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This study aims to improve the Additive Manufacturing (AM) design space for the popular multi-component Ni alloy Inconel 625 (IN625) thorough investigating the microstructural evolution, namely the solidification microstructure and the solid-state phase transformations during the Laser Powder Bed Fusion (LPBF) process. Highly non-equilibrium solidification and the complex reheating conditions during the LPBF process result in the formation of various types of solidification microstructures and grain morphologies which consequently lead to a wide range of mechanical properties. Understanding the melt’s thermal conditions, alloy chemistry, and thermodynamics during the rapid solidification and solid-state phase transformation in AM process will help to control material properties and even produce a material with specific microstructural features suited to a given application. This research helps to better understand the process-microstructure-property relationships of LPBF IN625. First, a set of simple but effective analytical solidification models were employed to evaluate their ability to predict the solidification microstructure in AM applications. As a case study, Solidification Microstructure Selection (SMS) maps were created to predict the solidification growth mode and grain morphology of a ternary Al-10Si-0.5Mg alloy manufactured by the LPBF process. The resulting SMS maps were validated against the experimentally obtained LPBF microstructure available in the literature for this alloy. The challenges, limitations, and potential of the SMS map method to predict the microstructural features in AM were comprehensively discussed. Second, The SMS map method was implemented to predict the solidification microstructure and grain morphology in an LPBF-built multi-component IN625 alloy. A single-track LPBF experiment was performed utilizing the EOSINT M280 machine to evaluate the SMS map predictions. The resulting microstructure was characterized both qualitatively and quantitatively in terms of the solidification microstructure, grain morphology, and Primary Dendrite Arm Spacing (PDAS). Comparing the experimentally obtained solidification microstructure to the SMS map prediction, it was found that the solidification mode and grain morphology were correctly predicted by the SMS maps. Although the formation of precipitates was predicted using the CALculation of PHAse Diagrams (CALPHAD) approach, it was not anticipated from the analytical solution results. Third, to further investigate the microsegregation and precipitation in IN625, Scanning Transmission Electron Microscopy (STEM) using Energy-Dispersive X-ray Spectroscopy (EDS), High-Angle Annular Dark-Field Scanning Transmission Electron Microscopy (HAADF-STEM), Scheil-Gulliver (with solute trapping) model, and DIffusion-Controlled TRAnsformations (DICTRA) method were employed. It was found that the microstructural morphology mainly consists of the Nickel-Chromium (gamma-FCC) dendrites and a small volume fraction of precipitates embedded into the interdendritic regions. The precipitates predicted with the computational method were compared with the precipitates identified via HAADF-STEM analysis inside the interdendritic region. The level of elemental microsegregation was overestimated in DICTRA simulations compared to the STEM-EDS results; however, a good agreement was observed between the Scheil and STEM-EDS microsegregation estimations. Finally, the spatial variations in mechanical properties and the underlying microstructural heterogeneity of a multi-layer as-built LPBF part were investigated to complete the process-structure-properties relationships loop of LPBF IN625. Towards this end, numerical thermal simulation, electron microscopy, nano hardness test, and a CALPHAD approach were utilized to investigate the mechanical and microstructural heterogeneity in terms of grain size and morphology, PDAS, microsegregation pattern, precipitation, and hardness along the build direction. It was found that the as-built microstructure contained mostly columnar (Nickel–Chromium) dendrites were growing epitaxially from the substrate along the build direction. The hardness was found to be minimum in the middle and maximum in the bottom layers of the build’s height. Smaller melt pools, grains, and PDAS and higher thermal gradients and cooling rates were observed in the bottom layers compared to the top layers. Microsegregation patterns in multiple layers were also simulated using DICTRA, and the results were compared with the STEM-EDS results. The mechanism of the formation of precipitates in different regions along the build direction and the precipitates’ corresponding effects on the mechanical properties were also discussed. / Thesis / Doctor of Philosophy (PhD)

The rise of additive manufacturing has enabled new degrees of freedom in terms of design and functionality. In this context, this contribution addresses the design and characterization of structural unit cells that are intended as building blocks of highly porous lattice structures with tailored properties. While typical lattice structures are often composed of gyroid or diamond lattices, this study presents stackable unit cells of different sizes created by a generative design approach tomeet boundary conditions such as printability and homogeneous stress distributions under a given mechanical load. Suitable laser powder bed fusion (LPBF) parameterswere determined forAlSi10Mg to ensure high resolution and process reproducibility for all considered unit cells. Stacks of unit cells were integrated into tensile and pressure test specimens for which the mechanical performance of the cells was evaluated. Experimentally measured material properties, applied process parameters, and mechanical test results were employed for calibration and validation of finite element (FE) simulations of both the LPBF process as well as the subsequent mechanical characterization. The obtained data therefore provides the basis to combine the different unit cells into tailored lattice structures and to numerically investigate the local variation of properties in the resulting structures. / Durch die Einführung der Additiven Fertigung können neue Freiheitsgrade in Bezug auf Gestaltungsfreiheit und Funktionalität erreicht werden. In diesem Zusammenhang adressiert dieser Beitrag das Design und die Charakterisierung struktureller Einheitszellen als Bausteine für hochgradig poröse Gitterstrukturen mit maßgeschneiderten Eigenschaften. Während typische Gitterstrukturen oft auf Gyroid- oder Diamantstrukturen basieren, präsentiert dieser Beitrag stapelbare Einheitszellen unterschiedlicher Größe, die durch einen generativen Designansatz erstellt wurden. Hierdurch sollen verschiedene Randbedingungen wie eine gute Druckbarkeit und homogene Spannungsverteilung unter gegebenen mechanischen Lasten erreicht werden. Um eine hohe Auflösung und Reproduzierbarkeit der Einheitszellen zu erreichen, wurden für den verwendeten Werkstoff AlSi10Mg geeignete Druckparameter für das Laserstrahlschmelzen (LPBF) ermittelt. Stapel von Einheitszellen wurden in Zug- und Druckproben integriert, anhand derer die mechanische Stabilität der Zellen ermittelt wurde. Experimentell bestimmte Materialeigenschaften, die verwendeten Prozessparameter und die Ergebnisse der mechanischen Untersuchungen wurden anschließend für die Kalibrierung und Validierung Finiter Elemente (FE) Simulationen herangezogen, wobei simulationsseitig sowohl der Prozess des Laserstrahlschmelzens als auch die nachgelagerte mechanische Charakterisierung berücksichtigt wurden. Die hier präsentierten Ergebnisse sollen als Basis sowohl für eine gezielte Anordnung der Einheitszellen zu maßgeschneiderten Gitterstrukturen dienen als auch für die numerische Auswertung der lokal variierenden Eigenschaften der somit resultierenden Strukturen.

Microstructure and micro-mechanical characterization of as-built and heat-treated samples of Hastelloy X produced by laser powder bed fusion (LPBF) process has been carried out in this study. As-built LPBF blocks were solution heat-treated at 1177°C and 1220°C followed by fast cooling. The microstructure of as-built and heat-treated samples were studied by light optical microscopy, scanning electron microscopy, and electron backscatter diffraction. Instrumented indentation micro Vickers testing was performed to obtain microhardness and elastic modulus of asbuilt and heat-treated samples. Microtensile samples from as-built and heat-treated blocks were prepared and polished for mechanical characterization. Microtensile testing inside the scanning electron microscope was performed to evaluate the mechanical properties and to get information about the microstructural changes during plastic deformation. Microstructure characterization revealed disrupted epitaxial grain growth for the as-built samples whereas the two heated-treated Hastelloy X samples exhibited equiaxed grains with varying twin fractions. As-built Hastelloy X samples exhibited higher mean hardness than heat-treated samples. The yield strength of as-built samples reveals higher values as compared to conventional wrought Hastelloy X samples, whereas lower yield strength and higher elongation were observed for heat-treated samples as compared to as-built samples. Higher elongation and lower yield strength values were observed for the samples solution heat-treated at 1220°C compared to the solution heat-treated at 1177°C. Microstructural evaluation at different plastic strains during in-situ microtensile testing reveals a clear difference in dislocation density for as-built and heat-treated samples.