This thesis aims to investigate the manufacturability of nickel-based superalloys, IN625 and IN718, using the laser powder bed fusion (LPBF) process. The study provides a better understanding of the process-structure-property of nickel-based superalloys, their fatigue life, and subsequent post-processing. First, the process-structure-property was investigated by selecting a wide range of process parameters to print coupons for IN625 and IN718. Next, a subset of process parameters was defined that would produce high relative density (>99%), low surface roughness (~2 μm), and a low tensile RS. Second, a multi-scale finite element model was constructed to predict the temperature gradients, cooling rates, and their effect on RS. At constant energy density, RS is affected by scan speed, laser power, and hatch spacing, respectively. Third, the optimum set of parameters was used to manufacture and test as-built and shot-peened samples to investigate the fatigue life without costly heat treatment processes. It was found that shot peening resulted in a fatigue life comparable to wrought heat-treated unnotched specimen. Additionally, IN625 had a better fatigue life compared to IN718 due to higher dislocations density as well as the absence of γ´ and γ´´ in IN718 due to the rapid cooling in LPBF. Finally, the effect of post-processing on dimensional accuracy and surface integrity was investigated. A new approach using low-frequency vibration-assisted drilling (VAD) proved feasible by enhancing the as-built hole accuracy while inducing compressive in-depth RS compared to laser peening, which only affects the RS. These favorable findings contributed to the scientific knowledge of LPBF of nickel-based superalloys by determining the process parameters optimum window and reducing the post-processes to obtain a high fatigue life, a better dimensional accuracy, and improved surface integrity. / Thesis / Doctor of Philosophy (PhD)

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Additive manufacturing (AM) – and laser powder bed fusion (LPBF) specifically – constructs geometry that would not be possible using standard manufacturing techniques. This geometric versatility allows integration of multiple components into a single part. While this practice can reduce weight and part count, there are also serious drawbacks. One is that the LPBF process can only build parts with a single material. This limitation generally results in over-designing some areas of the part to compensate for the compromise in material choice. Over-designing can lead to decreased functional efficiency, increased weight, etc. in LPBF parts. Methods to control the material composition spatially throughout a build would allow designers to experience the full benefits of functionality integration. Spatial composition control has been performed successfully in other AM processes – like directed energy deposition and material jetting – however, these processes are limited compared to LPBF in terms of material properties and can have inferior spatial resolution. This capability applied to the LPBF process would extend manufacturing abilities beyond what any of these AM processes can currently produce. A novel concept for spatial composition control – currently under development at Brigham Young University – utilizes liquid or liquid-encased dopants to selectively alter the composition of the powder bed, which is then fused with the substrate to form a solid part. This work is focused on evaluating the feasibility and usefulness of this novel composition control process. To do this, the present work evaluates two deposition methods that could be used; explores and maps the laser parameter process space for zirconia-doped SS 316L; and investigates the incorporation of zirconia dopant into SS 316L melt pools. In evaluating deposition methods, inkjet printing is recommended to be implemented as it performs better than direct write material extrusion in every assessed category. For the process space, the range of input parameters over which balling occurred expanded dramatically with the addition of zirconia dopant and shifted with changes in dopant input quantities. This suggests the need for composition-dependent adjustments to processing parameters in order to obtain desired properties in fused parts. Substantial amounts of dopant material were confirmed to be incorporated into the laser-fused melt tracks. Individual inclusions of 100 $nm$ particles distributed throughout the melt pool in SEM images. Howewver, EDX data shows that the majority of the incorporated dopant material is located around the edges of the melt pools. Variations of dopant deposition, drying, and laser scanning parameters should be studied to improve the resulting dopant incorporation and dispersion in single-track line scans. Area scans and multi-layer builds should also be performed to evaluate their effect on dopant content and dispersion in the fused region.

This thesis is about laser powder bed fusion (L-PBF) of the nickel-based superalloy: Alloy 247LC. Alloy 247LC is used mainly in gas turbine blades and processing the blades with L-PBF confers performance advantage over the blades manufactured with conventional methods. This is mainly because L-PBF is more suitable, than conventional methods, for manufacturing the complex cooling holes in the blades. The research was motivated by the need for academia and industry to gain knowledge about the processability of the alloy using L-PBF. The knowledge is essential in order to eventually solve the problem of cracking which is a major problem when manufacturing the alloy. In addition, dense parts with low void content should be manufactured and the parts should meet the required performance. Thus, the thesis answered some of the important questions related to process parameter-microstructure-defect relationships. The thesis presented an introduction in chapter 1. A literature review was made in chapter 2 to 4. In chapter 2, the topic of additive manufacturing was introduced followed by an overview of laser powder bed fusion. Chapter 3 focused on superalloys. Here, a review was made from the broader perspective of superalloys but was eventually narrowed down to the characteristics of nickelbased superalloys and finally Alloy 247LC. Chapter 4 reviewed the main research on L-PBF of Alloy 247LC. The methodology applied in the thesis was discussed in chapter 5. The thesis applied statistical design of experiments to show the influence of process parameters on the defects and microstructure, so a detail description of the method was warranted. This was given at the beginning of chapter 5 and followed by the description of the L-PBF manufacturing and the characterization methods. The main results and discussions, in chapter 6, included a preliminary investigation on how the process parameters influenced the amount of discontinuity in single track samples. This was followed by the results and discussions on the investigation of voids, cracks and microhardness in cube samples (detail presentation was given in the attached paper B). Finally, the thesis presented results of the microstructure obtainable in L-PBF manufactured Alloy 247LC. The initial results of the microstructure investigation were presented in paper A.

The interest for additive manufacturing techniques have in recent years increased considerably because of their association to good printing resolution, unique design possibilities and microstructure. In this master project, 316L stainless steel was printed using metal laser powder bed fusion in an attempt to find process parameters which yield good productivity while maintaining as good material properties as possible. Laser powder bed fusion works by melting a powder bed locally with a laser. When one slice of the material is done, the powder bed is lowered, new powder is added on top, and the process is repeated, building the components layer by layer. In this thesis, samples produced with a powder layer thickness of 80 μm and 100 μm has been investigated. Process parameters like laser power, scanning speed and hatch spacing were investigated in order to establish clear processing windows where the highest productivity and lowest porosity are obtained. The most common defects in all sample batches were lack of fusion, gas pores, and spatter related pores. The best samples with regard to both porosity and build rate were obtained at normalized build rates between 1,3-1,6 and porosity-values in the 0,01-0,1 % range.

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Nickel-based superalloys, an alloy system bases on nickel as the matrix element with the addition of up to 10 more alloying elements including chromium, aluminum, cobalt, tungsten, molybdenum, titanium, and so on. Through the development and improvement of nickel-based superalloys in the past century, they are well proved to show excellent performance at the elevated service temperature. Owing to the combination of extraordinary high-temperature mechanical properties, such as monotonic and cyclic deformation resistance, fatigue crack propagation resistance; and high-temperature chemical properties, such as corrosion and oxidation resistance, phase stability, nickel-based superalloys are widely used in the critical hot-section components in aerospace and energy generation industries. The success of nickel-based superalloy systems attributes to both the well-tailored microstructures with the assistance of carefully doped alloying elements, and the intently developed manufacturing processes. The microstructure of the modern nickel-based superalloys consists of a two-phase configuration: the intermetallic precipitates (Ni,Co)3(Al,Ti,Ta) known as γ′ phase dispersed into the austenite γ matrix, which is firstly introduced in the 1940s.  The recently developed additive manufacturing (AM) techniques, acting as the disruptive manufacturing process, offers a new avenue for producing the nickel-based superalloy components with complicated geometries. However, γ′ strengthened nickel-based superalloys always suffer from the micro-cracking during the AM process, which is barely eliminated by the process optimization. On this basis, the new compositions of γ′ strengthened nickel-based superalloy adapted to the AM process are of great interest and significance. This study sought to design novel γ′ strengthened nickel-based superalloys readily for AM process with limited cracking susceptibility, based on the understanding of the cracking mechanisms. A two-parameter model is developed to predict the additive manufacturability for any given composition of a nickel-based superalloy. One materials index is derived from the comparison of the deformation-resistant capacity between dendritic and interdendritic regions, while another index is derived from the difference of heat resistant capacity of these two spaces. By plotting the additive manufacturability diagram, the superalloys family can be categorized into the easy-to-weld, fairly-weldable, and non-weldable regime with the good agreement of the existed knowledge. To design a novel superalloy, a Cr-Co-Mo-W-Al-Ti-Ta-Nb-Fe-Ni alloy family is proposed containing 921,600 composition recipes in total. Through the examination of additive manufacturability, undesired phase formation propensity, and the precipitation fraction, one composition of superalloy, MAD542, out of the 921,600 candidates is selected. Validation of additive manufacturability of MAD542 is carried out by laser powder bed fusion (LPBF). By optimizing the LPBF process parameters, the crack-free MAD542 part is achieved. In addition, the MAD542 superalloy shows great resistance to the post-processing treatment-induced cracking. During the post-processing treatment, extensive annealing twins are promoted to achieve the recrystallization microstructure, ensuring the rapid reduction of stored energy. After ageing treatment, up to 60-65% volume fraction of γ′ precipitates are developed, indicating the huge potential of γ′ formation. Examined by the high-temperature slow strain rate tensile and constant loading creep testing, the MAD542 superalloy shows superior strength than the LPBF processed and hot isostatic pressed plus heat-treated IN738LC superalloy. While the low ductility of MAD542 is existed, which is expected to be improved by modifying the post-processing treatment scenarios and by the adjusting building direction in the following stages of the Ph.D. research. MAD542 superalloy so far shows both good additive manufacturability and mechanical potentials. Additionally, the results in this study will contribute to a novel paradigm for alloy design and encourage more γ′-strengthened nickel-based superalloys tailored for AM processes in the future. / <p>Additional funding agencies: Agora Materiae Graduate School for multidisiplinary PhD students at Linköping University, and Stiftelsen Axel Hultgren.</p>

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This work identifies alloy terminal freezing range, columnar growth, grain coarsening, liquid availability towards the terminal stage of solidification, and segregation towards boundaries as primary factors affecting the hot-cracking susceptibility of fusion-based additive manufacturing (F-BAM) processed alloys. Additionally, an integrated computational materials engineering (ICME)-based approach has been formulated to design novel Al alloys, and high entropy alloys for F-BAM processing. The ICME-based approach has led to heterogeneous nucleation-induced grain refinement, terminal eutectic solidification-enabled liquid availability, and segregation-induced coalescence of solidification boundaries during laser-powder bed fusion (L-PBF) processing. In addition to exhibiting a wide crack-free L-PBF processing window, the designed alloys exhibited microstructural heterogeneity and hierarchy (MHH), and thus could leverage the unique process dynamics of L-PBF to produce a fine-tunable MHH and mechanical behavior. Furthermore, alloy chemistry-based fine tuning of the stacking fault energy has led to transformative damage tolerant alloys. Such alloys can shield defects stemming from the stochastic powder bed in L-PBF, and consequently can prevent catastrophic failure despite the solidification defects. A modified materials systems approach that explicitly includes alloy chemistry as a means to modify the printability, properties and performance with F-BAM is also presented. Overall, this work is expected to facilitate application specific manufacture with F-BAM and eventually facilitate widespread adoption of F-BAM in structural application.

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