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.

Hypersonic aerospace vehicles are severely limited by the lack of adequate high temperature materials that can withstand the harsh hypersonic environment. Tantalum carbide (TaC), with a melting point of 3880°C, is an ultrahigh temperature ceramic (UHTC) with potential applications such as scramjet engines, leading edges, and zero erosion nozzles. However, consolidation of TaC to a dense structure and its low fracture toughness are major challenges that make it currently unviable for hypersonic applications. In this study, Graphene NanoPlatelets (GNP) reinforced TaC composites are synthesized by spark plasma sintering (SPS) at extreme conditions of 1850˚C and 80-100 MPa. The addition of GNP improves densification and enhances fracture toughness of TaC by up to ~100% through mechanisms such as GNP bending, sliding, pull-out, grain wrapping, crack bridging, and crack deflection. Also, TaC-GNP composites display improved oxidation behavior over TaC when exposed to a high temperature plasma flow exceeding 2500 ˚C.

The main goal of this thesis is to deposit metal particles on the surface of 2D nanoplatelets using a controlled cementation process. As a proof of concept, copper (Cu) and Graphene Nanoplatelets (GNP) were chosen as the representative metal and 2D nanoplatelets, respectively. Specific goals of this study include depositing nanometer scale Cu particles on the surface of GNP at a low concentration (approximately 5 vol.%) while maintaining clustering and impurities at a minimum. Parametric studies were done to attain these goals by investigating various metallic reducer types and morphologies, GNP surface activation process, acid volume % and copper (II) sulfate concentrations. Optimal conditions were obtained with Mg ribbon as a reducer, 3 minutes of activation, 1 vol.% of acetic acid and 0.01 M CuSO4. The GNP-Cu powder synthesized in this work is a precursor material to be consolidated via spark plasma sintering (SPS) to make a nacre-like, layered structure for future studies.

Carbon nanotubes (CNTs) and graphene nanoplatelets (GNPs) are attractive reinforcements for lightweight and high strength metal matrix composites due to their excellent mechanical and physical properties. The present work is an attempt towards investigating the effect of CNT and GNP reinforcements on the mechanical properties of nickel matrix composites. The CNT/Ni (dry milled) nanocomposites exhibiting a tensile yield strength of 350 MPa (about two times that of SPS processed monolithic nickel ~ 160 MPa) and an elongation to failure ~ 30%. In contrast, CNT/Ni (molecular level mixed) exhibited substantially higher tensile yield strength (~ 690 MPa) but limited ductility with an elongation to failure ~ 8%. The Ni-1vol%GNP (dry milled) nanocomposite exhibited the best balance of properties in terms of strength and ductility. The enhancement in the tensile strength (i.e. 370 MPa) and substantial ductility (~40%) of Ni-1vol%GNP nanocomposites was achieved due to the combined effects of grain refinement, homogeneous dispersion of GNPs in the nickel matrix, and well-bonded Ni-GNP interface, which effectively transfers stress across metal-GNP interface during tensile deformation. A second emphasis of this work was on the detailed 3D microstructural characterization of a new class of Ni-Ti-C based metal matrix composites, developed using the laser engineered net shaping (LENSTM) process. These composites consist of an in situ formed and homogeneously distributed titanium carbide (TiC) as well as graphite phase reinforcing the nickel matrix. 3D microstructure helps in determining true morphology and spatial distribution of TiC and graphite phase as well as the phase evolution sequence. These Ni-TiC-C composites exhibit excellent tribological properties (low COF), while maintaining a relatively high hardness.

The aim of this thesis is preparation and characterization of bulk Mg–Ti based materials. In the first theoretical part properties of base materials and the complexity of preparation alloy from these metals is discussed. Second part is focused on powder metallurgy and its applicability on Mg–Ti system. In another part particle composites are described. In chapter current research another possible methods of alloy preparation from magnesium and titanium are mentioned. The experimental part of this thesis was the preparation of bulk Mg–Ti materials from metal powders. For sample preparation conventional methods of powder metallurgy and spark plasma sintering was employed. Furthermore a characterisation of these materials was done. Microstructure was observed. Present phases were found using X-ray diffraction analysis. Amounts of these phases were determined using a scanning electron microscope with energy–dispersive spectrometry and using X-ray fluorescence. Furthermore hardness was measured and bending test with evaluation was done. Significant difference in results of sample preparation using conventional methods of powder metallurgy and spark plasma sintering was observed.

Cold sintering process (CSP) je nová metoda pro slinování keramik a skel. Tato metoda vede ke snížení teploty (

Mechanical properties of aluminium alloys highly depend on their phase composition and microstructure. High strength can be achieved among others by introduction of a high volume fraction of fine, homogeneously distributed second phase particles and by a refinement of the grain size. Powder metallurgy allows to prepare fine grained materials with increased solid solubility which are favourable precursors for further precipitation strengthening. Gas atomization was used for the preparation of powders of the commercial Al7075 alloy and its modification containing 1 wt% Zr. A part of gas atomized powders was mechanically milled at different conditions. Mechanical milling reduced the grain size down to the nano-size range and the corresponding microhardness exceeded the value of 300 HV. Powders were consolidated by the spark plasma sintering method to nearly fully dense compacts. Due to a short time and relatively low temperature of sintering the favourable microstructure can be preserved in the bulk material. The grain size of compacts prepared from milled powder was retained in the submicrocrystalline range and the microhardness close to 200 HV exceeded that of the specially heat treated ingot metallurgical counterparts. The prepared compacts retained their fine grained structure and high...

This thesis is focused on carbide ceramics synthesis, more specifically on the synthesis of a Ti2AlC MAX Phase carbide using solution chemistry rather than powder metallurgy. Chloride and nitrate precursors have been used as a source of metals and citric acid as a source of carbon for carbothermal reduction and as a complexing agent. A new route of precursor synthesis has been developed based on peroxo-titanic acid, which helps retain aluminium. The syntheses were performed using the SPS facility to ensure high heating rates. Al4C3 and TiC carbides and their mixtures were prepared successfully. However, the Ti2AlC phase was not synthesized under used conditions. The phase composition, structure and grain sizes of the samples were investigated by powder X-ray diffraction, X-ray fluorescence and electron microscopy. The contents of carbon in the precursors were determined by thermogravimetric analysis.

No description available.