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Copper is a material of interest to Additive Manufacturing (AM) owing to its outstanding material properties, which finds use in enhanced heat transfer and electronics applications. Its high thermal conductivity and reflectivity cause challenges in the use of Powder Bed Fusion AM systems that involve supplying high-energy lasers or electron beams. This makes Binder Jetting a better alternative as it separates part creation (binding together of powders) from energy supply (post-process sintering). However, it is challenging to fabricate parts of high density using this method due to low packing density of powder while printing. This work aims to investigate the effects of Hot Isostatic Pressing (HIP) as a secondary post-processing step on the densification of Binder Jet copper parts. By understanding the effects of HIP, the author attempts to create parts of near-full density, and subsequently to quantify the effects of the developed process chain on the material properties of resultant copper parts. The goal is to be able to print parts of desired properties suited to particular applications through control of the processing conditions, and hence the porosity. First, 99.47% dense copper was fabricated using optimized powder configurations and process parameters. Further, the HIP of parts sintered to three densities using different powder configurations was shown to result in an improvement in strength and ductility with porosity in spite of grain coarsening. The strength, ductility, thermal and electrical conductivity were then compared to various physical and empirical models in the literature to develop an understanding of the process-property-performance relationship. / Master of Science

A presente Tese de Doutorado analisa as modificações induzidas por prensagem isostática a quente (HIP) após a sinterização na resistência à fadiga de compósitos de metal duro com partículas de carboneto de tamanho médio na faixa de 0,6 a 2,0 ?m. A correlação entre a redução de porosidade no processo de prensagem isostática a quente e o aumento de resistência à ruptura transversal é bem conhecida. No entanto, existem questões em relação à eficácia deste processo no aumento da resistência à fadiga, devido à existência de outras imperfeições na microestrutura do material. Um aumento maior na resistência transversal é reportado na literatura para temperaturas de HIP acima do ponto eutético da liga. Os experimentos foram realizados em dois níveis diferentes de pressão de HIP, simulando condições de processo que existem em fornos de média e alta pressão (5,4 MPa e 150 MPa). Também são analisadas duas condições de temperatura de sinterização, 1.350ºC e 1.430ºC. A análise das diferentes condições de processamento mostra que a microestrutura mais homogênea, praticamente sem presença de lagos de cobalto, foi obtida a 1.430°C de temperatura de sinterização e de HIP. Esta condição de processamento resultou em melhores valores de resistência mecânica (estática e dinâmica). As diferenças de microestrutura e propriedades mecânicas obtidas nas duas condições de pressão de HIP (5,4 MPa e 150 MPa) são pouco significativas, tendo maior impacto a correlação entre a microestrutura e propriedades mecânicas em função dos diferentes ciclos de temperatura e tempo de sinterização. A análise das superfícies de fratura do material em fadiga indica uma importante influência de defeitos microestruturais, como regiões alinhadas da fase ? entre grãos de carboneto de tungstênio na iniciação e na propagação da trinca de fratura. / The present Thesis evaluates modifications induced by hot isostatic pressing (HIP) after sintering on fatigue strength of WC-11Co (in weight %) composites with sintered tungsten carbide grains of 0.6 to 2 ?m. The correlation between decreasing porosity due to hot isostatic pressing process and subsequent increase on transversal rupture strength is well known. Nevertheless, there are questions related to the efficiency of HIP process to increase fatigue strength, mainly due to the existence of microstructure defects besides porosity. An increase on transversal rupture strength is reported in the literature for HIP temperatures above the eutectic point of the composite. Experiments were carried out at two different levels of HIP pressure (5.4 and 150 MPa) covering conditions existing on medium and high pressure furnaces. Two temperatures were also evaluated (1,350 and 1,430°C). The analysis of different processing conditions shows that a more uniform microstructure, without the presence of cobalt lakes, was obtained at a sintering and HIP temperature of 1,430°C. This processing condition also resulted in better statical and dynamical mechanical properties. Microstructure and mechanical properties obtained at two different HIP pressure conditions (5.4 and 150 MPa) were rather similar. Major changes in microstructure and mechanical properties were found as a function of different cycles of temperature and sintering time. Fatigue fracture surfaces were evaluated revealing major influence of microstructural defects such as regions of aligned ? phase where crack initiation and fracture propagation are favored.

A presente Tese de Doutorado analisa as modificações induzidas por prensagem isostática a quente (HIP) após a sinterização na resistência à fadiga de compósitos de metal duro com partículas de carboneto de tamanho médio na faixa de 0,6 a 2,0 ?m. A correlação entre a redução de porosidade no processo de prensagem isostática a quente e o aumento de resistência à ruptura transversal é bem conhecida. No entanto, existem questões em relação à eficácia deste processo no aumento da resistência à fadiga, devido à existência de outras imperfeições na microestrutura do material. Um aumento maior na resistência transversal é reportado na literatura para temperaturas de HIP acima do ponto eutético da liga. Os experimentos foram realizados em dois níveis diferentes de pressão de HIP, simulando condições de processo que existem em fornos de média e alta pressão (5,4 MPa e 150 MPa). Também são analisadas duas condições de temperatura de sinterização, 1.350ºC e 1.430ºC. A análise das diferentes condições de processamento mostra que a microestrutura mais homogênea, praticamente sem presença de lagos de cobalto, foi obtida a 1.430°C de temperatura de sinterização e de HIP. Esta condição de processamento resultou em melhores valores de resistência mecânica (estática e dinâmica). As diferenças de microestrutura e propriedades mecânicas obtidas nas duas condições de pressão de HIP (5,4 MPa e 150 MPa) são pouco significativas, tendo maior impacto a correlação entre a microestrutura e propriedades mecânicas em função dos diferentes ciclos de temperatura e tempo de sinterização. A análise das superfícies de fratura do material em fadiga indica uma importante influência de defeitos microestruturais, como regiões alinhadas da fase ? entre grãos de carboneto de tungstênio na iniciação e na propagação da trinca de fratura. / The present Thesis evaluates modifications induced by hot isostatic pressing (HIP) after sintering on fatigue strength of WC-11Co (in weight %) composites with sintered tungsten carbide grains of 0.6 to 2 ?m. The correlation between decreasing porosity due to hot isostatic pressing process and subsequent increase on transversal rupture strength is well known. Nevertheless, there are questions related to the efficiency of HIP process to increase fatigue strength, mainly due to the existence of microstructure defects besides porosity. An increase on transversal rupture strength is reported in the literature for HIP temperatures above the eutectic point of the composite. Experiments were carried out at two different levels of HIP pressure (5.4 and 150 MPa) covering conditions existing on medium and high pressure furnaces. Two temperatures were also evaluated (1,350 and 1,430°C). The analysis of different processing conditions shows that a more uniform microstructure, without the presence of cobalt lakes, was obtained at a sintering and HIP temperature of 1,430°C. This processing condition also resulted in better statical and dynamical mechanical properties. Microstructure and mechanical properties obtained at two different HIP pressure conditions (5.4 and 150 MPa) were rather similar. Major changes in microstructure and mechanical properties were found as a function of different cycles of temperature and sintering time. Fatigue fracture surfaces were evaluated revealing major influence of microstructural defects such as regions of aligned ? phase where crack initiation and fracture propagation are favored.

To minimize the production cost and time of the heat treatment of critical application aluminum castings within the automotive industry a combined hot isostatic pressing (HIP)/solution heat treat process is desired. A successfully combined process would produce parts of equal quality to those produced by the individual processes of HIP and subsequent heat treatment with increased efficiency in time and energy. In this study, an experimental combined process was designed and implemented in a production facility. Industrially produced aluminum castings were subjected to the combined process and results were quantified via tensile and fatigue testing and microscopic examination. Comparisons in fatigue and tensile strength were made to raditionally HIPed and heat treated samples, as well as un-HIPed samples in the T6 condition. Results show that castings produced with the combined process show fatigue properties that are equal in magnitude to castings produced with the independent HIP and heat treatment processes. Furthermore, an order of magnitude improvement in the fatigue life in those castings that were produced with the combined process exists compared to the castings that were only heat treated. This study shows no difference in the tensile properties that result from any of the processing routes compared. Also, microstructural comparison of the castings processed show no difference between the process routes other than porosity, which is only evident in the un-HIPed samples. Dendrite cell size and dendritic structure of the samples that were solutionized for the same time is identical. Theoretical examination of the combined process was also completed to quantify the energy consumption of the combined process compared to the independent processes. Thermodynamic calculations revealed that the energy consumed by the combined process for a typically loaded HIP vessel is fifty percent less than the energy required to process the same quantity of castings with the two individual processes. However, it was determined that a critical ratio of the volume occupied in the HIP vessel by castings to the total HIP vessel volume exists that ultimately determines the efficiency of the combined process. This critical ratio was calculated to be approximately fifteen percent. If the volume ratio is less than fifteen percent then the combined process is less energy efficient then conventional processing. These thermodynamic calculations were experimentally verified with power consumption process data in a production facility. In addition, the time required for the combined process of HIP and solution heat treatment was calculated as thirty-percent less than the conventional two-step process. This calculation was verified via the comparison of data compiled from the experimental combined process.

Transparent ceramics are used in a variety of applications such as protective visors, thermo-graphic lens, night vision devices and windowpane of an armed vehicle, missile domes and in aircrafts. Yttrium Aluminium Garnet (YAG, Y3Al5O12) exhibits uniform index of refraction without birefringence owing to its cubic crystal structure and offers a range of optical and mechanical properties that makes it suitable for transparent applications.

The structure and properties of chemical vapor deposited zinc sulfide (CVD ZnS) were assessed before and after heat treatments, involving different annealing and hot isostatic pressing (HIPing) profiles. Samples were characterized using optical microscopy, SEM, TEM, electron diffraction, polycrystalline and powder x-ray diffraction, x-ray chemical microanalysis, photoluminescence, ultraviolet through longwave infrared transmission, and mechanical testing. Before heat treatment, CVD ZnS consists of lamellar twinned structures in 10 to 100 nm layers aggregated into domains which compose grains typically 5 to 10 μm in diameter with an overall crystallographic texture on the {100} planes. The scattering behavior of CVD ZnS was investigated and described by a surface scattering model based on internal surface roughness and refractive index variations due to onedimensional stacking disorder. The two to five percent hexagonality measured by x-ray diffraction is believed to form due to oxygen impurities at the twin boundaries which cause nanostructural polytypism and result in differential refractive index and scattering. CVD ZnS variants in low temperature deposited red ZnS and sulfur precursor elemental ZnS are examined as well. Color in CVD ZnS is believed to be due to band edge position, probably due to oxygen content, and not directly related to the hydride absorption at 6 μm. After annealing or hot isostatic pressing above 850 °C for sufficient time, CVD ZnS recrystallizes and becomes strongly textured on the {111} planes. This recrystallization is required to remove stacking disorder, resulting in a structure with less than half a percent hexagonality and low visible scattering. The recrystallization is believed to proceed by diffusing the oxygen at the nano-twin boundaries back into the lattice, thus unpinning the boundaries and allowing them to move and grow into the tabular recrystallized morphology by polytype induced exaggerated grain growth. The presence of active metals like platinum, silver, copper, or nickel during hot isostatic pressing causes a reaction with sulfur and lowers the temperature required for recrystallization. The optical scattering model is consistent in describing standard CVD ZnS, elemental ZnS, and multispectral recrystallized ZnS as having successively lower birefringence at internal surfaces.

A hot isostatic press (HIP) is a system which utilises high temperatures and pressure in order to densifyand enhance the material properties of components in the aerospace, automotive and additive manufacturingindustries, to mention a few. Quintus is a world leading manufacturer of HIP systems, and this master’s thesiswork has been written in collaboration with them. A HIP consists of a cylinder which gets filled with an inert gas, a gas which is then pressurised using compressors.Inside of the cylinder are heaters which ensure that the gas and load reach the desired temperature. Quintus’HIP construction has a wire wound cylinder. This means that a pre-stressed wire is wound around the cylinderfor a number of laps, resulting in the cylinder always being in a compressive stress state, thus ensuring a safeconstruction if a crack were to propagate in the material. This construction also allows for a more slim design ofthe cylinder which is beneficial when the gas is to be cooled, as the heat gets transported through the cylinder.An alternative design to this wire wound cylinder is a so called monoblock cylinder. This is a solid, thicker,cylinder, not wound by any wire. Quintus does not manufacture the monoblock HIP system, but these HIPs areon the market and therefore Quintus is keen to learn more about them. In this work, differences in the cooling capabilities with respect to the cylinders’ strength has been investigated,regarding the wire wound and monoblock cylinders. This has been done by the means of CFD and FEM(ANSYS CFX and ANSYS Mechanical), where a simplified 2D axisymmetric model of each HIP version wasused. In CFX, both a steady state and transient simulation was run for each model in order to capture the coolingof the gas. The resulting temperature load on the cylinder was then exported to the Mechanical setup to solvefor the arising stresses of the cylinders. The results of the work showed that the wire wound HIP does indeed exceed the monoblock cylinder when itcomes to the cooling rate, especially after some time when the gas has cooled off. Neither one of the cylinderswere at risk of yielding, and the monoblock cylinder was calculated to withstand >20 000 cycles, which is alsothe fatigue life of the wire in Quintus’ HIPs. The models and boundary conditions used in this work weresubjected to approximations, but the results obtained have still brought a lot of new insights to the monoblockconstruction, and have provided a good foundation for further analyses.

Boron carbide nano-powders, singly-doped over a range of compositions, were pressurelessly-sintered at identical temperature and atmospheric conditions in a dif- ferential dilatometer to investigate sintering behavior. Samples that achieved relative densities greater than 93% of theoretical density were post-HIPed. Post-HIPing re- sulted in an increase in relative density as well as an increase in Vicker's hardness. To optimize the sintering behavior, nano-powders with multiple dopants were prepared based on the results of single dopant experiments. These powders were studied using the same heating schedule as the single dopant samples. The powder with optimized composition was selected, and 44.45 mm diameter disks were pressed to determine the effects of sample size. Powder composition #166 with Al, Ti, W and Mg additions was processed using di¢çerent methods in order to create defect-free green bodies after uniaxial press- ing. The 44.45 mm diameter compacts were heat-treated to remove organics and B₂O₃coatings on particles and then encapsulated in an evacuated fused silica am- pule. Encapsulated samples were HIPed at temperatures below the coarsening region observed in the dilatometric traces of multiply-doped nano-powders. The E-HIPed sample showed a relative density of 96% with a limited extent of nano-sized grain microstructure.