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Paper des Monats
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In the past two decades, numerous relaxation or physical aging experiments of metallic glasses have revealed signatures of intermittent atomic-scale processes. Revealed via intensity cross-correlations from coherent scattering using X-ray photon correlation spectroscopy (XPCS), the observed abrupt changes in the time-domain of atomic motion does not fit the picture of gradual slowing down of relaxation times and their origin continues to remain unclear. Using a binary Lennard-Jones model glass subjected to microsecond-long isotherms, we show here that temporally and spatially heterogeneous atomic-cluster activity at different length-scales drive the emergence of highly non-monotonous intensity cross-correlations. The simulated XPCS experiments reveal a variety of time-dependent intensity-cross correlations that, depending on both the structural evolution and the 𝑞-space sampling, give detailed insights into the possible structural origins of intermittent aging measured with XPCS.
Mean-field modeling and Phase-field simulation of Grain Growth under Directional driving forces
(2024)
Directional grain growth is a common phenomenon in the synthetic and natural evolution of various polycrystals. It occurs in the presence of an external driving force, such as a temperature gradient, along which grains show a preferred, yet competitive, growth. Novel additive manufacturing processes, with intense, localized energy deposition, are prominent examples of when directional grain growth can occur, beneath the melting pool. In this work, we derive a phenomenological mean-field model and perform 3D phase-field simulations to investigate the directional grain growth and its underlying physical mechanisms. The effect of the intensity of driving force is simulated and systematically analyzed at the evolving growth front as well as various cross-sections perpendicular to the direction of the driving force. We found that although the directional growth significantly deviates from normal grain growth, it is still governed by a power law relation <R> \propto t^n with an exponent n ~ 0.6–0.7. The exponent
exhibits a nontrivial dependence on the magnitude of the directional driving force, such that the lowest growth exponent is observed for intermediate driving forces. We elaborate that this can originate from the fact that the forces at grain boundary junctions evolve out of balance under the influence of the directional driving force. With increasing the driving forces, the growth exponent asymptotically approaches a value of n~0.63, imposed by the largest possible grain aspect ratio for given grain boundary energies. The current combined mean-field and phase-field framework pave the way for future exploration in broader contexts such as the evolution of complex additively manufactured microstructures.
Reliable measurement of the size of polydisperse, complex-shaped commercial nanopowders is a difficult but necessary task, e.g., for regulatory requirements and toxicity risk assessment. Suitable methods exist for the accurate characterization of the size of non-aggregated, stabilized, spherical and monodisperse nanoparticles. In contrast, industrial nanoscale powders usually require dedicated sample preparation procedures developed for the analysis method of choice. These nano-powders tend to agglomerate and/or aggregate, a behavior which in combination with an innate broad particle size distribution and irregular shape often significantly alters the achievable accuracy of the measured size parameters. The present study systematically tests two commercially available nanoscale powders using different sample preparation methods for correlative analysis by scanning electron microscopy, dynamic light scattering, Brunauer–Emmet–Teller method and differential mobility analysis. One focus was set on the sample preparation by embedding nanoparticles in carbon-based hot-mounting resin. Literature on this topic is scarce and the accuracy of the data extracted from cross sections of these particles is unclearly stated. In this paper systematic simulations on the deviation of the size parameters of well-defined series of nanoparticles with different shapes from the nominal value were carried out and the contributing factors are discussed.
AbstractHigh-strength aluminum alloys used in aerospace and automotive applications obtain their strength through precipitation hardening. Achieving the desired mechanical properties requires precise control over the nanometer-sized precipitates. However, the microstructure of these alloys changes over time due to aging, leading to a deterioration in strength. Typically, the size, number, and distribution of precipitates for a quantitative assessment of microstructural changes are determined by manual analysis, which is subjective and time-consuming. In our work, we introduce a progressive and automatable approach that enables a more efficient, objective, and reproducible analysis of precipitates. The method involves several sequential steps using an image repository containing dark-field transmission electron microscopy (DF-TEM) images depicting various aging states of an aluminum alloy. During the process, precipitation contours are generated and quantitatively evaluated, and the results are comprehensibly transferred into semantic data structures. The use and deployment of Jupyter Notebooks, along with the beneficial implementation of Semantic Web technologies, significantly enhances the reproducibility and comparability of the findings. This work serves as an exemplar of FAIR image and research data management.
A density-based phase field model is developed where the free energy functional is explicitly linked with molecular dynamics and is referred to as the Molecular Phase Field Method (MoPF). MoPF simulations involve expressing interatomic potentials in terms of density to form a density based free energy functional. Inputs to this functional are taken from atomistics such that the phase field density profile matches the corresponding density profile from atomistic simulations. We analyze our results by comparing the MoPF calculated excess interfacial energies with excess interfacial energies calculated using molecular dynamics associated with several nickel grain boundaries. Additionally, a comparison is made between our results and the interfacial energies of a \Sigma7 boundary across a variety of FCC systems simulated using density functional theory. The MoPF method is able to successfully predict grain boundary free energy trends between grain boundary and material types offering an atomistically informed mesoscale formulation for studying grain boundary physics.
Knowledge representation in the Materials Science and Engineering (MSE) domain is a vast and multi-faceted challenge: Overlap, ambiguity, and inconsistency in terminology are common. Invariant (consistent) and variant (context-specific) knowledge are difficult to align cross-domain. Generic top-level semantic terminology often is too abstract, while MSE domain terminology often is too specific. In this paper, an approach how to maintain a comprehensive MSE-centric terminology composing a mid-level ontology–the Platform MaterialDigital Core Ontology (PMDco)–via MSE community-based curation procedures is presented. The illustrated findings show how the PMDco bridges semantic gaps between high-level, MSE-specific, and other science domain semantics. Additionally, it demonstrates how the PMDco lowers development and integration thresholds. Moreover, the research highlights how to fuel it with real-world data sources ranging from manually conducted experiments and simulations with continuously automated industrial applications.
This study investigates the sintering and crystallization behavior and kinetic of the bioactive glass (BG) 13–93 with nominal composition (in mol%): 54.6 SiO2 - 1.7 P2O3 - 22.1 CaO - 6.0 Na2O - 7.9 K2O - 7.7 MgO. Sintering and crystallization were investigated non-isothermally for various particle size fractions smaller than 315 μm as well as for bulk samples. Densification was not hindered by the presence of crystalline phases across all particle size fractions. Afterwards, wollastonite was found as the dominant crystal phase at higher temperature which resorb primary surface precipitation-like quartz crystallites. The growth direction shifts into volume when the sample surface is nearly covered. The crystal growth rate of wollastonite was calculated from the crystalline surface layer thickness measured during heating. The findings of this study are relevant for the high temperature processing of BG 13–93.
The unusual behavior observed in the coefficient of thermal expansion and specific heat capacity of CrFeNi, CoCrNi, and CoCrFeNi medium/high-entropy alloys is commonly referred to as the K-state effect. It is shown to be independent of the Curie temperature, as demonstrated by temperature-dependent magnetic moment measurements. CoCrFeNi alloy is chosen for detailed characterization; potential reasons for the K-state effect such as texture, recrystallization, and second-phase precipitation are ruled out. An examination of the electronic structure indicates the formation of a pseudo-gap in the Density of States, which suggests a specific chemical interaction between Ni and Cr atoms upon alloying. Hybrid Monte Carlo/Molecular Dynamic (MC/MD) simulations indicate the presence of non-negligible chemical short-range order (CSRO). Local lattice distortions are shown to be negligible, although deviations around Cr and Ni elements from those expected in a fully disordered structure are experimentally observed by X-ray absorption spectroscopy. The determined bonding distances are in good agreement with MC/MD calculations. A mechanism is proposed to explain the anomalies and calorimetric experiments and their results are used to validate the mechanism.
Irradiation assisted stress corrosion cracking (IASCC) is a form of intergranular stress corrosion cracking that occurs in irradiated austenitic alloys. It requires an irradiated microstructure along with high temperature water and stress. The process is ubiquitous in that it occurs in a wide range of austenitic alloys and water chemistries, but only when the alloy is irradiated. Despite evidence of this degradation mode that dates back to the 1960s, the mechanism by which it occurs has remained elusive. Here, using high resolution electron backscattering detection to analyze local stress-strain states, high resolution transmission electron microscopy to identify grain boundary phases at crack tips, and decoupling the roles of stress and grain boundary oxidation, we are able to unfold the complexities of the phenomenon to reveal the mechanism by which IASCC occurs. The significance of the findings impacts the mechanical integrity of core components of both current and advanced nuclear reactor designs worldwide.
Extended X-ray absorption fine structure (EXAFS) conducted on an equiatomic MoNbTaW bcc medium-entropy alloy that was annealed at 2273 K reveals unexpectedly small 1st and 2nd shell element-specific lattice distortions. An experimental size-mismatch parameter, δexp, is determined to be ca. 50% lower than the corresponding calculated value. Around W, short-range order (SRO) preferring 4d elements in the 1st and 2nd shells persists. A Nb-W ordering is found, which is reminiscent of ordering emerging at lower temperatures in the B2(Mo,W;Ta,Nb)- and B32(Nb,W)-phases. With high-temperature ordering preferences in fcc also foreshadowing low-temperature phase, these findings suggest a general feature of high-temperature SRO.
The digitalization of materials science and engineering (MSE) is currently leading to remarkable advancements in materials research, design, and optimization, fueled by computer‐driven simulations, artificial intelligence, and machine learning. While these developments promise to accelerate materials innovation, challenges in quality assurance, data interoperability, and data management have to be addressed. In response, the adoption of semantic web technologies has emerged as a powerful solution in MSE. Ontologies provide structured and machine‐actionable knowledge representations that enable data integration, harmonization, and improved research collaboration. This study focuses on the tensile test ontology (TTO), which semantically represents the mechanical tensile test method and is developed within the project Plattform MaterialDigital (PMD) in connection with the PMD Core Ontology. Based on ISO 6892‐1, the test standard‐compliant TTO offers a structured vocabulary for tensile test data, ensuring data interoperability, transparency, and reproducibility. By categorizing measurement data and metadata, it facilitates comprehensive data analysis, interpretation, and systematic search in databases. The path from developing an ontology in accordance with an associated test standard, converting selected tensile test data into the interoperable resource description framework format, up to connecting the ontology and data is presented. Such a semantic connection using a data mapping procedure leads to an enhanced ability of querying. The TTO provides a valuable resource for materials researchers and engineers, promoting data and metadata standardization and sharing. Its usage ensures the generation of finable, accessible, interoperable, and reusable data while maintaining both human and machine actionability.
Along with the desire for developing novel multi-principal element alloys, also known as high-entropy alloys, the concern about their safe application is also increasingly growing. This relates to the alloys’ phase stability, in particular, the control required over unexpected phase decompositions resulting from solute segregation at grain boundaries. Yet, the mechanisms of co-segregation and grain boundary phase decomposition in multi-component alloys are rather challenging to explore. In fact, quantitative investigation of grain boundary behaviors is mostly conducted for binary and a few ternary alloys. In this work, we apply the recently introduced CALPHAD-integrated density-based formalism [RSC Advances 10 (2020) 26728-26741] for considering co-segregation phenomena in alloys with an arbitrary number of components —the term ‘co-segregation’ here refers to co-evolution and any mutual interplay among the solute atoms during their interaction with a grain boundary. Quaternary Fe-Co-Mn-Cr alloy system is studied. We present two major advances beyond previous results: First, a co-segregation-induced multi-component grain boundary spinodal decomposition is quantitatively simulated for the first time. We found that in addition to its low cohesive energy and asymmetrical mixing enthalpy due to magnetic ordering, Mn plays a leading role in triggering interfacial phase decomposition by having a relatively large, concentration-dependent atomic mobility. Second, as an alternative to grain boundary phase diagrams proposed for binary and ternary alloys, we introduce the concept of co-segregation maps for grain boundary segregation screening and design in multi-component alloys. Applying the co-segregation maps, the nonlinear Mn and Cr co-segregation are discussed. Depicted on the alloying composition and phase space, the co-segregation maps enable the required insights to guide a safer, more controlled design of high-entropy alloys.
Creep-fatigue of P92 in service-like tests with combined stress- and strain-controlled dwell times
(2023)
Complex service-like relaxation- and creep-fatigue tests with strain- and stress-controlled dwells and fatigue cycle durations of approx. 2200 s were performed exemplarily on a grade P92 steel at 620 ◦C in this study. The results indicate deviations in the prevailing creep mechanisms of long-term relaxation and creep dwells, affecting subsequent dwells, load shifts, and the macroscopic softening behavior quite differently. In addition, fracture surfaces and longitudinal metallographic sections reveal intergranular crack growth for complex loading with stress-controlled dwells, whereas complex strain-controlled tests enhance oxidation and transgranular crack propagation. These findings substantiate the limited transferability of relaxation-fatigue to creep-fatigue conditions.
The article covers data on the Brinell hardness of the forged precipitation-hardened aluminum alloy EN AW-2618A in the initial T61 condition (i. e. slightly underaged) and after isothermal aging for up to 25,0 0 0 h at aging temperatures between 160 °C and 350 °C. In addition, the hardness was determined on specimens after creep testing at 190 °C and various stresses. The hardness decreases with increasing ag- ing time due to the microstructural evolution of the harden- ing precipitates. The drop occurs faster the higher the aging temperature. Aging under creep load additionally accelerates the hardness decrease.
Melting is well understood in terms of the Lindemann criterion, which
essentially states that crystalline materials melt when the thermal vibrationsof their atoms become so vigorous that they shake themselves free of the binding forces. This picture does not necessarily have to hold for glasses, where the nature of the solid–liquid cross-over is highly debated. The Lindemann criterion implies that the thermal expansion coefficients of crystals are inversely proportional to their melting temperatures. Here we find that, in contrast, the thermal expansion coefficient of glasses decreases more strongly with increasing glass temperature, which marks the liquid–solid cross-over in this material class. However, this proportionality returns when the thermal expansion coefficient is scaled by the fragility, a measure of particle cooperativity. Therefore, for a glass to become liquid, it is not sufficient to simply overcome the interparticle binding energies.
Instead, more energy must be invested to break up the typical cooperative particle network that is common to glassy materials. The thermal expansion coefficient of the liquid phase reveals similar anomalous behaviour and is universally enhanced by a constant factor of approximately 3. These universalities allow the estimation of glass temperatures from thermal expansion and vice versa.
Metallic glasses are known to have a remarkably robust yield strength, admitting Weibull moduli as high as for crystalline engineering alloys. However, their postyielding behavior is strongly varying, with large scatter in both flow stress levels and strains at failure. Using x-ray tomography, we reveal how a strain-dependent internal evolution of shear-band cavities underlies this unpredictable postyielding response.We demonstrate how macroscopic strain softening coincides with the first detection of internal shear-band cavitation. Cavity growth during plastic flow is found to follow a power law, which yields a fractal dimension and a roughness exponent in excellent agreement with self-similar surface properties obtained after fracture. These findings demonstrate how internal microcracking coexists with shear-band plasticity along the plastic part of a stress-strain curve, rationalizing the large variability of plastic flow behavior seen for metallic glasses.
Aero-engine turbine disks are safety-relevant components which are operated under high thermal and mechanical stress conditions. The actual part qualification and certification procedures make use of spin-tests conducted on production-similar disks. While these tests provide, on the one hand, a reliable definition of the critical conditions for real components, on the other hand they represent a relevant cost item for engine manufacturers. The aim of this work is to present two alternative burst speed assessment methods under development based on the Failure Assessment Diagram (FAD) and a global stability criterion, respectively. In the scope of the fracture mechanics assessment, the failure modes hoop-burst and rim-peeling are investigated with semicircular surface cracks modelled at the critical regions on the turbine disk. The comparison of the predicted critical rotational speed shows good agreement between the assessment methods.
Crack propagation under low cycle fatigue and thermomechanical fatigue is characterized by high plastic and creep strains that extend over large regions around the crack, so that concepts of linear-elastic fracture mechanics cannot be applied. In these cases, the cyclic crack tip opening displacement 𝛥CTOD is a promising loading parameter to quantify crack growth. In this work, suitable definitions and Finite Element techniques are investigated and compared for an accurate calculation of 𝛥CTOD under cyclic mechanical and/or thermal loading. A viscoplastic temperature dependent material model of Chaboche-type is used along with large strain settings, specified for the austenitic cast iron Ni-resist. Extensive two-dimensional analyses of Single Edge Notch Tension specimens revealed that collapsed special crack tip elements are superior compared with commonly used regular quadrilateral 8-node elements. At the same level of accuracy of 𝛥CTOD, they require an about ten times coarser mesh and show less sensitivity
w.r.t. element size for both stationary and propagating cracks. In order to simulate fatigue crack growth, an efficient, fully automated FE-technique is developed for an incremental crack propagation by successive remeshing, whereby the deformations and internal state variables are mapped from the old mesh onto the new one. Recommendations are made regarding important numerical control parameters like optimal size of crack tip elements, length of crack growth increment in relation to plastic zone size and 𝛥CTOD value.
Prolonging structural integrity—Fatigue of scarf repairs for wind turbine blade shell applications
(2023)
The influence of scarf repair variables on the mechanical properties of glass fiber reinforced polymer sandwich structures is examined for the application of wind turbine blade shell repairs. Reference shell specimens are tested under fully-reversed cyclic loading to understand the fatigue behavior of the sub-component structure within a range of in-service loads, to which shell specimens with a scarf joint repair are compared. A fatiguesuperior repair material is shown to improve the fatigue behavior of the repaired structures compared to the reference specimens. In separating layup and geometry, damage development is examined on the subcomponent scale for a structural understanding of a scarf repair using in-situ digital image correlation-based strain field measurements as well as passive thermography. Within scarf repair variables, the geometry is shown to play a larger role than layup in the fatigue performance of the repaired structure.
Obtaining dense fine ceramics by the binder jetting additive manufacturing process is challenging. A slurry-based binder jetting process, such as the layerwise slurry deposition (LSD-print) process, can enable the printing of dense ceramic parts. This work describes a procedure to develop and qualify a suitable ink to manufacture silicon carbide green parts by LSD-print. Not only the printability but also the compatibility of the ink with the powder bed and the effect of the binding agent on the properties of the green parts are considered. Both aspects are important to obtain high green strength, which is necessary for printing large or thin-walled parts. Characterization methods, such as rheological and surface tension measurements, are applied to optimize three selected inks. The interplay between ink and powder bed is tested by contact angle measurements and by comparing the biaxial strength of cast and additively manufactured specimens.
Out of the three binding agents tested, a polyethyleneimine and a phenolic resin have a high potential for their use in the LSD-print of silicon carbide green bodies, whereas a polyacrylate binding agent did not show the required properties.
AbstractViscous healing of cracks induced by the Vickers indentation in a soda lime magnesium silicate, a soda borosilicate, and a soda aluminosilicate glass (NAS) was studied by laser scanning microscopy. Plots of the crack length, width, and depth normalized to the initial crack length versus time over viscosity merge into single master curves of each of these quantities for each glass. Despite glass properties do not differ strikingly from each other, however, these master curves strongly differ among the glasses. This finding was attributed to a different interplay of various crack healing phenomena. Lateral cracks were found to be responsible for the bulging of the sample surface around the Vickers imprint, which in turn promotes radial crack widening as the main cause of healing delay. The most rapid healing of lateral cracks was observed in NAS in which bulging and crack widening were least pronounced.
Silicate glass fracture surface energy calculated from crystal structure and bond-energy data
(2023)
We present a novel method to predict the fracture surface energy, γ, of isochemically crystallizing silicate glasses using readily available crystallographic structure data of their crystalline counterpart and tabled diatomic chemical bond energies, D0. The method assumes that γ equals the fracture surface energy of the most likely cleavage plane of the crystal. Calculated values were in excellent agreement with those calculated from glass density, network connectivity and D0 data in earlier work. This finding demonstrates a remarkable equivalence between crystal cleavage planes and glass fracture surfaces.
Controlled oriented crystallization of glass surfaces is desired for high precision applications, since the uppermost crystal layer significantly influences the properties of the material. In contrast to previous studies, the data presented here deal with separated crystals growing at defect-free surfaces in four atmospheres with different degrees of humidity (ambient/dry air, argon and vacuum). A glass with the composition 2 BaO–TiO2–2.75 SiO2 was heat-treated at 825 °C until fresnoite (Ba2TiSi2O8) grew to a significant size. The crystal growth rate is found to increase with increasing humidity. The morphology of the crystals changes from highly distorted dendrites in the driest atmosphere (vacuum) to circular/spear-head-shaped crystals in the wettest atmosphere (ambient air), which we attribute to a decrease in viscosity of the glass surface due to water uptake. The least distorted crystals appear in the form of depressions of up to 6 µm. This has an influence on the observed crystal orientation, as measured by electron backscatter diffraction (EBSD). The pulled-in crystals change the orientation during growth relative to the flat glass surface due to an enrichment in SiO2 at the crystal fronts. This confirms that the orientation of crystals is not fixed following nucleation.
Advanced experimental and numerical approaches are being developed to
capture the localization of plasticity at the nanometer scale as a function of the multiscale and heterogeneous microstructure present in metallic materials.
These innovative approaches promise new avenues to understand microstructural effects on mechanical properties, accelerate alloy design, and enable more accurate mechanical property prediction. This article provides an overview of emerging approaches with a focus on the localization of plasticity by crystallographic slip. New insights into the mechanisms and mechanics of strain localization are addressed. The consequences of the localization of plasticity by deformation slip for mechanical properties of metallic materials are also detailed.
This article refers to the research article entitled “Creep-Fatigue of P92 in Service-Like Tests with Combined Stress- and Strain-Controlled Dwell Times” [1]. It presents experimental mechanical data from complex service-like creep-fatigue experiments performed isothermally at 620 °C and a low strain amplitude of 0.2 % on tempered martensite-ferritic grade P92 steel. The data sets in text file format provide cyclic deformation (min. and max. stresses) and the total (hysteresis) data of all recorded fatigue cycles for three different creep-fatigue experiments: 1) a standard relaxation fatigue (RF) test with symmetrical dwell times of three minutes introduced at minimum and maximum strain, 2) a fully strain-controlled service-like relaxation (SLR) test combining these three-minute peak strain dwells with a 30-minute dwell in between at zero strain, and 3) a partly stress-controlled service-like creep (SLC) test combining the three-minute peak strain dwells with 30-minute dwells at constant stress. Such service-like (SL) tests with additional long-term stress- and strain-controlled dwell times are non-standard, rare, and expensive, making these data very valuable. They may be used to approximate cyclic softening in the technically relevant range, for the design of complex SL experiments, or for detailed analyses of stress-strain hystereses (e.g., for stress or strain partitioning methods, for the determination of hysteresis energies (work), inelastic strain components, etc.). In addition, the latter analyses may supply important input for advanced parametric lifetime modeling of components under creep-fatigue loading or model calibration parameters.
The crystallization proceeds by the advance of the crystal faces into the disordered phase at the expense of the material excess, the supersaturation. Using a conservation constraint for the transformation ratio α∈[0,1] as complementing the rescaled supersaturation to 1 and a kinetic law for the normal growth velocity as function of the supersaturation raised to power g, the growth order, we derive an equation for the rate of transformation dα/dt. We integrate it for the six combinations of the three spatial dimensions D = 1, 2, 3 and the two canonical values of g = 1, 2 towards obtaining expressions for αDg. The same equation, with g = 1 and D = n (n is the so called Avrami exponent) is obtained when taking only the linear in α term from the Taylor’s expansion around α = 0 of the model equation of Johnson-Mehl-Avrami-Kolmogorov (JMAK). We verify our model by fitting datasets of α21 and α31 (from α = 0 to αupper = 0.999) with JMAK to obtain from the fit n = 1.725, 2.43, resp. We show
further how the values of n depend on the value of αupper to which the fit is performed starting always from 0. Towards building a validation protocol, we start with validating α21 with published results.
The fundamental processes of nucleation and crystallization are widely observed in systems relevant to material synthesis and biomineralization; yet most often, their mechanism remains unclear. In this study, we unravel the discrete stages of nucleation and crystallization of Fe3(PO4)2·8H2O (vivianite). We experimentally monitored the formation and transformation from ions to solid products by employing correlated, time-resolved in situ and ex situ approaches. We show that vivianite crystallization occurs in distinct stages via a transient amorphous precursor phase. The metastable amorphous ferrous phosphate (AFEP) intermediate could be isolated and stabilized. We resolved the differences in bonding environments, structure, and symmetric changes of the Fe site during the transformation of AFEP to crystalline vivianite through synchrotron X-ray absorption spectroscopy at the Fe K-edge. This intermediate AFEP phase has a lower water content and less distorted local symmetry, compared to the crystalline end product vivianite. Our combined results indicate that a nonclassical, hydration-induced nucleation and transformation driven by the incorporation and rearrangement of water molecules and ions (Fe2+ and PO4 3−) within the AFEP is the dominating mechanism of vivianite formation at moderately high to low vivianite supersaturations (saturation index ≤ 10.19). We offer fundamental insights into the aqueous, amorphous-to-crystalline transformations in the Fe2+−PO4 system and highlight the different attributes of the AFEP, compared to its crystalline counterpart.
Laser melting manufacturing of large elements of lunar regolith simulant for paving on the Moon
(2023)
The next steps for the expansion of the human presence in the solar system will be taken on the Moon. However, due to the low lunar gravity, the suspended dust generated when lunar rovers move across the lunar soil is a significant risk for lunar missions as it can affect the systems of the exploration vehicles. One solution to mitigate this problem is the construction of roads and landing pads on the Moon. In addition, to increase the sustainability of future lunar missions, in-situ resource utilization (ISRU) techniques must be developed. In this paper, the use of concentrated light for paving on the Moon by melting the lunar regolith is investigated. As a substitute of the concentrated sunlight, a high-power CO2 laser is used in the experiments. With this set-up, a maximum laser spot diameter of 100 mm can be achieved, which translates in high thicknesses of the consolidated layers. Furthermore, the lunar regolith simulant EAC-1A is used as a substitute of the actual lunar soil. At the end of the study, large samples (approximately 250 × 250 mm) with interlocking capabilities were fabricated by melting the lunar simulant with the laser directly on the powder bed. Large areas of lunar soil can be covered with these samples and serve as roads and landing pads, decreasing the propagation of lunar dust. These manufactured samples were analysed regarding their ineralogical composition, internal structure and mechanical properties.
Magnetic shape memory alloys have been examined intensively due to their multifunctionality and multitude of physical phenomena. For both areas, epitaxial films are promising since the absence of grain boundaries is beneficial for applications in microsystems and they also allow to understand the influence of a reduced dimension on the physical effects. Despite many efforts on epitaxial films, two particular aspects remain open.
First, it is not clear how to keep epitaxial growth up to high film thickness, which is required for most microsystems.
Second, it is unknown how the microstructure of premartensite, a precursor state during the martensitic transformation, manifests in films and differs from that in bulk.
Here, we focus on micrometer-thick austenitic Ni-Mn-Ga films and explain two distinct microstructural features by combining high-resolution electron microscopy and X-ray diffraction methods. First, we identify pyramid-shaped defects, which originate from {1 1 1} growth twinning and cause the breakdown of epitaxial growth. We show that a sufficiently thick Cr buffer layer prevents this breakdown and allows epitaxial growth up to a thickness of at least 4 μm. Second, premartensite exhibits a hierarchical microstructure in epitaxial films. The reduced dimension of films results in variant selection and regions with distinct premartensite variants, unlike its microstructure in bulk.
The application and benefits of Semantic Web Technologies (SWT) for managing, sharing, and (re-)using of research data are demonstrated in implementations in the field of Materials Science and Engineering (MSE). However, a compilation and classification are needed to fully recognize the scattered published works with its unique added values. Here, the primary use of SWT at the interface with MSE is identified using specifically created categories. This overview highlights promising opportunities for the application of SWT to MSE, such as enhancing the quality of experimental processes, enriching data with contextual information in knowledge graphs, or using ontologies to perform specific queries on semantically structured data. While interdisciplinary work between the two fields is still in its early stages, a great need is identified to facilitate access for nonexperts and develop and provide user-friendly tools and workflows. The full potential of SWT can best be achieved in the long term by the broad acceptance and active participation of the MSE community. In perspective, these technological solutions will advance the field of MSE by making data FAIR. Data-driven approaches will benefit from these data structures and their connections to catalyze knowledge generation in MSE.
Liquid-metal embrittlement (LME) of galvanized (Zn-coated) advanced high-strength steels is a long-known problem in materials science. Here we reveal the initial microstructural processes underneath the Zn-coating that lead to LME-microcrack initiation in the steel substrate. We track the microstructural evolution during the first tens of milliseconds and find pronounced signatures of Fe-Zn intermetallic precipitation in both ferrite grain boundaries and at internal ferrite-oxide phase boundaries. In concert with novel CALPHAD-integrated density-based thermodynamic modelling, we demonstrate that Zn-rich intermetallic phase-nucleation can occur at markedly low processing temperatures due to a segregation transition. We show that a small Znenrichment caused by Zn bulk-diffusion during the initial temperature rise in a joining process is sufficient to induce the segregation transition and subsequent nucleation of Fe-Zn intermetallic grain-boundary phases, which the experiments link to crack initiation sites. These findings direct focus onto LME-controlling microstructural and thermodynamic phenomena at temperatures below the ductility trough and the austenite formation temperature.
Stereolithography processes such as lithography-based ceramic manufacturing (LCM) are technologies that can produce centimeter-sized structures in a reasonable time frame. However, for some parts specifications, they lack resolution. Two-photon-polymerization (2PP) ensures the highest geometric accuracy in additive manufacturing so far. Nevertheless, building up parts in sizes as large as a few millimeters or even centimeters is a time-consuming process, which makes the production of 2PP printed parts very costly. Regarding feedstock specification, the requirements for 2PP are different to those for LCM, and generally, feedstocks are designed to meet requirements for only one of these manufacturing technologies. In an attempt to fabricate highly precise ceramic components of a rather large size, it is necessary to develop a feedstock that suits both light-based technologies, taking advantage of LCM’s higher productivity and 2PP’s accuracy. Hybridization should bring the desired precision to the region of interest on reasonably large parts without escalating printing time and costs. In this study, specimens gained from a transparent feedstock with yttria stabilized zirconia (YSZ) particles of 5 nm at 70 wt% were presented. The resin was originally designed to suit 2PP, while being also printable with LCM. This work demonstrates how hybrid parts can be sintered into full YSZ ceramics.
Recently, efforts towards the development of patient-specific 3D printed scaffolds for bone tissue engineering from bioactive ceramics have continuously intensified. For reconstruction of segmental defects after subtotal mandibulectomy a suitable tissue engineered bioceramic bone graft needs to be endowed with homogenously distributed osteoblasts in order to mimic the advantageous features of vascularized autologous fibula grafts, which represent the standard of care, contain osteogenic cells and are transplanted with the respective blood vessel. Consequently, inducing vascularization early on is pivotal for bone tissue engineering. The current study explored an advanced bone tissue engineering approach combining an advanced 3D printing technique for bioactive resorbable ceramic scaffolds with a perfusion cell culture technique for pre-colonization with mesenchymal stem cells, and with an intrinsic angiogenesis technique for regenerating critical size, segmental discontinuity defects in vivo applying a rat model. To this end, the effect of differing Si-CAOP (silica containing calcium alkali orthophosphate) scaffold microarchitecture arising from 3D powder bed printing (RP) or the Schwarzwalder Somers (SSM) replica fabrication technique on vascularization and bone regeneration was analyzed in vivo. In 80 rats 6-mm segmental discontinuity defects were created in the left femur.
Ni-Mn-Ga shape-memory alloys are promising candidates for large strain actuation and magnetocaloric cooling devices. In view of potential small-scale applications, we probe here nanomechanically the stress-induced austenite–martensite transition in single crystalline austenitic thin films as a function of temperature. In 0.5 μm thin films, a marked incipient phase transformation to martensite is observed during nanoindentation, leaving behind pockets of residual martensite after unloading. These nanomechanical instabilities occur irrespective of deformation rate and temperature, are Weibull distributed, and reveal large spatial variations in transformation stress. In contrast, at a larger film thickness of 2 μm fully reversible transformations occur, and mechanical loading remains entirely smooth. Ab-initio simulations demonstrate how an in-plane constraint can considerably increase the martensitic transformation stress, explaining the thickness-dependent nanomechanical behavior. These findings for a shape-memory Heusler alloy give insights into how reduced dimensions and constraints can lead to unexpectedly large transformation stresses that need to be considered in small-scale actuation design.
Epoxy R-Glass Fiber-Reinforced Polymer (GFRP) composite plates were hydrothermally aged at 60 ◦C for 23, 75, and 133 days. The water content reached 0.97 wt%, 1.45 wt% and 1.63 wt%, respectively. The studied GFRP matrix was inert to hydrolysis or chain scission, allowing for investigation of irreversible changes in the fiber-matrix interphase due to hydrothermal aging upon re-drying. During each period, a subset of the specimens was removed from the water bath and dried in a chamber. The weight loss upon drying was explained with epoxy leaching (impurities), sizing-rich interphase hydrolysis, glass fiber surface hydrolysis, accumulated degradation products escaping, and water changing state from bound to free. The influence of hydrothermal aging on the fiber-matrix interfacial properties was investigated. Lower interfacial strength of hydrothermally aged (wet)
samples was attributed to plasticization of the epoxy, plasticization and degradation of the sizing-rich interphase (including formation of hydrolytic flaws), and hydrolytic degradation of the glass fiber surface. The kinetics of epoxy-compatible epoxysilane W2020 sizing-rich interphase hydrolysis provided an estimate of ca. 1.49%, 4.80%, and 8.49% of the total composite interphase degraded after 23, 75, and 133 days, respectively. At these conditions, the interface lost 39%, 48%, and 51% of its strength. Upon re-drying the specimens, a significant part of the interfacial strength was regained. Furthermore, an upward trend was observed, being 13%, 10% and 3% strength, respectively; thus, indicating a possibility of partial recovery of properties.
Manufacturing and deformation behavior of alumina and zirconia helical springs at room temperature
(2023)
Ceramic helical springs with identical dimensions were produced by hard machining from alumina, alumina toughened zirconia (ATZ), and tetragonal zirconia polycrystals (TZP) stabilized with different oxides. According to the results of the spring constant determination under deformation rates of 3 mm/min, the deformation behavior of all ceramic springs obeys to Hook’s law. However, variation of the deformation rate, tests under constant load, and spring recovery behavior revealed differences in the deformation behavior of alumina, TZP, and ATZ springs. Alumina springs exhibited time-independent deformation in all tests. In contrast, anelastic deformation at room temperature was demonstrated in all springs containing TZP. This deformation is completely reversible over a period of several days. Anelastic behavior is particularly pronounced in Y-TZP springs, whereas Ce-TZP springs exhibit comparatively very low but still reliably detectable anelasticity. Oxygen vacancies in the TZP ceramic are considered the most likely explanation for the anelastic behavior of TZP springs at room temperature.
The microstructure of an apatite-wollastonite (code name AP40) glass-ceramic is analyzed in this study by combining 2D microscopy, phase analysis, X-ray absorption and synchrotron X-ray refraction computed tomography (XCT and SXRCT, respectively). It is shown that this combination provides a useful toolbox to characterize the global microstructure in a wide scale range, from sub-micrometer to millimeter. The material displays a complex microstructure comprising a glassy matrix with embedded fluorapatite and wollastonite small crystals. In this matrix, large (up to 200 μm) spike-shaped structures are distributed. Such microstructural features are oriented around a central sphere, thereby forming a structure resembling a sea urchin. A unique feature of SXRCT, in contrast to XCT, is that internal interfaces are visualized; this allows one to show the 3D distribution of these urchins with exceptionally good contrast. Furthermore, it is revealed that the spike-shaped structures are not single crystals, but rather composed of sub-micrometric crystals, which are identified as fluorapatite and diopside phases by SEM-EDX analysis.
Metallic glasses (MGs) are known to be structurally heterogeneous at the nanometer (nm) scale. In addition, elastic property mapping has indicated the presence of at least an order-of-magnitude larger length scales, of which the origin continues to remain unknown. Here we demonstrate the existence of an elastic decorrelation length of the order of 100 nm in a Zr-based bulk MG using spatially resolved elastic property mapping via nanoindentation. Since compositional modulations sufficiently large to account for this elastic microstructure were not resolved by analytical scanning-transmission electron microscopy, chemical phase separation such as spinodal decomposition cannot explain their occurrence as previously suggested. Instead, we argue that the revealed long-range elastic modulations stem from structural variations affecting the local density. These emerge during solidification and are strongly influenced by the cooling constraints imposed on bulk MGs during the casting process.
The embrittlement of metallic alloys by liquid metals leads to catastrophic material failure and severely impacts their structural integrity. The weakening of grain boundaries by the ingress of liquid metal and preceding segregation in the solid are thought to promote early fracture. However, the potential of balancing between the segregation of cohesion-enhancing interstitial solutes and embrittling elements inducing grain boundary decohesion is not understood. Here, we unveil the mechanisms of how boron segregation mitigates the detrimental effects of the prime embrittler, zinc, in a Σ5 [0 0 1] tilt grain boundary in α −Fe (4 at.% Al). Zinc forms nanoscale segregation patterns inducing structurally and compositionally complex grain boundary states. Ab-initio simulations reveal that boron hinders zinc segregation and compensates for the zinc induced loss in grain boundary cohesion. Our work sheds new light on how interstitial solutes intimately modify grain boundaries, thereby opening pathways to use them as dopants for preventing disastrous material failure.
Thermoelectric generators are very attractive devices for waste heat energy harvesting as they transform a temperature difference into electrical power. However, commercially available generators show poor power density and limited operation temperatures. Research focuses on high‐temperature materials and innovative generator designs. Finding the optimal design for a given material system is challenging. Here, a theoretical framework is provided that allows appropriate generator design selection based on the particular material properties. For high‐temperature thermoelectric oxides, it can be clearly deduced that unileg multilayer generators have the highest potential for effective energy harvesting. Based on these considerations, prototype unileg multilayer generators from the currently best thermoelectric oxide Ca3Co4O9 are manufactured for the first time by industrially established ceramic multilayer technology. These generators exhibit a power density of 2.2 mW/cm² at a temperature difference of 260 K, matching simulated values and confirming the suitability of the technology. Further design improvements increase the power density by a factor of 22 to facilitate practicable power output at temperature differences as low as 7 K. This work demonstrates that reasonable energy harvesting at elevated temperatures is possible with oxide materials and appropriate multilayer design.
Density-based phase-field (DPF) methods have emerged as a technique for simulating grain boundary thermodynamics and kinetics. Compared to the classical phase-field, DPF gives a more physical description of the grain boundary structure and chemistry, bridging CALPHAD databases and atomistic simulations, with broad applications to grain boundary and segregation engineering. Notwithstanding their notable progress, further advancements are still warranted in DPF methods. Chief among these are the requirements to resolve its performance constraints associated with solving fourth-order partial differential equations (PDEs) and to enable the DPF methods for simulating moving grain boundaries. Presented in this work is a means by which the aforementioned problems are addressed by expressing the density field of a DPF simulation in terms of a traditional order parameter field. A generic DPF free energy functional is derived and used to carry out a series of equilibrium and dynamic simulations of grain boundaries in order to generate trends such as grain boundary width vs. gradient energy coefficient, grain boundary velocity vs. applied driving force, and spherical grain radius vs. time. These trends are compared with analytical solutions and the behavior of physical grain boundaries in order to ascertain the validity of the coupled DPF model. All tested quantities were found to agree with established theories of grain boundary behavior. In addition, the resulting simulations allow for DPF simulations to be carried out by existing phase-field solvers.
A round-robin study has been carried out to estimate the impact of the human element in small-angle scattering data analysis. Four corrected datasets were provided to participants ready for analysis. All datasets were measured on samples containing spherical scatterers, with two datasets in dilute dispersions and two from powders. Most of the 46 participants correctly identified the number of populations in the dilute dispersions, with half of the population mean entries within 1.5% and half of the population width entries within 40%. Due to the added complexity of the structure factor, far fewer people submitted answers on the powder datasets. For those that did, half of the entries for the means and widths were within 44 and 86%, respectively. This round-robin experiment highlights several causes for the discrepancies, for which solutions are proposed.
Optimizing the properties of next-generation high-temperature and corrosion-resistant alloys is rooted in balancing structure-property relationships and phase chemistry. Here, we implement a complementary approach based on transmission electron microscopy (TEM) and atom probe tomography (APT) to ascertain aspects of hierarchical phase separation behavior, by understanding the microstructural evolution and the three-dimensional (3D) nanochemistry of a single crystal Fe79.5Si15.5V5.0 (at%) alloy. A maze-like hierarchical microstructure forms, in which a complex network of metastable disordered α plates (A2 phase) emerges within ordered α1 precipitates (D03 phase). The supersaturation in α1 (D03) precipitates with Fe and V drives the formation of α (A2) plates. The morphology of α (A2) plates is discussed concerning crystal structure, lattice misfit, and elastic strain. Phase compositions and a ternary phase diagram aid the thermodynamic assessment of the hierarchical phase separation mechanism via the Gibbs energy of mixing. A perspective on the stabilization of hierarchical microstructures beyond Fe79.5Si15.5V5.0 is elaborated by comparing hierarchical alloys. We find that the ratio of elastic anisotropy (Zener ratio) serves as a predictor of the hierarchical particles’ morphology. We suggest that the strengthening effect of hierarchical microstructures can be harnessed by improving the temporal and thermal stability of hierarchical particles. This can be achieved through phase-targeted alloying aiming at the hierarchical particles phase by considering the constituents partitioning behavior. Beyond Fe79.5Si15.5V5.0, our results demonstrate a potential pathway for improving the properties of high-temperature structural materials.
Future lunar exploration will be based on in-situ resource utilization (ISRU) techniques. The most abundant raw material on the Moon is lunar regolith, which, however, is very scarce on Earth, making the study of simulants a necessity. The objective of this study is to characterize and investigate the sintering behavior of EAC-1A lunar regolith simulant. The characterization of the simulant included the determination of the phase assemblage, characteristic temperatures determination and water content analysis. The results are discussed in the context of sintering experiments of EAC-1A simulant, which showed that the material can be sintered to a relative density close to 90%, but only within a very narrow range of temperatures (20–30 °C). Sintering experiments were performed for sieved and unsieved, as well as for dried and non-dried specimens of EAC-1A. In addition, an analysis of the densification and mechanical properties of the sintered specimens was done. The sintering experiments at different temperatures showed that the finest fraction of sieved simulant can reach a higher maximum sintering temperature, and consequently a higher densification and biaxial strength. The non-dried powder exhibited higher densification and biaxial strength after sintering compared to the dried specimen. This difference was explained with a higher green density of the non-dried powder during pressing, rather than due to an actual influence on the sintering mechanism. Nevertheless, drying the powder prior to sintering is important to avoid the overestimation of the strength of specimens to be fabricated on the Moon.
Refractory chemically complex alloys with bcc-based microstructures show great potential for high-temperature applications but most of them exhibit limited room-temperature ductility, which remains a challenge. One such example is the AlMo0.5NbTa0.5TiZr alloy, mainly consisting of a nano-scaled structure with an ordered B2 matrix and a high-volume fraction of aligned cuboidal and coherently embedded A2 precipitates. This work aims to investigate how the cooling rate after hot isostatic pressing of the AlMo0.5NbTa0.5TiZr alloy affects its microstructure and its resulting hardness and fracture toughness at room temperature. A slow cooling rate of 5 °C/min leads to a coarse microstructure consisting of aligned slabs (mean A2 precipitate ≈ 25 nm) with a nanohardness of about 8 GPa. In contrast, after the fastest cooling rate (30 °C/min), the A2 precipitates become more cubic with an edge length of ≈ 16 nm, resulting in an increase in nanohardness by 10 %. The fracture toughness is roughly independent of the cooling rate and its mean value (≈ 4.2 MPa∙m1/2) resembles that of some B2 intermetallics and other A2/B2 alloys. As the lattice misfit between the A2 and B2 phases is known to play a key role in microstructure formation and evolution, its temperature dependence between 20 and 900 °C was investigated. These findings offer insights into the evolution of the microstructure and room-temperature mechanical properties of the AlMo0.5NbTa0.5TiZr alloy, which could help the development of advanced chemically complex alloys.
Understanding the mechanical behavior of silicon nanowires is essential for the implementation of advanced nanoscale devices. Although bending tests are predominantly used for this purpose, their findings should be properly interpreted through modeling. Various modeling approaches tend to ignore parts of the effective parameter set involved in the rather complex bending response. This oversimplification is the main reason behind the spread of the modulus of elasticity and strength data in the literature. Addressing this challenge, a surface-based nanomechanical model is introduced in this study. The proposed model considers two important factors that have so far remained neglected despite their significance: (i) intrinsic stresses composed of the initial residual stress and surface-induced residual stress and (ii) anisotropic implementation of surface stress and elasticity. The modeling study is consolidated with molecular dynamics-based study of the native oxide surface through reactive force fields and a series of nanoscale characterization work through in situ threepoint bending test and Raman spectroscopy. The treatment of the test data through a series of models with increasing complexity demonstrates a spread of 85 GPa for the modulus of elasticity and points to the origins of ambiguity regarding silicon nanowire properties, which are some of the most commonly employed nanoscale building blocks. A similar conclusion is reached for strength with variations of up to 3 GPa estimated by the aforementioned nanomechanical models. Precise consideration of the nanowire surface state is thus critical to comprehending the mechanical behavior of silicon nanowires accurately. Overall, this study highlights the need for a multiscale theoretical framework to fully understand the size-dependent mechanical behavior of silicon nanowires, with fortifying effects on the design and reliability assessment of future nanoelectromechanical systems.
Die klassische Metallographie basiert auf Abbildungen einzelner Schliffebenen und kann auf räumliche Formen und Anordnungen des Gefüges nur bedingt schließen. Die Idee, aus metallographischen Serienschliffen dreidimensionale Gefügestrukturen zu rekonstruieren, ist daher naheliegend und nicht neu. Allerdings ist der Aufwand, in Handarbeit viele Einzel-Schliffe zu präparieren und zu Bildstapeln zusammenzusetzen, sehr hoch und steht einer häufigen Anwendung entgegen.
Deshalb wird an der BAM ein Roboter-gestütztes 3D-Metallographie-System entwickelt, das an einer Schliffprobe die Schritte Präparation und Bildeinzug vollautomatisch mit vielen Wiederholungen ausführt. Die Präparation umfasst Schleifen, Polieren und optional Ätzen der Schlifffläche, der Bildeinzug autofokussierte lichtmikroskopische Aufnahmen bei mehreren Vergrößerungsstufen. Der erhaltene Bildstapel wird anschließend vorverarbeitet, segmentiert und in ein 3D-Modell umgesetzt, das einer mikrotomographischen Aufnahme ähnelt, allerdings mit besserer lateraler Auflösung bei großem Volumen. Im Gegensatz zu tomographischen Verfahren besteht die Möglichkeit der Kontrastierung durch klassische chemische Ätzung. Die Integration eines REMs ist geplant. Bislang durchgeführte Arbeiten verdeutlichen die Möglichkeiten der Darstellung von Heißgas-Korrosionsschichten, Grauguss-Werkstoffen und Keramik-basierten mikroelektronischen Strukturen (Vias).
A pseudosymmetric description of the crystal lattice derived from a single wideangle Kikuchi pattern can have several causes. The small size (<15%) of the sector covered by an electron backscatter diffraction pattern, the limited precision of the projection centre position and the Kikuchi band definition are crucial. Inherent pseudosymmetries of the crystal lattice and/or structure also pose a challenge in the analysis of Kikuchi patterns. To eliminate experimental errors as much as possible, simulated Kikuchi patterns of 350 phases have been analysed using the software CALM [Nolze et al. (2021). J. Appl. Cryst. 54, 1012–1022] in order to estimate the frequency of and reasons for pseudosymmetric crystal lattice descriptions. Misinterpretations occur in particular when the atomic scattering factors of non-equivalent positions are too similar and reciprocal-lattice points are systematically missing. As an example, a pseudosymmetry prediction depending on the elements involved is discussed for binary AB compounds with B1 and B2 structure types. However, since this is impossible for more complicated phases, this approach cannot be directly applied to compounds of arbitrary composition and structure.
To visualize the varying tetragonal distortions in high carbon martensitic steels by EBSD, two different approaches have been applied on backscattered Kikuchi diffraction (BKD) patterns. A band-edge refinement technique called Refined Accuracy (RA) (Oxford Instruments) is compared with a technique called Pattern Matching (PM), which optimizes the fit to a simulated BKD signal. RA distinguishes between hypothetical phases of different fixed 𝑐∕𝑎, while PM determines a best fitting continuous 𝑐∕𝑎 by projective transformation of a master pattern. Both techniques require stored BKD patterns.
The sensitivity of the 𝑐∕𝑎-determination was tested by investigating the microstructure of a ferritic steel with an expected 𝑐∕𝑎 = 1. The influence of the Kikuchi pattern noise on 𝑐∕𝑎 was compared for a single or 40 averaged frames per measuring point, and turned out to be not significant. The application of RA and PM on the martensitic microstructure delivered qualitatively similar maps of 𝑐∕𝑎. The comparison of RA and PM shows that RA is suitably fast and precise during mapping the martensite 𝑐∕𝑎 ratio in analyses of high carbon martensite, especially for fast initial surveys. As RA leads quantitatively to higher noise in 𝑐∕𝑎, the PM analysis can be used for higher precision results.
Fatigue tests were performed on the forged aluminum alloy EN AW-2618A in the T61 state. Different stress ratios (R = -1, R = 0.1) were selected to study the influence of mean stress on fatigue life. Two overaged states (10 h/230 ◦C, 1000 h/230 ◦C) were also tested to investigate the influence of overaging on fatigue life. Transmission electron microscopy (TEM) was used to characterize the precipitates (S-phase), which are mainly responsible for the strength of the alloy. A fractographic analysis was also performed to determine the failure mode. Overaging reduces the fatigue life compared to the T61 state. The longer the aging time, the lower the fatigue resistance. The reason is the decrease in (yield) strength, which correlates with the radius of the S-phase: the precipitate radius increases by a factor of approximately two for the overaged states compared to the initial state. The analysis of the fracture surfaces showed crack initiation occurs predominantly on the outer surface and is
associated with the primary phases.