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Additive manufacturing (AM) offers reduced material waste and energy usage, as well as an increase in precision. Direct metal AM is used not only for prototyping, but to produce final production parts in the aerospace, medical, automotive and other industries. Process mapping is an approach that represents process outcomes in terms of process input variables. Solidification microstructure process maps are developed for single bead and thin wall deposits of Ti-6Al-4V via an electron beam wire feed and electron beam powder bed AM process. Process variable combinations yielding constant beta grain size and morphology are identified. Comparison with the process maps for melt pool geometry shows that by maintaining a constant melt pool cross sectional area, a constant grain size will also be achieved. Additionally, the grain morphology boundaries are similar to curves of constant melt pool aspect ratio. Experimental results are presented to support the numerical predictions and identify a proportional size scaling between beta grain widths and melt pool widths. Results demonstrate that in situ, indirect control of solidification microstructure is possible through direct melt pool dimension control. The ability to control solidification microstructure can greatly accelerate AM process qualification potentially allow for tailored microstructure to the desired application.

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L'objectif de cette étude est de comprendre l'influence du silicium sur la microstructure d'alliages base TiAl. En effet, de faibles additions de silicium peuvent améliorer la tenue à chaud de ces intermétalliques. Nous montrons que le silicium a tendance à ségréger fortement durant la solidification, à l'échelle microscopique, provoquant l'apparition de siliciures primaires dans les zones interdendritiques. Après étude de cette ségrégation, nous avons procédé à des traitements thermiques d'homogénéisation afin d'étudier quantitativement les transformations solide-solide ayant lieu dans ces alliages. Ainsi, nous avons pu observer la précipitation de siliciures aux interfaces gamma/alpha2 dans des structures lamellaires homogènes. Mais, la structure lamellaire tend à se modifier en même temps que les siliciures germent et croissent. Les liens entre ces deux transformations simultanées sont mis en évidence expérimentalement, avant d'être modélisés à partir d'hypothèses simples. La réalisation d'essais mécaniques sur des microstructures contrôlées permet, en guise de conclusion, de donner des tendances quant à l'influence du silicium sur le comportement à chaud des alliages TiAl / The goal of this study is the understanding of the influence of silicon on the microstructure of TiAl-based alloys. Small additions of silicon are actually known to improve the heat resistance of these intermetallics. It is shown here that silicon segregates strongly at the microscopic scale during solidification, leading to the apparition of primary silicides in the interdendritic regions. After a study of this segregation, homogenization heat treatments were performed in order to focus on a quantitative study of the solid-solid transformations occuring in these alloys. Thus, silicide precipitation was observed at the gamma/alpha2 interfaces in homogeneous lamellar structures. However, the lamellar structure undergoes its own evolution as the silicides nucleate and grow. The links between these simultaneous transformations are shown by our experimental results, then modelled through simple considerations. As a conclusion, mechanical tests on controlled microstructures give some trends on the influence of silicon on the high temperature mechanical properties of TiAl alloys

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)

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Frequent systematic misindexing of electron backscatter diffraction patterns with five differently oriented pseudosymmetric solutions was observed for the cubic α-Al(Fe,M)Si phase with M = Mn, Cr encountered in secondary Al-Si casting alloy. That misindexing can be ascribed to the close structural relationship of the cubic crystal structure of α-Al(Fe,M)Si to that of the corresponding icosahedral quasicrystal. Robust identification of the correct among the five nearby solutions during automatic indexing can be achieved, which sensitively depends on the accuracy of Kikuchi-band detection applying Hough-space related indexing methods. Based on the correct crystallographic orientation solution, facets of the particles with bulk polyhedral and Chinese script morphology were determined to be {110} planes. Likewise, the habit planes of the α-Al(Fe,M)Si phase particles located at the naturally occurring oxide film are {110} planes.