Additive manufacturing (AM) processes may introduce large residual stresses in the as-built part, in particular the laser powder bed fusion process (L-PBF). The residual stress state is an inherent consequence of the heterogeneous heating and subsequent cooling during the process. L-PBF has become renowned for its “free complexity” and rapid prototyping capabilities. However, it is vital to ensure shape stability after the component is removed from the build plate, which can be problematic due to the residual stress inducing nature of this manufacturing process. Residual stresses can be analyzed via many different characterization routes (e.g. X-ray and neutron diffraction, hole drilling, etc.), both quantitatively and qualitatively. From an industrial perspective, most of these techniques are either prohibitively expensive, complex or too slow to be implementable during the early prototyping stages of AM manufacturing. In this work a deformation based method employing a specific geometry, a so called “keyhole”-geometry, has been investigated to qualitatively evaluate the effect of different stress relief annealing routes with respect to macroscopic part deformation, mechanical properties and microstructure. Previous published work has focused on structures with open geometry, commonly referred to as bridge-like structures where the deformation required for analysis occurs during removal from the build plate. The proposed keyhole-geometry can be removed from the build plate without releasing the residual stresses required for subsequent measurement, which enables bulk manufacturing on single build plates, prior to removal and stress relief annealing.  Two L-PBF manufactured austenitic stainless steel alloys were studied, 316L and 21-6-9. Tensile specimen blanks were manufactured and the subsequent heat treatments were carried out in pairs of keyhole and tensile blank. Both a contact (micrometer measurement), and a non-contact (optical profilometry) method were employed to measure the residual stress induced deformation in the keyholes. The annealing heat treatment matrix was iteratively expanded with input from the deformation analysis to find the lowest temperature at which approximately zero deformation remained after opening the structure via wire electrical discharge machining. The lowest allowable annealing temperature was sought after to minimize strength loss.  After stress relief annealing at 900 ℃ for 1 hour, the 316L keyhole-geometry was considered shape stable. The lateral micrometer measurement yielded a length change of 1 µm, and a radius of 140 m (over the 22 mm top surface) was assigned from curve fitting the top surface height profiles. The complementary microstructural characterization revealed that this temperature corresponded to where the last remains of the cellular sub-grain structures disappears. Tensile testing showed that the specimen subjected to the 900 ℃ heat treatment had a marked reduction in yield stress (YS) compared to that of the as-built: 540 MPa → 402 MPa, whereas ultimate tensile strength (UTS) only reduced slightly: 595 MPa → 570 MPa. The ductility (4D elongation) was found to be ~13 % higher for the specimen heat treated at 900 ℃ than that of the as-built specimen, 76% and 67% respectively.  For alloy 21-6-9 the residual stress induced deformation minimum (zero measurable deformation) was found after stress relief heat treatment at 850 ℃ for 1 hour. Slight changes in the microstructure were observable through light optical microscopy when comparing the different heat treatment temperatures. The characteristic sub-grain features associated with alloy 316L were not verified for alloy 21-6-9. Similar to the results for 316L, UTS was slightly lower for the tensile specimen subjected to the heat treatment temperature required for shape stability (850 ℃) compared to the as-built specimen: 810 MPa → 775 MPa. The measured ductility (4D elongation) was found to be approximately equal for the as-built (47%), and heat treated (48%) specimen. As-built material exhibited a YS of 640 MPa while the heat treated specimen had a YS of 540 MPa. For alloy 21-6-9, the lateral micrometer deformation measurements were compared with stress relaxation testing performed at 600 ℃, 700℃ and 800 ℃. Stress relaxation results were in good agreement with the results from the lateral deformation measurements.  The study showed that for both steel alloys, the keyhole method could be successfully employed to rapidly find a suitable stress relief heat treatment route when shape stability is vital.

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)

No description available.

Laser powder bed fusion is an additive manufacturing technique that is capable of building metallic parts by spreading many layers of metal powder over a build surface and using a laser to melt specific sections of the surface. The part is built by melting consecutive layers on top of each other until the design is completed. However, during this process defects can occur. These defects have impacts on the part’s physical properties, and it is important to detect them for quality assurance. A single part takes several hundred or thousands of layers to build. While each layer is built, cameras and sensors are used to create images of each layer. These images are used for identification and classification of defects that could have a negative impact on a printed part’s physical properties, such as tensile strength. Classification of defects would reduce manual inspection of the printed part. Thus, the classification of defects in each layer must be automated, as it would be infeasible to manually classify each layer. Recently, machine learning have proven to be an effective method for automating defect classification in laser powder bed fusion. However, machine learning and especially deep-learning approaches generally require a large amount of labeled training data, which is typically not available for laser powder bed fusion printed parts. Labeling of images requires manual labor and domain knowledge. One of the greatest obstacles in defect classification, is how machine learning can be applied despite this absence of labeled data. A machine learning approach that show potential for being trained with less data, is the siamese neural network approach. In this thesis, a novel approach for automating defect classification is developed, using layer images from a laser powder bed fusion printing process. In order to cope with the limited access to labeled data, the classifiers are based on the siamese neural network structure. Two siamese neural network structures are developed, a one-shot classifier, which directly classifies the instance, and a hierarchical classifier with a hierarchical classification process according to the hierarchy of the defect classes. The classifiers are evaluated by inferring a test set of images collected from the laser powder bed fusion process. The one-shot classifier is able to classify the images with an accuracy of 70%and the hierarchical classifier with an accuracy of 86%. For the hierarchical classifier area of the ROC curves were calculated to be, 0.96 and 0.95 for the normal vs defect and overheating vs spattering stages respectively. Unlabeled images were added to the training set of a new instance of the hierarchical classifier, which could infer the test set without any major changes to test set accuracy.

Laser-material interaction of Nickel based superalloy Haynes 282 melt pools were studied for laser parameters similar to laser powder bed fusion (PBF-LB) without powder. The effect of power, speed, hatch distance and laser focus offset were analysed by characterizing different types of melt pool behaviour, including conduction, transition to keyhole, and keyhole mode. Focus offset parameter was found to modify the melting mode from keyhole to conduction type in experiments with and without powder. This change in melting mode is attributed to the variation in laser beam spot size for the same line energy. Such manipulation of type of melting with control of focus offset can be utilized as a method to optimize process parameters for novel materials in the PBF-LB process at high layer thickness. Based on the above study, cubes were built with refined process parameters utilizing powder layer thicknesses of 60- and 90-microns for improved productivity, using partial factorial design of experiment. The conduction mode of melting helped reducing defects, minimizing lack of fusion and keyhole porosity in specimens built with powder at 60- and 90-microns layer thickness. Effect of process parameters and indirect measure like area energy, on the melt pool overlap, defect level and dominant shape of the defects are presented. Optimizing the process parameters to identify the boundaries for building cubes with reduced porosity is also discussed. / Den Ni-baserade superlegeringen, Haynes 282, skannades med laserparametrar liknande de som används i laserpulverbäddfusion (PBF-LB), men utan pulver.Studien undersökte inverkan av effekt, hastighet, avstånd mellan två intilliggandeskanningspass och laserfokusförskjutning, vilket karakteriserades genom olikatyper av beteenden hos smältbadet, inklusive värmeledning, övergång frånvärmeledning till nyckelhål, och nyckelhål. Fokusförskjutningen visade sig ändrasmältbadets läge från nyckelhål till värmeledning. Denna förändring observeradesbåde i experiment utan pulver och i de med pulver. Förändringen beror påbreddningen av laserstrålens punktstorlek samtidigt som samma linjeenergibibehålls. Denna förändring i smältningstyp genom fokusförskjutning kananvändas som en metod för att optimera utforskningen av nya material i PBFLB-processen. Baserat på detta byggdes kuber med pulver med lagertjocklekar på 60 och 90mikrometer, användande olika processparametrar enligt en experimentell designbaserad på en central sammansatt design. Smältning genom värmeledning bidrogtill att minska defekter, minimera bindningsfel och nyckelhålsporositet i proversom byggts med pulver med lagertjocklekar på 60 och 90 mikrometer. Inverkanav processparametrarna och indirekta mått såsom areaenergi på smältbadetsöverlappning, defektnivå och den dominerande formen på defekter presenteras.Optimering av processparametrarna samt identifiering av parameterrymden föratt bygga kuber med minskad porositet undersöks också. / <p>Paper A is to be submitted, and paper C is acceptet and are not included in this licentiate thesis. We do  not have permission to publish paper B in the digital version.</p>

This work investigates the influence of microstructure and cooling and heating rates on the physical and chemical properties of fast crystallizing polymers. The primary objectives were to 1) utilize advanced methodologies to accurately determine the fundamental thermodynamic value of equilibrium melting temperature (Tmo) for the semi-crystalline polymer poly(ether ketone ketone) (PEKK), 2) increase understanding of the influence of microstructure (random versus blocky) of functionalized semi-crystalline polymers on physical and chemical properties, and 3) understand the influence of additive manufacturing process parameters on semi-crystalline polymer crystallization and final properties. All objectives utilized the advanced characterization technique of fast scanning calorimetry (FSC) using the Mettler Toledo Flash DSC 1. The first half of this work focuses on the high-performance semi-crystalline aromatic polymer poly(ether ketone ketone) (PEKK) with a copolymerization ratio of terephthalate to isophthalate moieties (i.e., T/I ratio) of 80/20. Due to the fast heating and cooling rates of the Flash DSC, PEKK underwent melt-reorganization upon heating at slow heating rates. This discovery resulted in utilizing a Hoffman-Weeks linear extrapolation of the zero-entropy production temperature to establish a new equilibrium melting temperature of 382 oC. Additionally, a new NMR solvent, dichloroacetic acid, was discovered for PEKK, allowing for comprehensive NMR analysis of PEKK for the first time. Diphenyl acetone (DPA) was discovered as a novel, benign gelation solvent for PEKK, enabling heterogeneous gel-state bromination and sulfonation to afford blocky microstructures. The gel state functionalization process resulted in a blocky microstructure with runs of pristine crystallizable PEKK retained within the crystalline domains, and amorphous domains containing the functionalized PEKK monomers. The preservation of the pristine crystalline domains resulted in enhanced physical and chemical properties compared to the randomly functionalized analogs. Additionally, heterogeneous gel state functionalization of PEKK gels prepared from different solvents and gelation temperatures resulted in differences in crystallization behavior between blocky microstructures of the same degree of functionalization. This result demonstrates that the blocky microstructure can be tuned through controlling the starting gel morphology. The second half of this work focuses on understanding the influence of cooling and heating rates on the melting, crystal morphology, and crystallization kinetics on isotactic polypropylene (iPP), iPP-polyethylene copolymers (iPP-PE), and iPP/iPP-PE blends and using this information to gain understanding of how these polymers crystallize during the additive manufacturing processes of powder bed fusion (PBF) and material extrusion (MatEx). The crystallization kinetics of iPP, iPP-PE copolymers, and iPP/iPP-PE blends exhibited bimodal parabolic-like behavior attributed to crystallization of the mesomorphic crystal polymorph at low temperatures and the α-form crystal at high temperatures. Incorporation of non-crystallizable polyethylene fractions both covalently and blended as a secondary component, resulted in decreasing crystallization rates, inhibition of crystallization, and decreased crystallizability. Additionally, the non-isothermal crystallization behavior of these systems shows that the non-crystallizable fractions influence the crystal nucleation density and temperature at which polymorphic crystallization occurs. Utilizing in-situ IR thermography in the PBF system, the heating and cooling rates observed for a single-layer PBF print were used to mimic the PBF process by FSC. Partial melting in the printing process leads to self-seeding and increased crystallization onset temperatures upon cooling, which influences the final part melting morphology. Nucleation from surrounding powder and partially melted crystals greatly influences the crystallization kinetics and crystal morphology of the final part. Utilizing rheological experiments and process-relevant cooling rates observed in the MatEx process, the miscibility of iPP/iPP-PE blends influenced the nucleation behavior and crystallization rates, subsequently leading to differences in printed part properties. / Doctor of Philosophy / The crystalline morphology of semi-crystalline polymers depends on their microstructure and thermal history. The resultant crystalline morphology greatly affects the physical and chemical properties. In the first part of this work, the effect of microstructure on material properties is explored. Block copolymer microstructures consist of two or more blocks of distinct polymer segments covalently bonded to one another. This leads to self-organization of the components into unique structural order that would not be attainable if the polymer segments were randomly bonded together. This structural order enhances material properties; thus, block copolymers are advantageous for many applications. However, synthesis of block copolymers can be tedious and expensive. Thus, additional methodologies for block copolymer synthesis are desired. In this work blocky (i.e., statistically non-random) copolymers are synthesized through a facile post-polymerization functionalization method. These blocky copolymers result in enhanced physical and chemical properties compared to the randomly synthesized analogs. This work shows blocky functionalization of a new polymer under new post-polymerization conditions and expands upon the synthesis methodology for block copolymers. In the second part of this work, the effect of heating and cooling rates on the formation of crystals during additive manufacturing is explored. Additive manufacturing modalities of powder bed fusion and material extrusion consist of rapid heating and cooling processes, which can affect how crystals form and ultimately affect the final printed part properties. Using a technique called fast scanning calorimetry, the different heating and cooling rates that the polymer witnesses during printing can be mimicked, and the formation of crystals under these different conditions can be replicated. This mimicking analysis can be related to the printing process and be used to help guide printing processes to enhance printed part properties.

<p>The Powder Bed Fusion (PBF) process is increasingly employed by industry to fabricate complex parts with stringent standard criteria. However, fabricating parts free of defects using this process is still a major challenge. As reported in the literature, thermally induced abnormalities form the majority of generated defects and are largely attributed to thermal evolution. Various methodologies have been introduced in the literature to eliminate or mitigate such abnormalities. However, most of these methodologies are post-process in nature, lacking adaptability and customization to accommodate different geometries or materials. Consequently, they fall short of adequately addressing these challenges. Monitoring and controlling temperature, along with its distribution throughout each layer during fabrication, is an effective and efficient proxy to control the thermal evolution of the process. This, in turn, provides a real-time solution to effectively overcome such challenges. </p> <p>The objective of this dissertation is to introduce a novel online thermography and closedloop hybrid-control (NOTCH)©, an ultra-fast and practical control approach, to modify the scan strategy in metal PBF in real time. This methodology employs different mathematical-thermophysical concept-based or thermophysical-based models combined with optimization algorithms designed to optimize the printing sequence of islands/stripes/zones in order to avoid or mitigate residual stress and distortion. This methodology is adaptable to different geometries, dimensions, and materials, and is capable of being used with machines having varying ranges of specifications. </p> <p>NOTCH’s objective is to achieve a uniform temperature distribution throughout an entire layer and through the printed part (between layers) to mitigate residual stress and thermally related distortion. To attain this objective, this study explores modifying or optimizing the printing sequence of islands/stripes in an island or the strip scanning strategy. This dissertation presents three key contributions: </p> <p>First, this work introduces two potential models: the Genetic Algorithm Maximum Path (GAMP) strategy and Generalized Advanced Graph Theory. Preliminary results for a printed/simulated prototype are presented. These models, along with the Tessellation algorithm (developed in my M.Sc. thesis), were employed within NOTCH.</p> <p>Second, I developed two optimization algorithms based on the greedy and evolutionary approaches. Both algorithms are direct-derivative-free methods. The greedy optimization provides a definitive solution at each printing step, selecting the island/stripe that ensures the highest temperature uniformity. Conversely, the evolutionary algorithm seeks to obtain the final optimal solution at the end of the printing process, i.e., the printing sequence with the highest uniformity in the last printing step. This approach is inspired by the concept of Random Search algorithms, offering a non-definitive solution to find an optimal solution. </p> <p>Last, this work presents the NOTCH methodology, enabling real-time modification of printing sequences through the integration of a novel thermography methodology (developed in my M.Sc. thesis), developed models, and optimization algorithms.</p> <p><br></p>

This study aims to introduce a new qualification approach designed to enhance the overall integrity of complex cooling structures in gas turbine blades produced through 3D printing, with a focus on achieving maximum density. The primary objective is to present a comprehensive qualification and validation methodology tailored for components manufactured via binder jetting printing and non-selective laser melting (SLM) powder-based atomic diffusion additive manufacturing. This innovative qualification approach undergoes validation through stages encompassing design, printing, comprehension of thermal debinding and sintering processes, post-processing, optimization, and characterization, all aimed at achieving complex cooling structures with optimal density using stainless steel material and In718 as a case study. Subsequently, the material properties obtained are compared with those of IN718 produced via laser-based manufacturing. Thorough characterization is conducted before and after sintering to assess the impact of sintering on density enhancement. Experimental optimization employing the Taguchi matrix with an L9 orthogonal array involves the selection of three key parameters: sintering time, sintering temperature, and heat treatment. The procedural framework established in this research applies to high-temperature applications wherein components are fabricated using atomic diffusion additive manufacturing or binder jetting printing techniques. Testing and inspection procedures involve neutron scattering, radiography, and CT scanning methods, with a specific emphasis on neutron scattering measurements conducted under externally heated and internally cooled conditions to evaluate residual strains within the gas turbine environment. Understanding the interplay between residual stresses originating from manufacturing processes and thermal stresses provides valuable insights into the impact of additive manufacturing on component performance in thermal environments, thus contributing to the advancement of the proposed study.

<p dir="ltr">The increasing use of additive manufacturing technologies such as Laser Powder Bed Fusion (LPBF) has enabled the manufacturing of parts with complex features such as optimized cooling channels. However, due to the layer-by-layer deposition of LPBF requiring an approximation of design intent, cooling channels manufactured by LPBF are affected by surface roughness effects and manufacturing inaccuracies. Consequently, the effect of implementing them on the mechanical properties of parts should be studied to understand their limits of applicability. This study aims to determine the effect of helical cooling channels in LPBF GRCop-42 specimens on their high-cycle fatigue properties. We present monotonic tensile testing and high-cycle fatigue testing results for three specimen types (no channel, straight channel and helical channel) of LPBF GRCop-42 under uniaxial loading, tested at two temperature conditions (room and 500°C). We show that at room temperature, the no channel specimens had the highest fatigue strength, followed by the straight channel and then helical channel specimens. The relative significance of potential causes for the detriment in fatigue life for the straight and helical channeled specimens were quantified using finite element analysis (FEA) and analytical fatigue models (based on Murakami-type defect corrections), and the findings from this analysis were validated by experimental observations from fracture surface analysis. Our results demonstrate that for the straight channel specimens, manufacturing-induced porosity around the channel is relatively a stronger driver for the detriment of fatigue life, compared to surface roughness. For the helical channel specimens, intended to simulate complex cooling channels in real-world applications, the effects of surface roughness combined with multiaxial stress concentrations around the channel were the primary driver for the lesser fatigue life. We anticipate our results will be useful for designers and manufacturers of LPBF components with complex features, and those involved in the potential implementation of LPBF GRCop-42 parts in high-cycle fatigue applications.</p>

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.