5 Werkstofftechnik
Filtern
Dokumenttyp
Sprache
- Englisch (355) (entfernen)
Referierte Publikation
- ja (355) (entfernen)
Schlagworte
- Additive manufacturing (20)
- EBSD (16)
- Additive Manufacturing (14)
- Microstructure (14)
- Corrosion (12)
- Residual stress (12)
- Transmission electron microscopy (12)
- Creep (10)
- Glass (9)
- Crystallization (8)
Organisationseinheit der BAM
- 5 Werkstofftechnik (355) (entfernen)
Paper des Monats
- ja (11)
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.
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.
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.
Since the TEM has the capacity to observe the atomic structure of materials, in-situ TEM synthesis methods are uniquely suited to advance our fundamental understanding of the bottom-up dynamics that drive the formation of nanostructures. E-beam induced fragmentation (potentially identified as a manifestation of Coulomb explosion) and electron stimulated desorption (ESD) are phenomena that have received attention because they trigger chemical and physical reactions that can lead to the production of various nanostructures. Here we report a simple TEM protocol implemented on WO2.9 microparticles supported on thin amorphous carbon substrates. The method produces various nanostructures such as WC nanoparticles, WC supported films and others. Nevertheless, we focus on the gradual graphitization and gasification of the C substrate as it interacts with the material expelled from the WO2.9 microparticles. The progressive gasification transforms the substrate from amorphous C down to hybrid graphitic nanoribbons incorporating W nanoparticles. We think these observations open interesting possibilities for the synthesis of 2D nanomaterials in the TEM.
To accelerate the growth of Industry 4.0 technologies, the digitalization of mechanical testing laboratories as one of the main data-driven units of materials processing industries is introduced in this paper. The digital lab infrastructure consists of highly detailed and standard-compliant materials testing knowledge graphs for a wide range of mechanical testing processes, as well as some tools that enable the efficient ontology development and conversion of heterogeneous materials’ mechanical testing data to the machine-readable data of uniform and standardized structures. As a basis for designing such a digital lab, the mechanical testing ontology (MTO) was developed based on the ISO 23718 and ISO/IEC 21838-2 standards for the semantic representation of the mechanical testing experiments, quantities, artifacts, and report data. The trial digitalization of materials mechanical testing lab was successfully performed by utilizing the developed tools and knowledge graph of processes for converting the various experimental test data of heterogeneous structures, languages, and formats to standardized Resource Description Framework (RDF) data formats. The concepts of data storage and data sharing in data spaces were also introduced and SPARQL queries were utilized to evaluate how the introduced approach can result in the data retrieval and response to the competency questions. The proposed digital materials mechanical testing lab approach allows the industries to access lots of trustworthy and traceable mechanical testing data of other academic and industrial organizations, and subsequently organize various data-driven research for their faster and cheaper product development leading to a higher performance of products in engineering and ecological aspects.
Irradiation assisted stress corrosion cracking (IASCC) is known to be a combination of applied stress, and a corrosive environment in irradiated materials, but an appropriate understanding of how each of these components affects cracking is not yet clear. In this work, we isolate the role of grain boundary (GB) oxidation in IASCC. For this purpose, solution-annealed 304L stainless steel irradiated in reactor to 5.4 or 69 dpa was studied using a miniaturized four-point bend technique. Two modes of bend tests were conducted; straining in simulated pressurized water reactor primary water (PW) at 320 ◦C in an incremental manner, and pre-oxidation in PW at 320 ◦C without application of stress followed by dynamic straining in purified Ar at the same temperature until crack initiation. Exposure of the 5.4 dpa sample for 210 h in high temperature water initiated cracks in Ar at 60% of the yield stress (0.6YS), whereas the companion sample of the same dose exposed for 1010 h cracked in Ar at 0.5YS. The long-term exposure in water led to GB oxidation that ultimately lowered the crack initiation stress. Dynamic straining in water resulted in larger crack lengths and greater crack depths indicating stress accelerated oxidation and cracking. Dislocation pile-ups at dislocation channel-grain boundary sites provide an amplification of the applied stress to a level consistent with the fracture stress of the grain boundary oxide, providing an explanation for IASCC that occurs at applied stresses well below the irradiated yield stress of the alloy. There was no evidence of cracking upon straining of an unoxidized 69 dpa sample in Ar to well above yield, confirming that the irradiated state is not inherently susceptible to intergranular (IG) cracking and that oxidized GBs are responsible for initiation of IG cracking.
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.
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.
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.
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.
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.
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.
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.
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.
This article reports temperature-dependent elastic properties (Young’s modulus, shear modulus) of three alloys measured by the dynamic resonance method. The alloys Ti-6Al-4V, Inconel IN718, and AISI 316 L were each investigated in a variant produced by an additive manufacturing processing route and by a conventional manufacturing processing route. The datasets include information on processing routes and parameters, heat treatments, grain size, specimen dimensions, and weight, as well as Young’s and shear modulus along with their measurement uncertainty. The process routes and methods are described in detail. The datasets were generated in an accredited testing lab, audited as BAM reference data, and are hosted in the open data repository Zenodo. Possible data usages include the verification of the correctness of the test setup via Young’s modulus comparison in low-cycle fatigue (LCF) or thermo-mechanical fatigue (TMF) testing campaigns, the design auf VHCF specimens and the use as input data for simulation purposes.
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.
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.
Although layer-based additive manufacturing methods such as laser powder bed fusion (PBF-LB) offer an immense geometrical freedom in design, they are typically subject to a build-up of internal stress (i.e. thermal stress) during manufacturing. As a consequence, significant residual stress (RS) is retained in the final part as a footprint of these internal stresses. Furthermore, localized melting and solidification inherently induce columnar-type grain growth accompanied by crystallographic texture. Although diffraction-based methods are commonly used to determine the RS distribution in PBF-LB parts, such features pose metrological challenges in their application. In theory, preferred grain orientation invalidates the hypothesis of isotropic material behavior underlying the common methods to determine RS. In this work, more refined methods are employed to determine RS in PBF-LB/M/IN718 prisms, based on crystallographic texture data. In fact, the employment of direction-dependent elastic constants (i.e. stress factors) for the calculation of RS results in insignificant differences from conventional approaches based on the hypothesis of isotropic mechanical properties. It can be concluded that this result is directly linked to the fact that the {311} lattice planes typically used for RS analysis in nickel-based alloys have high multiplicity and less strong texture intensities compared with other lattice planes. It is also found that the length of the laser scan vectors determines the surface RS distribution in prisms prior to their removal from the baseplate. On removal from the baseplate the surface RS considerably relaxes and/or redistributes; a combination of the geometry and the scanning strategy dictates the sub-surface RS distribution.
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.
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.
The damage mechanisms of metallic components produced by process laser powder bed fusion differ significantly from those typically observed in conventionally manufactured variants of the same alloy. This is due to the unique microstructures of additively manufactured materials. Herein, the focus is on the study of the evolution of creep damage in stainless steel 316L specimens produced by laser powder bed fusion. X-ray computed tomography is used to unravel the influence of the process-specific microstructure from the influence of the initial void distribution on creep damage mechanisms. The void distribution of two specimens tested at 600 °C and 650 °C is analyzed before a creep test, after an interruption, and after fracture. The results indicate that the formation of damage is not connected to the initial void distribution. Instead, damage accumulation at grain boundaries resulting from intergranular cracking is observed.
In this work, we employed glow discharge optical emission spectrometry (GD-OES) depth profiling as a fast and semi-quantitative method to investigate the aluminum (Al) current collector degradation in commercial lithium cobalt oxide (LCO) pouch cells with no Al2O3 pretreatment. After battery aging, a heterogeneous deposit was found on the surface of the cathode. Gray hotspot areas within an extensive pale white region were formed. Consistent with energy dispersive X-ray (EDX) analysis of micro-cross sections milled via targeted focused ion beam (FIB), an Al-containing layer of approximately 3 µm can be observed using GD-OES. We attribute one main cause of this layer is the degradation of the Al current collector. The nonuniform growth of this layer was investigated by performing GD-OES depth profiling at different in-plane positions. We found that the gray area has a higher mass concentration of Al, probably in metallic form, whereas the white area was probably covered more homogeneously with Al2O3, resulting from the inhomogeneous distribution of the pitting positions on the current collector. Compared to FIB-EDX, GD-OES enables a faster and more convenient depth profile analysis, which allows the more productive characterization of lithium-ion batteries (LIBs), and consequently benefits the development of preferable battery materials.
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.
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.
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.
A band width determination using the first derivative of the band profile systematically underestimates the true Bragg angle. Corrections are proposed to compensate for the resulting offset Δa/a of the mean lattice parameters derived from as many Kikuchi band widths as possible. For dynamically simulated Kikuchi patterns, Δa/a can reach up to 8% for phases with a high mean atomic number Z, whereas for much more common low-Z materials the offset decreases linearly. A predicted offset Δa/a = f(Z) is therefore proposed, which also includes the unit-cell volume and thus takes into account the packing density of the scatterers in the material. Since Z is not always available for unknown phases, its substitution by Zmax, i.e. the atomic number of the heaviest element in the compound, is still acceptable for an approximate correction. For simulated Kikuchi patterns the offset-corrected lattice parameter deviation is Δa/a < 1.5%. The lattice parameter ratios, and the angles α, β and γ between the basis vectors, are not affected at all.1.5%. The lattice parameter ratios, and the angles , and between the basis vectors, are not affected at all.
The derivation of a crystal structure and its phase-specific parameters from a single wide-angle backscattered Kikuchi diffraction pattern requires reliable extraction of the Bragg angles. By means of the first derivative of the lattice profile, an attempt is made to determine fully automatically and reproducibly the band widths in simulated Kikuchi patterns. Even under such ideal conditions (projection centre, wavelength and lattice plane traces are perfectly known), this leads to a lattice parameter distribution whose mean shows a linear offset that correlates with the mean atomic number Z of the pattern-forming phase. The consideration of as many Kikuchi bands as possible reduces the errors that typically occur if only a single band is analysed. On the other hand, the width of the resulting distribution is such that higher image resolution of diffraction patterns, employing longer wavelengths to produce wider bands or the use of higher interference orders is less advantageous than commonly assumed.
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.
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.
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.
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.
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.
The interest in repair technologies for polymer composites has increased significantly over the last decades, due to the growing use of these materials in structural applications. In this study, poly (ethylene-co-methacrylic acid) (EMAA) was used as self-healing agent to glass fiber/epoxy composite. Materials with EMAA contents of 2 wt% and 5 wt% were manufactured using Resin Transfer Molding (RTM) and the effects of the healing agent on the properties were investigated using tensile tests and Dynamic Mechanical Analysis (DMA). Results show slight variation of properties, which was more pronounced as the content of EMAA increased. In addition, the healing efficiency was investigated through fatigue tests and the addition of higher content of EMAA increased the number of cycles to failure after the healing activation cycle.
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.
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.
This contribution contains the raw data used to compare experimental results with thermodynamic calculations using the CALPHAD method, which is related to the research article “The AlMo0.5NbTa0.5TiZr refractory high entropy superalloy: experimental findings and comparison with calculations using the CALPHAD method” [1] , and therefore this article can be used as a basis for interpreting the data contained therein. The AlMo0.5NbTa0.5TiZr refractory superalloy was characterized in the cast and annealed condition (1400 °C for 24 h) in order to measure grain size and to identify and measure the size and area fraction of the phases present. The raw data of this article include X-ray diffraction (XRD) measurements, microstructural characterization by scanning and transmission electron microscopy (SEM and TEM), and elemental analysis by energy dispersive X-ray spectroscopy (EDX). XRD includes the determination of phases and the lattice parameters (A2, B2, and hexagonal structure). Microstructural analysis by scanning and transmission electron microscopy includes (1) identification of composition, size, and volume fraction of the present phases and (2) determination of grain size. Based on these experimental data, it is possible to identify similarities and discrepancies with the data calculated using the CALPHAD method for the alloy under study in Ref. [1] , which provides the basis for better and more efficient development of reliable databases.
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.
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.
Using the creation relaxation algorithm developed for the atomistic modeling of the high-dose irradiation limit of crystalline systems, we explore the limits of the structural rejuvenation of a highly excited model binary glass. This high-energy athermal amorphous structure exhibits a direct transition to homogeneous plastic flow and a microstructure that is largely insensitive to this flow, being characterized by a porous system-spanning network of minimally frustrated structural motifs. The observed homogeneous plasticity is mediated by the same string-like structural excitations, which mediate structural relaxation and microplasticity at finite temperature in more relaxed structures. This highly rejuvenated structural asymptote is not far from the structural state of regions, which have experienced athermal shear localization in more relaxed samples, suggesting an optimally rejuvenated glassy structure will always be limited by that produced by shear localization.
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.
This paper presents the results of a study of the morphology and structure at the weld interface in a brass–Invar bimetal, which belongs to the class of so-called thermostatic bimetals, or thermobimetals. The structure of the brass–Invar weld interface was analyzed using optical microscopy and scanning electron microscopy (SEM), with the use of energy-dispersive X-ray (EDX) spectrometry and back-scattered electron diffraction (BSE) to identify the phases. The distribution of the crystallographic orientation of the grains at the weld interface was obtained using an e-Flash HR electron back-scatter diffraction (EBSD) detector and a forward-scatter detector (FSD). The results of the study indicated that the weld interface had the wavy structure typical of explosive welding. The wave crests and troughs showed the presence of melted zones consisting of a disordered Cu–Zn–Fe–Ni solid solution and undissolved Invar particles. The pattern quality map showed that the structure of brass and Invar after explosive welding consisted of grains that were strongly elongated towards the area of the highest intensive plastic flow. In addition, numerous deformation twins, dislocation accumulations and shear bands were observed. Thus, based on the results of this study, the mechanism of Cu–Zn–Fe–Ni structure formation can be proposed.
This work investigates the effect of the tribotesting parameters (temperature, atmosphere, and third body chemical composition) on the coefficient of friction (CoF) during pin-on-disc dry (PoD) sliding tribotests using artificial third bodies. The third body comprised nanometric Fe3O4-based binary to quaternary chemical compositions containing copper, graphite, and zirconia. These mixtures were manually or ball-milled prepared, and pin-on-disc tribotests were conducted at 23 °C and 400 °C under air or nitrogen atmospheres. Combining PoD and artificial third body to create synthetic tribofilms might be useful for testing new formulations of Cu-free friction materials. Microstructural characterisation of the tribofilms was used to study the stability of the Fe3O4, copper, and graphite nanoparticles under different testing conditions to understand their effects on the CoF. For the Fe3O4-C-ZrO2-X systems, the ball milling mixing promoted the formation of turbostratic graphite in the tribofilm, impairing the lubricating effect of the graphite under air atmosphere at 23 °C. The formation of monoclinic CuO in the tribofilms during tribotests at 400 °C under air and N2 atmospheres promoted a lubricating effect.
Filigree structures can be manufactured via two-photon-polymerization (2PP) operating in the regime of non-linear light absorption. For the first time it is possible to apply this technique to the powder processing of ceramic structures with a feature size in the range of the critical defect size responsible for brittle fracture and, thus, affecting fracture toughness of high-performance ceramics. In this way, tailoring of advanced properties can be achieved already in the shaping process. Traditionally, 2PP relies on transparent polymerizable resins, which is diametrically opposed to the usually completely opaque ceramic resins and slurries. Here we present a transparent and photocurable suspension of nanoparticles (resin) with very high mass fractions of yttria-stabilized zirconia particles (YSZ). Due to the extremely well dispersed nanoparticles, scattering of light can be effectively suppressed at the process-relevant wavelength of 800 nm. Sintered ceramic structures with a resolution of down to 500 nm were obtained. Even at reduced densities of 1 to 4 g/cm³, the resulting compressive strength with 4,5 GPa is equivalent or even exceeding bulk monolithic yttria stabilized zirconia. A ceramic metamaterial is born, where the mechanical properties of yttria stabilized zirconia are altered by changing geometrical parameters and gives access to a new class of ceramic materials.
The need for new solutions for electrical insulation is growing due to the increased electrification in numerous industrial sectors, opening the door for innovation. Plasma spraying is a fast and efficient way to deposit various ceramics as electrical insulators, which are used in conditions where polymers are not suitable. Alumina (Al2O3) is among the most employed ceramics in the coating industry since it exhibits good dielectric properties, high hardness, and high melting point, while still being cost-effective. Various parameters (e.g., feedstock type, spray distance, plasma power) significantly influence the resulting coating in terms of microstructure, porosity, and metastable phase formation. Consequently, these parameters need to be investigated to estimate the impact on the dielectric properties of plasma-sprayed alumina coatings. In this work, alumina coatings with different spray distances have been prepared via atmospheric plasma spray (APS) on copper substrates. The microstructure, porosity, and corresponding phase formation have been analyzed with optical microscopy, X-ray diffraction (XRD), and scanning electron microscopy (SEM). Moreover, we present an in-depth analysis of the fundamental dielectric properties e.g., direct current (DC) resistance, breakdown strength, dielectric loss tangent, and permittivity. Our results show that decreasing spray distance reduces the resistivity from 6.31 × 109 Ωm (130 mm) to 6.33 × 108 Ωm (70 mm), while at the same time enhances the formation of the metastable δ-Al2O3 phase. Furthermore, space charge polarization is determined as the main polarization mechanism at low frequencies.
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 morphology of pores partially shrunk during a half-hour HIP at temperature of 1288 °C and pressure of 103 MPa has been investigated in nickel-based superalloy CMSX-4. The investigation resulted in the following findings: surrounding the shrinking pores by a c¢-shell (Ni3Al), faceting of the pores surface by {023} and {011} planes, and formation the submicroscopic satellite pores connected by channels with the neighboring larger pores. It is assumed that the formation of the c¢-shell around the pores and the faceting of the pore surface is due to diffusion processes occurring during pore shrinkage, and therefore these findings can be considered as arguments supporting the vacancy model of pore annihilation. The submicroscopic satellite pores are expected to be the result of dividing the casting pores of a complex initial shape during their shrinking. The connecting channels are probably required for the gas to escape from the rapidly shrinking small satellite pores into the slowly shrinking large pore. Thus, it is reasonable to assume that the casting pores may contain some amount of gas.
Among the strategies to produce healable thermosetting systems is their modification by the addition of thermoplastic particles. This work investigates the influence of poly(ethylene-co-methacrylic acid) (EMAA) on fibermatrix interfacial properties of a glass fiber reinforced epoxy matrix composite. Epoxy-EMAA interactions were evaluated using differential scanning calorimetry (DSC) and infrared spectroscopy. The effects of EMAA on the epoxy network formation were evidenced by changes in glass transition temperature, cure kinetics and alteration of chemical groups during cure. Interfacial shear strength (IFSS) measurements obtained by single fiber pull-out tests indicate similar interfacial properties for pure and EMAA modified epoxy. Additionally, the potential for self-healing ability of an EMAA modified epoxy was demonstrated. However, IFSS after a healing cycle for the EMAA modified epoxy was lower as compared to the pure epoxy, because of the lower fiber-EMAA interfacial shear strength. So, thermoplastic healing agents has not only to fill cracks in the matrix material, but also have to be optimized regarding its interface properties to the reinforcing fibers.
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.
Grain boundaries (GBs)’s role in determining the functional and mechanical properties of polycrystalline materials is inscribed in both their structure and chemistry. Upon solute segregation, the structure and composition of a GB can change concurrently. We study the co-evolution of GB’s structure and segregation by enhancing the density-based phase-field model to account for the in-plane structural variations in the GB. Significant mutual coupling is revealed between the GB’s chemical and structural states during Mn segregation in Fe-Mn alloys. We found that the structural degrees of freedom in a GB (the ability of the GB structure to respond to the chemical variation) amplifies Mn segregation transition, even when the GB structure stays unchanged. When the GB structure is not uniform, that is the usual case, the coupling between GB structure and segregation evolution also enables the spinodally formed low- and high-Mn phases (upon segregation transition) to co-exist within the GB region. These findings explain the stabilizing mechanism of pronounced interfacial segregation fluctuations, experimentally evidenced in Fe-Mn GBs, and give new insights on the structural sensitivity of GBs’ segregation phenomena and the mutual chemo-structural interplay.
Molten salt containing systems gain in importance for sustainable energy use and production. For research and development, interactions of molten salts with potential container materials are of major interest. This article introduces preparation procedures to display an intact metal and salt microstructure and their interface using light optical microscopy and scanning electron microscopy. The exemplary material combination is the ternary salt mixture NaCl-KCl-MgCl2 and the low alloyed steel 1.4901 (T92) with a maximum service temperature of 550 °C. These are potential elements/materials for use in latent heat thermal energy storages.