Electron beam powder bed fusion (PBF-EB/M) has been attracting great research interest as a promising technology for additive manufacturing of titanium aluminide alloys. However, challenges often arise from the process-induced evaporation of aluminum, which is linked to the PBF-EB/M process parameters. This study applies different volumetric energy densities during PBF-EB/M processing to deliberately adjust the aluminum contents in additively manufactured Ti–43.5Al–4Nb–1Mo–0.1B (TNM-B1) samples. The specimens are subsequently subjected to hot isostatic pressing (HIP) and a two-step heat treatment. The influence of process parameter variation and heat treatments on microstructure and defect distribution are investigated using optical and scanning electron microscopy, as well as X-ray computed tomography (CT). Depending on the aluminum content, shifts in the phase transition temperatures can be identified via differential scanning calorimetry (DSC). It is confirmed that the microstructure after heat treatment is strongly linked to the PBF-EB/M parameters and the associated aluminum evaporation. The feasibility of producing locally adapted microstructures within one component through process parameter variation and subsequent heat treatment can be demonstrated. Thus, fully lamellar and nearly lamellar microstructures in two adjacent component areas can be adjusted, respectively.

<p></p><p>This doctoral dissertation takes the reader through a journey where applied shear rheology and flow-velocimetry are used to understand the mesoscopic factors that control the flow behavior of three microstructured fluids. Three individual protocols that measure relative physical and mechanical properties of the flow are developed. Each protocol aims to advance the particular transformation of novel soft materials into a commercial product converging in the demonstration of the real the chemical, physical and thermodynamical factors that could potentially drive their successful transformation. </p> <p> </p> <p>First, this dissertation introduces the use of rotational and oscillatory shear rheometry to quantify the solvent evaporation effect on the flow behavior of polymer solutions used to fabricate isoporous asymmetric membranes. Three different A-B-C triblock copolymer were evaluated: polyisoprene-<i>b</i>-polystyrene-<i>b</i>-poly(4-vinylpyridine) (ISV); polyisoprene-<i>b</i>-polystyrene-<i>b</i>-poly(<i>N</i>,<i>N</i>-dimethylacrylamide) (ISD); and polyisoprene-<i>b</i>-polystyrene-<i>b</i>-poly(<i>tert</i>-butyl methacrylate) (ISB). The resulting evaporation-induced microstructure showed a solution viscosity and film viscoelasticity strongly dependent on the chemical structure of the triblock copolymer molecules. </p> <p> </p> <p>Furthermore, basic shear rheometry, flow birefringence, and advanced flow-velocimetry are used to deconvolute the flow-microstructure relationships of concentrated surfactant solutions. Sodium laureth sulfate in water (SLE₁S) was used to replicate spherical, worm-like, and hexagonally packed micelles and lamellar structures. Interesting findings demonstrated that regular features of flow curves, such as power-law shear thinning behavior, resulted from a wide variety of experimental artifacts that appeared when measuring microstructured fluids with shear rheometry.</p> <p> </p> <p>Finally, the successful integration of shear rheometry to calculate essential parameters to be used in a cost-effective visualization technique (still in development) used to calculate the dissolution time of polymers is addressed. The use of oscillatory rheometry successfully quantify the viscoelastic response of polyvinyl alcohol (PVA) solutions and identify formulations changes such as additive addition. The flow behavior of PVA solutions was correlated to dissolution behavior proving that the developed protocol has a high potential as a first screening tool.</p><br><p></p>

The compression behavior of a newly developed near eutectic Al-Si based cast alloy with three different microstructures has been investigated in the present work. Microstructures with modified and unmodified Si particles and matrix with different tempers are investigated. The main objective of this work is to understand the effect of heat treatment and modification on the fracture behavior of the alloy under compression. This alloy is subjected to compressive loading at different strain rates and temperatures during the operation of the engines. Hence, the effect of strain rates and temperatures is also considered. The compression tests are carried out at different strain rates from quasi-static to dynamic viz., 3*10-4 to 102/s and three different temperatures RT, 100°C and 200°C. Microstructure of the alloys studied predominantly consists of eutectic colonies of α-Al and Si with a few interspersed α-Al dendrites. Modified alloy has more globular Si particles than unmodified alloy. Heat treated alloys are found to have hardening precipitates S’ & Al7Cu4Ni and 3-7 atomic layer thick zones, which may be precursors to S’ phase. A variety of large intermetallics, viz., plate like particles Al4.5FeSi, Chinese script like particles Al19Fe4MnSi2 and bulky phase Al3NiCu are also observed in the alloys. Mechanical behavior of the alloys is found to be different for different microstructures. Modification improves strength and ductility. Heat treatment improves strength of the alloy at the expense of ductility. A transition in mechanical behavior is observed after a particular strain rate for all the alloys studied. This transition strain rate is dependent on heat treatment, Si particle size and temperature. This transition can be explained on the basis of dislocation-precipitate and dislocation-Si particle interactions. Work hardening behavior of the alloys depends on the matrix microstructure in the unmodified alloys, and both matrix and particles play a role in the modified alloy. A statistically robust quantitative micro structural analysis has been carried out after compressing the samples at various strain rates and temperatures. The unique contribution of this work is the understanding of combined effect of strain rate and temperature on Si particle fracture characteristics in the alloy with different microstructures. From the fracture characteristics of Si particles, it is concluded that both dislocation pile-up mechanism and fibre loading are responsible for particle fracture in the modified alloy, whereas the fibre loading mechanism alone is sufficient to explain the particle fracture characteristics in the unmodified alloy. Si particles in the modified condition are found to cleave along the lowest surface energy planes {112} & {110} and the particles with orientations {112} & {111} are more prone to fracture. In addition to Si particle fracture, elongated Fe rich intermetallic particles are also seen to show peculiar fracture behavior. The Al4.5FeSi intermetallics with (100) as the plane of the plate cleave along (100) planes. This is a novel finding in this work and could have immense implications on the role of Fe impurities in the fracture behavior of these alloys. Moreover, since these cleavage fractures are seen to be more than 200 microns in size (which implies that the real penny shaped crack would be even larger) their role cannot be assumed to be negligible, as was previously thought. The load sharing between the Al matrix and eutectic Si particles are simulated by microstructure based finite element modeling. The program OOF (Object-Oriented Finite element analysis) is used to generate the finite element meshes for real microstructures with different Si morphology. The experimentally obtained stress – strain properties of the alloy is given as an input to describe the plastic behavior of the Al matrix, in the finite element simulation. This analysis helps to understand the effect of particle size, shape, orientation & clustering and matrix temper on the stress transferred to the Si particles. Combination of Electron Back-Scattered Diffraction (EBSD) and frequency shift, polarized micro-Raman technique is applied to validate the stress states in Si particles with {111} orientations. The stress at fracture of Si particles is also estimated from Raman technique. Even though the alloys with different microstructures show different mechanical behavior, the sequence of fracture mechanisms is found to be same for all the alloys. The failure occurs in three stages: cracking of Si particles at low strains, micro-crack formation along the fractured particles, micro-crack coalescence and propagation leading to final failure. Thus, the proposed analysis links various deformation mechanisms ranging from nano precipitate-dislocation interactions to micro short-fiber theory of load sharing by eutectic silicon along with coupled effect of strain rate and temperature. In addition, negative strain rate sensitivity is also observed in the lower strain rate regimes (3*10-4, 10-3& 102/s) at RT and 100°C for all the three alloys, and serrated flow is also observed in the same strain rate and temperature regimes. Some of the features of serrated flow can be explained by the dynamic strain aging model and some other features by precipitate shearing.

Additive manufacturing (AM) introduces high variability in the microstructure and defect distributions, compared with conventional processing techniques, which introduces greater uncertainty in the resulting fatigue performance of manufactured parts. As a result, qualification of AM parts poses as a problem in continued adoption of these materials in safety-critical components for the aerospace industry. Hence, there is a need to develop precise and accurate, physics-based predictive models to quantify the fatigue performance, as a means to accelerate the qualification of AM parts. The fatigue performance is a critical requirement in the safe-life design philosophy used in the aerospace industry. Fatigue failure is governed by the loading conditions and the attributes of the material microstructure, namely, grain size distribution, texture, and defects. In this work, the crystal plasticity finite element (CPFE) method is employed to model the microstructure-based material response of an additively manufactured Ni-based superalloy, Inconel 718 (IN718). Using CPFE and associated experiments, methodologies were developed to assess multiple aspects of the fatigue behavior of IN718 using four studies. In the first study, a CPFE framework is developed to estimate the critical characteristics of porosity, namely the pore size and proximity that would cause a significant debit in the fatigue life. The second study is performed to evaluate multiple metrics based on plastic strain and local stress in their ability to predict both the modes of failure as seen in fractography experiments and estimate the scatter in fatigue life due to microstructural variability as obtained from fatigue testing. In the third study, a systematic analysis was performed to investigate the role of the simulation volume and the microstructural constraints on the fatigue life predictions to provide informed guidelines for simulation volume selection that is both computationally tractable and results in consistent scatter predictions. In the fourth study, validation of the CPFE results with the experiments were performed to build confidence in the model predictions. To this end, 3D realistic microstructures representative of the test specimen were created based on the multi-modal experimental data obtained from high-energy diffraction experiments and electron backscatter diffraction microscopy. Following this, the location of failure is predicted using the model, which resulted in an unambiguous one to one correlation with the experiment. In summary, the development of microstructure-sensitive predictive methods for fatigue assessment presents a tangible step towards the adoption of model-based approaches that can be used to compliment and reduce the overall number of physical tests necessary to qualify a material for use in application.

Im Rahmen der vorliegenden Arbeit wurde ein Spritzgießwerkzeug mit einem neuartigen Mehrschichtverbundheizsystem zur dynamischen Temperierung entwickelt und umgesetzt. Dabei wurde das ausgewählte Heiz‐ und Kühlsystem unter theoretischen und praktischen Gesichtspunkten betrachtet und für den variothermen Fertigungsprozess verifiziert. Aus den ersten durchgeführten praktischen Versuchen zeigte sich, dass dieses Heizsystem zur dynamischen Temperierung von Formwerkzeugen geeignet ist. Anschließend wurden mit dem realisierten Spritzgießwerkzeug Versuchskörper mit spezieller Oberflächenstrukturierung und variierenden Werkzeugwandtemperaturen angefertigt und untersucht. Ziel war es, über diese Strukturierung eine Beeinflussung der Glasfaserverteilung im Formteilrandbereich zu erreichen und die tribologischen Eigenschaften bei Kunststoff‐Kunststoff‐Gleitpaarungen hinsichtlich Reibung und Verschleiß zu verbessern. Mit einer kleinen Auswahl an Strukturen und entsprechenden thermoplastischen Polymermaterialien wurden praktische Versuche zur tribologischen Prüfung durchgeführt. / In the present work an injection mould was developed and implemented with a novel multilayer composite heating system for dynamic temperature control. Here the selected heating and cooling system was considered from a theoretical and practical point of view and verified for the variothermal manufacturing process. The first practical tests showed that this heating system is suitable for the dynamic temperature control of tools. Subsequently, with this injection mould, test specimens with a special surface structure and varying mould wall temperatures were produced and examined. The aim was to achieve through this structuring an impact on the distribution of glass fibres in the edge region of mouldings and improve the tribological properties of plastic‐plastic‐pairings in terms of friction and wear. With a small selection of structures and corresponding thermoplastic polymeric materials practical experiments for tribological testing were performed.

<div>In this thesis, the role of location-specific microstructural features in the fatigue performance of the safety-critical aerospace components made of Nickel (Ni)-base superalloys and linear friction welded (LFW) Titanium (Ti) alloys has been studied using crystal plasticity finite element (CPFE) simulations, energy dispersive X-ray diffraction (EDD), backscatter electron (BSE) images and digital image correlation (DIC).</div><div><br></div><div>In order to develop a microstructure-sensitive fatigue life prediction framework, first, it is essential to build trust in the quantitative prediction from CPFE analysis by quantifying uncertainties in the mechanical response from CPFE simulations. Second, it is necessary to construct a unified fatigue life prediction metric, applicable to multiple material systems; and a calibration strategy of the unified fatigue life model parameter accounting for uncertainties originating from CPFE simulations and inherent in the experimental calibration dataset. To achieve the first task, a genetic algorithm framework is used to obtain the statistical distributions of the crystal plasticity (CP) parameters. Subsequently, these distributions are used in a first-order, second-moment method to compute the mean and the standard deviation for the stress along the loading direction (σ_load), plastic strain accumulation (PSA), and stored plastic strain energy density (SPSED). The results suggest that an ~10% variability in σ_load and 20%-25% variability in the PSA and SPSED values may exist due to the uncertainty in the CP parameter estimation. Further, the contribution of a specific CP parameter to the overall uncertainty is path-dependent and varies based on the load step under consideration. To accomplish the second goal, in this thesis, it is postulated that a critical value of the SPSED is associated with fatigue failure in metals and independent of the applied load. Unlike the classical approach of estimating the (homogenized) SPSED as the cumulative area enclosed within the macroscopic stress-strain hysteresis loops, CPFE simulations are used to compute the (local) SPSED at each material point within polycrystalline aggregates of 718Plus, an additively manufactured Ni-base superalloy. A Bayesian inference method is utilized to calibrate the critical SPSED, which is subsequently used to predict fatigue lives at nine different strain ranges, including strain ratios of 0.05 and -1, using nine statistically equivalent microstructures. For each strain range, the predicted lives from all simulated microstructures follow a log-normal distribution; for a given strain ratio, the predicted scatter is seen to be increasing with decreasing strain amplitude and are indicative of the scatter observed in the fatigue experiments. Further, the log-normal mean lives at each strain range are in good agreement with the experimental evidence. Since the critical SPSED captures the experimental data with reasonable accuracy across various loading regimes, it is hypothesized to be a material property and sufficient to predict the fatigue life.</div><div><br></div><div>Inclusions are unavoidable in Ni-base superalloys, which lead to two competing failure modes, namely inclusion- and matrix-driven failures. Each factor related to the inclusion, which may contribute to crack initiation, is isolated and systematically investigated within RR1000, a powder metallurgy produced Ni-base superalloy, using CPFE simulations. Specifically, the role of the inclusion stiffness, loading regime, loading direction, a debonded region in the inclusion-matrix interface, microstructural variability around the inclusion, inclusion size, dissimilar coefficient of thermal expansion (CTE), temperature, residual stress, and distance of the inclusion from the free surface are studied in the emergence of two failure modes. The CPFE analysis indicates that the emergence of a failure mode is an outcome of the complex interaction between the aforementioned factors. However, the possibility of a higher probability of failure due to inclusions is observed with increasing temperature, if the CTE of the inclusion is higher than the matrix, and vice versa. Any overall correlation between the inclusion size and its propensity for damage is not found, based on inclusion that is of the order of the mean grain size. Further, the CPFE simulations indicate that the surface inclusions are more damaging than the interior inclusions for similar surrounding microstructures. These observations are utilized to instantiate twenty realistic statistically equivalent microstructures of RR1000 – ten containing inclusions and remaining ten without inclusions. Using CPFE simulations with these microstructures at four different temperatures and three strain ranges for each temperature, the critical SPSED is calibrated as a function of temperature for RR1000. The results suggest that critical SPSED decreases almost linearly with increasing temperature and is appropriate to predict the realistic emergence of the competing failure modes as a function of applied strain range and temperature.</div><div><br></div><div>LFW process leads to the development of significant residual stress in the components, and the role of residual stress in the fatigue performance of materials cannot be overstated. Hence, to ensure fatigue performance of the LFW Ti alloys, residual strains in LFW of similar (Ti-6Al-4V welded to Ti-6Al-4V or Ti64-Ti64) and dissimilar (Ti-6Al-4V welded to Ti-5Al-5V-5Mo-3Cr or Ti64-Ti5553) Ti alloys have been characterized using EDD. For each type of LFW, one sample is chosen in the as-welded (AW) condition and another sample is selected after a post-weld heat treatment (HT). Residual strains have been separately studied in the alpha and beta phases of the material, and five components (three axial and two shear) have been reported in each case. In-plane axial components of the residual strains show a smooth and symmetric behavior about the weld center for the Ti64-Ti64 LFW samples in the AW condition, whereas these components in the Ti64-Ti5553 LFW sample show a symmetric trend with jump discontinuities. Such jump discontinuities, observed in both the AW and HT conditions of the Ti64-Ti5553 samples, suggest different strain-free lattice parameters in the weld region and the parent material. In contrast, the results from the Ti64-Ti64 LFW samples in both AW and HT conditions suggest nearly uniform strain-free lattice parameters throughout the weld region. The observed trends in the in-plane axial residual strain components have been rationalized by the corresponding microstructural changes and variations across the weld region via BSE images. </div><div><br></div><div>In the literature, fatigue crack initiation in the LFW Ti-6Al-4V specimens does not usually take place in the seemingly weakest location, i.e., the weld region. From the BSE images, Ti-6Al-4V microstructure, at a distance from the weld-center, which is typically associated with crack initiation in the literature, are identified in both AW and HT samples and found to be identical, specifically, equiaxed alpha grains with beta phases present at the alpha grain boundaries and triple points. Hence, subsequent fatigue performance in LFW Ti-6Al-4V is analyzed considering the equiaxed alpha microstructure.</div><div><br></div><div>The LFW components made of Ti-6Al-4V are often designed for high cycle fatigue performance under high mean stress or high R ratios. In engineering practice, mean stress corrections are employed to assess the fatigue performance of a material or structure; albeit this is problematic for Ti-6Al-4V, which experiences anomalous behavior at high R ratios. To address this problem, high cycle fatigue analyses are performed on two Ti-6Al-4V specimens with equiaxed alpha microstructures at a high R ratio. In one specimen, two micro-textured regions (MTRs) having their c-axes near-parallel and perpendicular to the loading direction are identified. High-resolution DIC is performed in the MTRs to study grain-level strain localization. In the other specimen, DIC is performed on a larger area, and crack initiation is observed in a random-textured region. To accompany the experiments, CPFE simulations are performed to investigate the mechanistic aspects of crack initiation, and the relative activity of different families of slip systems as a function of R ratio. A critical soft-hard-soft grain combination is associated with crack initiation indicating possible dwell effect at high R ratios, which could be attributed to the high-applied mean stress and high creep sensitivity of Ti-6Al-4V at room temperature. Further, simulations indicated more heterogeneous deformation, specifically the activation of multiple families of slip systems with fewer grains being plasticized, at higher R ratios. Such behavior is exacerbated within MTRs, especially the MTR composed of grains with their c-axes near parallel to the loading direction. These features of micro-plasticity make the high R ratio regime more vulnerable to fatigue damage accumulation and justify the anomalous mean stress behavior experienced by Ti-6Al-4V at high R ratios.</div><div><br></div>