matériaux. Le cofrittage est la solution la plus attractive pour les réaliser. La première étape du travail a donc été de diminuer la température de frittage du tungstène afin de réaliser ce cofrittage. La mise en forme d'un MGF continus étant délicat, des calculs thermomécaniques ont été réalisés afin de déterminer le nombre et la composition chimique des couches W-Cu pour augmenter la durée de vie des CFPs. Les conditions de frittage par Spark Plasma Sintering ont été optimisées afin d'avoir une densité maximale des monomatériaux WxCu1-x. L'influence de la teneur en cuivre et de la densité des monomatériaux sur les propriétés thermiques et mécaniques a été étudiée. Les conditions de frittage SPS des monomatériaux ont été appliquées sur des assemblages W/CuCrZr composés de plusieurs couches intercalaires. L'importance du temps d'assemblages pour l'intégrité de ceux-ci a été mise en évidence. L'étude du temps de palier lors des assemblages W/CuCrZr a permis d'identifier un paramètre permettant de qualifier l'intégrité de l'assemblage quelle que soit la composition et la nature de la couche de compliance. De plus, les phénomènes associés à la formation des interfaces de l'assemblage ont été identifiés. L'interface W/WxCu1-x est formée par l'extrusion du cuivre de la couche WxCu1-x dans les porosités du tungstène. L'interface WyCu1-y/CuCrZr est formée par la migration du cuivre de la couche CuCrZr dans la couche WyCu1-y. Enfin l'optimisation des conditions d'assemblage a montré que les contraintes mécaniques dues à la densification du Matériau à gradient de Propriétés Fonctionnelles pouvaient être limitées en frittant préalablement ce matériau. / The objective of this study was to develop a Functionally Graded Material (FGM) W / Cu to replace the compliance layer (Cu-OFHC) in the plasma facing components of thermonuclear fusion reactor like ITER. The peculiarity of this work is to elaborate these materials without exceeding the melting temperature of copper in order to control its microstructure. The co-sintering is the most attractive solution to achieve this goal.The first phase of this study has been to decrease the sintering temperature of the tungsten to achieve this co-sintering. The elaboration of a Functionally Graded Materials being delicate, thermo-mechanical calculations were performed in order to determine the number and chemical composition in order to increase the lifespan of Plasma Facing Components. Spark Plasma Sintering conditions were optimized in order to achieve maximum density of WxCu1-x composites. The effect of copper content and density of the WxCu1-x composites on thermal and mechanical properties was investigated. The SPS conditions were applied for W/CuCrZr assemblies with a compliance layer composed of several interlayers. The importance of time for the integrity of assemblies thereof has been highlighted.The study of the dwell time during W/CuCrZr assembly leads to identify a parameter to characterize the integrity of the interface regardless of the composition and the nature of the layer of compliance. Moreover, the phenomena associated with the formation of the interface assembly have been identified. The interface W/WxCu1-x is formed by the extrusion of the copper layer of the WxCu1-x inside the tungsten porosities. The WyCu1-y/CuCrZr interface is formed by copper migration of CuCrZr layer inside the WyCu1-y layer. Finally optimization assembly conditions showed that the mechanical stresses due to the densification of the Functionally Graded Materials can be limited by sintering the FGM before the assembly.

1. Beim feldaktivierten Sintern im Temperaturbereich von 500 bis 1000 °C fließen elektrische Ströme mit einer Dichte von 1 bis 3 A/mm². 2. Daraus folgt für die größten verwendeten Pulverteilchen mit einem Radius von 50 µm ein Strom je Teilchenkontakt von 10 bis 50 mA. 3. Die durch das Aufbringen des prozesstechnisch notwendigen Pressdruckes gebildeten relativen Kontaktradien (Kontaktradius geteilt durch Teilchenradius) haben eine Größe von 0,05 bis 0,3. 4. Die Einengung der Strompfade im Kontakt der Pulverteilchen erhöht, zusammen mit dem elektrischen Widerstand der Oxidschicht auf den Pulverteilchen, den elektrischen Widerstand des Pulverpresslings. 5. Der Stromfluss durch die Teilchenkontakte führt mit dem zusätzlichen elektrischen Widerstand dieser Teilchenkontakte zu einer lokalen Temperaturerhöhung (Übertemperatur) von 10-4 bis 1 Kelvin für Kupfer- respektive Stahlpulver. 6. Der zusätzliche elektrische Widerstand der Oxidschicht kann die Übertemperatur beim Kupferpulver auf bis zu 1 mK erhöhen. 7. Mit abnehmendem Teilchenradius sinkt die Übertemperatur quadratisch. 8. Das Wachstum der Teilchenkontakte im Verlauf der Verdichtung führt zu einer kontinuierlichen Verringerung der Übertemperatur. 9. Das Auftreten von schmelzflüssiger Phase, von Metalldampf oder von Plasma wird in den untersuchten metallischen Systemen ausgeschlossen. 10. Auch Elektromigration, Thermomigration oder andere Wirkungen des elektrischen Stromes spielen keine Rolle für die Verdichtung beim feldaktivierten Sintern. 11. Die Verwendung von gepulstem anstelle von kontinuierlichem Gleichstrom beeinflusst die Verdichtung der untersuchten Werkstoffe nicht. 12. Die Verdichtung vom Pulver zum kompakten Werkstoff findet für Pulverteilchen mit einem Radius größer als R = 10 µm über plastische Verformung durch verschiedene Formen des Kriechens statt. 13. Die Verformung ist im Anfangsstadium auf den Kontaktbereich begrenzt. 14. Bei Pulverteilen mit Teilchenradien unter R = 10 µm findet die Verdichtung zunächst als Folge von Leerstellenströmen in die Kontaktkorngrenze statt (Sintern). 15. Durch die schnelle Verdichtung bei niedriger homologer Temperatur werden Kornwachstum und Rekristallisation verringert.