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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.

Die neuen TRIP-Matrix-Composite-Werkstoffe - verstärkt durch mit MgO teilstabilisiertem ZrO2 - gestatten es, durch die Besonderheiten der beteiligten Phasen eine gute Eigenschaftskombination hinsichtlich hoher Festigkeits- und Dehnungswerte zu erzielen. Aus diesem Grund ist die vorliegende Arbeit der Erforschung wissenschaftlicher Grundlagen zur Herstellung von TRIP-Matrix-Compositen sowie zur Analyse deren Eigenschaften in Abhängigkeit von den unterschiedlichen pulvermetallurgischen Herstellungsverfahren, wie konventionelles und konduktives Sintern sowie Heißpressen gewidmet worden. Als Ergebnis ist ein tieferes Verständnis der Kinetik von Sinterprozessen mit dem Aufbau eines physikalisch-mathematischen Modells festzuhalten. Ferner wurden mit weiterführenden Untersuchungen erste Ansätze zur Auslegung von Warmumformprozessen von gesinterten Halbzeugen aus dem Verbundwerkstoff durch quantitative Beschreibung der Entfestigungskinetik geleistet.

In this thesis, novel bulk Al-based alloys with high content of Al have been produced by powder metallurgy methods from amorphous and partially amorphous materials. Different processing routes, i.e. mechanical alloying of elemental powder mixtures, controlled pulverization of melt-spun glassy ribbons and gas atomization, have been employed for the production of the Al-based powders. Among the different processing routes, gas atomization is the best choice for the production of Al-based amorphous and partially amorphous powders as precursors for the subsequent consolidation step because it allows the production of large quantities of powders with homogeneous properties (e.g. structure and thermal stability) along with a uniform size distribution of particles. Amorphous and nanocrystalline powders have to be consolidated to achieve dense bulk specimens. However, consolidation of these phases is not an easy task and special care has to be taken with respect to accurate control of the consolidation parameters in order to achieve dense bulk specimens without inducing undesirable microstructural transformations (e.g. crystallization and grain coarsening) or insufficient particle bonding. Consequently, the effect of temperature on viscosity as well as on phase formation has been studied in detail in order to select the proper consolidation parameters. Following their characterization, the Al-based powders have been consolidated into bulk specimens by hot pressing (HP), hot extrusion and spark plasma sintering (SPS) and their microstructure and mechanical properties have been extensively investigated. Consolidation into highly-dense bulk samples cannot be achieved without extended crystallization of the glassy precursors. Nevertheless, partial or full crystallization during consolidation leads to remarkable mechanical properties. For example, HP Al84Gd6Ni7Co3 samples display a remarkably high strength of about 1500 MPa, which is three times larger than the conventional high-strength Al-based alloys, along with a limited but distinct plastic deformability (3.5 – 4%). Lower strength (930 MPa) but remarkably larger plastic strain exceeding 25 % has been achieved for the Al87Ni8La5 gas-atomized powders consolidated by SPS above their crystallization temperature. Similarly, HP Al90.4Y4.4Ni4.3Co0.9 bulk samples display high compression strength ranging between 820 and 925 MPa combined with plastic strain in the range 14 – 30%. Finally, preliminary tensile tests for the Al90.4Y4.3Ni4.4Co0.9 alloy reveal promising tensile properties comparable to commercial high-strength Al-based alloys. The mechanical behavior of the consolidated specimens is strictly linked with their microstructure. High strength and reduced plasticity are observed when a residual amorphous phase is present. On the other hand, reduced strength but enhanced plastic deformation is a result of the complete crystallization of the glass and of the formation of a partially or fully interconnected network of deformable fcc Al. These results indicate that the combined devitrification and consolidation of glassy precursors is a particularly suitable method for the production of Al-based materials characterized by high strength combined with considerable plastic strain. Through this method, the mechanical properties of the consolidated samples can be varied within a wide range of strength and ductility depending on the microstructure and the consolidation techniques used. This might open a new route for the development of innovative high-performance Al-based materials for transport applications.

19 Dec 2004. / Published through the Information Bridge: DOE Scientific and Technical Information. "IS-T 1983" Fei Tang. 12/19/2004. Report is also available in paper and microfiche from NTIS.

Ce travail de recherche porte sur l'élaboration de céramiques transparentes de CaLa₂S₄ pour la réalisation d'optiques MWIR et LWIR. Différentes méthodes de synthèse de poudres ont été explorées afin d'élaborer des poudres céramiques de grande pureté, cubiques et de morphologie adaptée à la densification. Il en a résulté le développement d'une méthode combustion comme nouvelle voie de synthèse de ce matériau. Différentes techniques de frittage ont été explorées : le SPS, le pressage à chaud (HP) et le frittage sous sulfure d'hydrogène (H₂S) suivi d'un post-frittage HIP. Le pressage à chaud permet d'élaborer des céramiques transparentes dans l'IR. Cependant leurs propriétés optiques sont dégradées par la présence de bandes d'absorption et par un noircissement important dû à l'interaction du matériau avec le graphite. Ces deux problématiques ont été résolues en combinant frittage naturel et compaction isostatique à chaud. La transmission des céramiques obtenues par ce procédé atteint à 13µm la transmission théorique de 68%. / This work focuses on the elaboration of CaLa₂S₄ transparent ceramics for IR optical applications in the MWIR and LWIR atmospheric windows. Various synthesis methods were explored for the elaboration of high purity cubic ceramic powders with adequate morphology for densification. As a result, we developed an innovative combustion method of this material. Different sintering techniques were investigated: Spark Plasma Sintering (SPS), Hot Pressing (HP) and Sintering in sulfurizing atmosphere (H₂S) combined to Hot Isostatic Pressing (HIP). Hot Pressing produces IR transparent ceramics. However, their optical properties are affected by the presence of absorption bands and significant blackening due to the interaction of the material with the graphite. These two issues have been solved by using sintering coupled to post-HIP. Transmission of the optics obtained by this process reaches the theoretical transmission of 68 % at 13μm.

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.

Diploma thesis focuses on preparation and characterization of bulk material prepared from pure magnesium powder. The topic includes all the parts of process of bulk material preparation, sintering at hot pressing, diffusion processes and structurally-mechanical properties with respect to final material porosity of the produced material. Thesis solving focuses on study and control of processes during bulk material preparation and description of the processes from physically-chemical point of view of the structure creation and final material properties.

Transparent polycrystalline aluminum oxide is a promising optical material, particularly in applications that require ballistic protection. However, the rhombohedral crystal structure of alumina limits its transparency due to birefringent scattering. One method of reducing birefringent scattering is to align the particles along the same crystallographic direction, minimizing the refractive index mismatch. This dissertation explores the use of high aspect-ratio platelet-morphology alumina powder in order to process a crystallographically aligned polycrystalline alumina part, with improved optical properties. The optimal hot-pressing parameters of non-pre-aligned platelet alumina were explored, showing that a low pre-load pressure (0MPa), a high maximum temperature (1800°C), a low maximum pressure (10MPa), and a long isothermal hold time (>5hrs) yields dense, transparent parts. These parameters resulted in samples with a high in-line transmission (>65%) despite a large grain size (>60μm). This is due to a high degree of crystallographic orientation, which minimizes the refractive index mismatch between grains, reducing birefringent scattering. Pre-alignment resulted in a further increase in crystallographic orientation, indicating that the pre-alignment procedure effectively aligns the platelets along the same crystallographic orientation. However, pre-alignment resulted in a minimal improvement in optical properties due to the pre-aligned platelets decreasing the densification. Mechanical properties were characterized, resulting in a flexure stress and Vickers hardness of approximately 175MPa and 17GPa, respectively. These low mechanical properties are due to the large grain size. The Vickers hardness was also characterized along different alignment/hot-pressing directions, showing that the hardness matches that of sapphire along corresponding crystallographic directions. Modifications to the Rayleigh-Gans-Debye model were made, accounting for crystallographic orientation. The modified model more closely matches the experimental optical data, illustrating the importance of accounting for crystallographic alignment. This dissertation emphasizes the importance of characterizing optical losses in transparent ceramics and how they relate to the microstructure, as well as the significance of crystallographic alignment in a birefringent transparent ceramic like alumina.

<div> <div> <div> <p>Transparent alumina is a candidate material for ballistic applications where visible or infrared wavelength transmission is required. However, the transparency of polycrystalline alumina can be limited due to the rhombohedral crystal structure being inherently birefringent. Birefringence causes light scattering at grain boundaries and is detrimental to the transparency. It has been shown experimentally that the application of a high magnetic field during processing can lead to crystallographic alignment and the reduction of birefringent light scattering. This alignment method is effective but is limited in terms of scalability. This research addresses these limitations through the use of simple and cost-effective shear and elongational forming processes such as uniaxial warm pressing and direct ink writing (DIW) for the improvement of final sintered transparency. To further support the improvement of these processes as alternatives and to evaluate the possibility of using powder ratios to improve the alignment, this research will also investigate the sintering behavior during hot-pressing of equiaxed and platelet powders. </p> <p>Platelet ceramic-filled thermoplastic blends were developed and formed into sheets through uniaxial warm pressing. The solids loading (30 – 40 vol.%) and platelet diameter (1.2 and 11μm) were varied to compare effects on viscosity, percent reduction, and final alignment. All ceramic- filled thermoplastic polymer blends exhibited pseudoplastic behavior. Crystallographic alignment of green body samples was quantified by the orientation parameter (r) and grain misalignment angle (full width at half maximum, FWHM) obtained from rocking curve analysis. Blends with 11μm diameter platelets displayed a higher temperature sensitivity constant, better flow properties, and higher alignment compared to blends with 1.2μm diameter platelets. Optimal samples produced with blends containing 30 vol.% of 11μm diameter platelets demonstrated an alignment of r = 0.251 +/- 0.017; FWHM = 11.16° +/- 1.16°. A sample with optimal alignment was hot-pressed to transparency and obtained an in-line transmission of 70.0% at 645nm. The final alignment of this pre-aligned hot-pressed sample (r = 0.254 +/- 0.008; FWHM = 11.38° +/- 0.54°) improved when compared to a non-pre-aligned sample (r = 0.283 +/- 0.005; FWHM = 13.40° +/- 0.38°).</p><p>Additionally, the use of direct ink writing, an additive manufacturing technique, as a viable alignment process for producing transparent alumina was investigated. Highly loaded (> 54 vol.%) equiaxed alumina suspensions were developed with platelet additions ranging from 0-20vol.% of the total solids loading. An increase in the amount of platelet powders from 5-20vol.% increased the dynamic yield stress from 104Pa to 169Pa and decreased in the equilibrium storage modulus from 17,036Pa to 13,816Pa. It was found that the DIW process significantly increased the alignment in one orientation when compared to samples cast from the same suspensions and this behavior may be connected to the rheological properties. Lastly, an optical analysis showed that sample developed with 5vol.% platelet suspensions had higher in-line transmission values across the visible spectrum when compared to samples developed with 20vol.% suspensions. A sample cast from a 5vol.% platelet suspensions had the lowest grain alignment but possessed an in-line transmission of 42.8% at 645nm, which was the highest of the samples produced in this study. An optical loss analysis showed, that this sample has the lowest backwards scattering losses due to residual porosity and this result was supported by the density data. It is suggested that the alignment of the DIW samples is more complex and a more advanced texture analysis will need to be conducted to properly characterize the grain alignment.</p><p>Lastly, the densification behavior of equiaxed and platelet powder ratios with no intentional pre-alignment was investigated. An initial sintering investigation identified the optimum maximum pressure selected for the hot-pressing process as 20MPa. Under the selected hot- pressing parameters, the effects of 0, 25, 50, 75, and 100wt.% equiaxed powder additions on the sintering behavior, optical properties, and grain alignment was investigated. The data showed that an increase in the amount of equiaxed powders decreased the initial powder compact displacements rate. Additionally, an increase in the wt.% equiaxed powders from 0wt% to 75wt% decreases the in-line transmission from 70.9% to 40.2%, respectively at 645nm. Lastly, an increase in the wt.% equiaxed powders from 0wt% to 75wt decreased the alignment from (r = 0.321 +/- 0.005; FWHM = 16.26° +/- 0.40°) to (r = 0.509 +/- 0.022; FWHM = 34.63° +/- 2.61°), respectively.</p></div></div></div>