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Organisationseinheit der BAM
- 5 Werkstofftechnik (1137)
- 5.1 Mikrostruktur Design und Degradation (338)
- 5.2 Metallische Hochtemperaturwerkstoffe (277)
- 5.4 Multimateriale Fertigungsprozesse (216)
- 5.6 Glas (151)
- 5.3 Polymere Verbundwerkstoffe (131)
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- 9 Komponentensicherheit (98)
- 7 Bauwerkssicherheit (91)
Paper des Monats
- ja (11)
In dieser Präsentation werden die letzten Entwicklungen in der Plattform MaterialDigital (PMD) im DIN Normenausschuss 062-01-42 AA zur Zug- und Duktilitätsprüfung für Metalle vorgestellt. Dabei werden hauptsächlich die Entwicklungen und Neustrukturierung der PMD Core Ontology (PMDco) sowie die entsprechende Anpassung der Zugversuchsontologie (Tensile Test Ontology - TTO) inklusive des Datenmappings adressiert. Für das Datenmapping wurde ein speziell im Zusammenhang mit der PMD erstellter Zugversuchsdatensatz verwendet, welcher frei verfügbar in einem online Zenodo Repository veröffentlicht ist. Weiterhin wird die Weiterentwicklung der Norm in Verbindung mit ihrer folgenden Revision hinsichtlich der Integration von Aspekten zur Digitalisierung in der Materialwissenschaft und Werkstofftechnik sowie der Verwendung von semantischen Technologien, wie unter anderem ontologischen Repräsentationen von Materialien und Prozessen, diskutiert.
This is an interactive workshop of the Plattform MaterialDigital (PMD) on Semantic Web technologies (SWT) where we delve into the world of ontology development and data structuring in the field of materials science and engineering (MSE). This workshop is designed to equip participants with essential skills in categorizing classes within ontologies, with a special emphasis on the PMD Core Ontology (PMDco). Discover the immense value of ontologies for MSE data reproducibility and reuse and harness the power of PMDco to foster your data management practices.
In this workshop, you will explore the intricacies of class categorization when developing ontologies in the MSE domain. Through interactive discussions and hands-on exercises, you will learn effective techniques for structuring and organizing ontologies to enhance data retrieval and analysis. You will gain valuable insights into best practices and considerations for class categorization, aiming at optimal data organization and management within your MSE projects.
One of the highlights of this workshop is the introduction to PMDco, a mid-level ontology in the field of MSE developed community-driven in the frame of the project PMD. Learn about PMDco, its underlying concepts, and its application in detail. Discover how PMDco provides a comprehensive framework for MSE data representation, enabling seamless integration and interoperability across different systems and platforms. In addition to exploring PMDco, this workshop will illustrate the benefits of data interoperability and SWT with respect to leveraging the full potential of MSE data.
LTCCs (Low-temperature co-fired ceramics) consist of three-dimensionally distributed, hermetically bonded ceramic and metallic components with structure sizes within [10; 100] µm. A non-destructive imaging technique is needed that provides 3D, sharp, high-contrast resolution of these structures, as well as porosity and defect analysis, which is made difficult by the very different X-ray absorption coefficients of the individual components of the microstructure. A HDR method is being developed that allows a combination of different tomograms, each with X-ray energies adapted to individual materials.
The high-temperature corrosion behaviors of the equimolar CrCoNi medium- and CrMnFeCoNi high-entropy alloy were studied in a gas atmosphere consisting of a volumetric mixture of 10% H2O, 2% O2, 0.5% SO2, and 87.5% Ar at 800 °C for up to 96 h. Both alloys were initially single-phase fcc structured and showed a mean grain size of ~50 µm and a homogeneous chemical composition. The oxide layer thickness of the Cantor alloy CrMnFeCoNi increased linearly with exposure time while it remained constant at ~1 µm for CrCoNi. A Cr2O3 layer and minor amounts of (Co,Ni)Cr2O4 developed on CrCoNi while three layers were detected on the Cantor alloy. These layers were a thin and continuous chromium rich oxide layer at the oxide/alloy interface, a dense (Mn,Cr)3O4 layer in the center and a thick and porous layer of Mn3O4 and MnSO4 at the gas/oxide interface. Additionally, a few metal sulfides were observed in the CrMnFeCoNi matrix. These results were found to be in reasonable agreement with thermodynamic calculations.
High entropy alloys (HEA) are a new class of materials that have been investigated since the early 2000s and offer great potential to replace conventional alloys. However, since they sometimes have significant contents of expensive alloying elements such as Co or Ni, their use is only conceivable in highly stressed areas of components. For this purpose, the weldability with conventional alloys such as high-alloy austenitic steels must be investigated. In addition to the resulting microstructure, the mechanical properties are also fundamental for the usability of HEAs in DMWs. For this purpose, TIG welds of CoCrFeMnNi HEA (cold rolled and recrystallized state) with AISI 304 austenitic steel are investigated. These mechanical properties are analyzed in this work by means of tensile tests and local hardness measurement. The local strain behavior of the welded joints is also characterized by means of Digital Image Correlation (DIC). The results of the local hardness measurement show a clear influence of the initial condition of the HEA on the HAZ. Thus, the HEA in the cold-rolled condition shows a clear softening because of recrystallization processes in the HAZ. On the other hand, there is no influence on the hardness of the weld metal, which is approx. 200 HV0.1 in both cases. The tensile tests show a consistent failure of the weld in the weld metal. However, regardless of the HEA condition, strengths in the range of the recrystallized HEA (RM ~ 550–600 MPa) are achieved, although with significantly reduced fracture elongations.
Slow crack growth (SCG) under the influence of external fluid media, usually termed environmental stress cracking (ESC), is still one of the most frequent origins of severe damage and failure of polymeric materials. For polyethylene (PE) this is relevant for mass products, like bottles for consumer products, but also for high-performance materials for pipes or industrial packaging, including containers for chemicals and other dangerous goods. Especially for high-density polyethylene (PE-HD) the susceptibility to SGC and ESC is depending on the complex interplay between molecular weight and architecture and the resulting semicrystalline morphology, especially the formation of tie-molecules.
A reliable assessment of the resistance against this damage phenomenon is essential for demanding as well as safety-critical applications and has to take into account suitable testing methodologies and conditions in combination with environmental media reflecting the properties representative for typical fillings and relevant components causing ESC. In this context a better understanding of different influencing factors, such as sorption, swelling or surface activity is necessary together with a detailed characterization of different stages of crack propagation and underlying mechanisms. Therefor well-established testing methods, such as the Full Notch Creep Test (FNCT), were complemented by detailed fracture surface analysis using e.g. LSM and SEM in combination with a time-dependent optical monitoring of the progressing crack growth.
For the crack growth also the ratio of fibrillated craze zone to crack opening is important for the deeper understanding of crack propagation and related material parameters which can be additionally addressed by X-ray computed tomography.
Im Vortrag werden das Messprinzip einer Photozentrifuge erläutert und die Anforderungen der zugrundeliegenden Normen diskutiert. Die praktische Durchführung der Messung und insbesondere auch die vorbereitenden Arbeiten, sowie die Auswertung der Rohdaten bilden den Schwerpunkt des Vortrags. Gezeigt werden auch die Validierung sowie ein Beispiel zur regelmäßigen Verifizierung des Verfahrens. Nach Anwendungsbeispielen und Vergleichen zu Ergebnissen mit anderen Messverfahren, wird das Verfahren in einer Zusammenfassung bewertet.
In Leichtbauanwendungen sind Materialien mit geringen Dichten und hohen Festigkeiten gefragt. Insbesondere Faser-Kunststoff-Verbunde (FKV) erfüllen diese Anforderungen und werden zunehmend für Strukturbauteile eingesetzt. Die Oberflächen moderner Rotorblätter von Windkraftanlagen werden aus FKV gefertigt. Das Versagen dieser Materialien hat massiven Einfluss auf die Einsatzfähigkeit der gesamten Windkraftanlage. Daher ist die Kenntnis des Versagensverhaltens dieser Komponenten unter statischer und zyklischer Belastung von großem Interesse, um die Betriebsbeanspruchung abzuschätzen. Im Idealfall wird die Schadensentwicklung unter Betriebslast mit zerstörungsfreien in-situ-Prüfverfahren ermittelt. Hier berichten wir über die Beobachtung der Rissentwicklung in Carbon-Faserverstärkten Kunststoffen (CFK) unter kontinuierlicher Zugbelastung durch in-situ Synchrotron-Röntgenrefraktionsradiographie. Eine selbst entwickelte elektromechanische Zugprüfmaschine mit einem Kraftbereich bis zu 15 kN wurde in den Strahlengang an der BAMline (BESSY II) integriert. Da in herkömmlichen (Absorptions-) Radiographien Defekte wie Zwischenfaserbrüche oder Faser-Matrix-Enthaftung keinen ausreichenden Kontrast verursachen, wird zur Kontrastanhebung die Röntgenrefraktion benutzt. Hier wird das sogenannte Diffraction Enhanced Imaging (DEI) angewandt, um Primär- und gebrochene Strahlung mit Hilfe eines Analysatorkristalls zu trennen. Diese Technik ermöglicht schnelle Messungen mit einem Gesichtsfeld von einigen Quadratmillimetern (hier: 14 mm × 7.2 mm) und ist ideal für in-situ Untersuchungen. Die Bildgebung und der Zugversuch erfolgen mit einer Bildfrequenz von 0.7 / s und einer Dehnrate von 0.00055 / s . Bei 0°/90° Fasergelegen treten die ersten Zwischenfaserrisse bei 380 MPa (Dehnung 0.8 %) auf. Vor dem Versagen bei ca. 760 MPa (Dehnung 2.0 %) beobachten wir die Ausbildung eines nahezu äquidistanten Rissmusters (Risse in ca. 1 mm Abstand), das sich im geschädigten Zustand über die gesamte Probe erstreckt.
In Leichtbauanwendungen sind Materialien mit geringen Dichten und hohen Festigkeiten gefragt. Insbesondere Faser-Kunststoff-Verbunde (FKV) erfüllen diese Anforderungen und werden zunehmend für Strukturbauteile eingesetzt. Die Oberflächen moderner Rotorblätter von Windkraftanlagen werden aus FKV gefertigt. Das Versagen dieser Materialien hat massiven Einfluss auf die Einsatzfähigkeit der gesamten Windkraftanlage. Daher ist die Kenntnis des Versagensverhaltens dieser Komponenten unter statischer und zyklischer Belastung von großem Interesse, um die Betriebsbeanspruchung abzuschätzen. Im Idealfall wird die Schadensentwicklung unter Betriebslast mit zerstörungsfreien in-situ-Prüfverfahren ermittelt. Hier berichten wir über die Beobachtung der Rissentwicklung in Carbon-Faserverstärkten Kunststoffen (CFK) unter kontinuierlicher Zugbelastung durch in-situ Synchrotron-Röntgenrefraktionsradiographie. Eine selbst entwickelte elektromechanische Zugprüfmaschine mit einem Kraftbereich bis zu 15 kN wurde in den Strahlengang an der BAMline (BESSY II) integriert. Da in herkömmlichen (Absorptions-) Radiographien Defekte wie Zwischenfaserbrüche oder Faser-Matrix-Enthaftung keinen ausreichenden Kontrast verursachen, wird zur Kontrastanhebung die Röntgenrefraktion benutzt. Hier wird das sogenannte Diffraction Enhanced Imaging (DEI) angewandt, um Primär- und gebrochene Strahlung mit Hilfe eines Analysatorkristalls zu trennen. Diese Technik ermöglicht schnelle Messungen mit einem Gesichtsfeld von einigen Quadratmillimetern (hier: 14 mm × 7.2 mm) und ist ideal für in-situ Untersuchungen. Die Bildgebung und der Zugversuch erfolgen mit einer Bildfrequenz von 0.7 / s und einer Dehnrate von 0.00055 / s . Bei 0°/90° Fasergelegen treten die ersten Zwischenfaserrisse bei 380 MPa (Dehnung 0.8 %) auf. Vor dem Versagen bei ca. 760 MPa (Dehnung 2.0 %) beobachten wir die Ausbildung eines nahezu äquidistanten Rissmusters (Risse in ca. 1 mm Abstand), das sich im geschädigten Zustand über die gesamte Probe erstreckt.
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 efforts taken within the project ‘platform MaterialDigital’ (PMD, materialdigital.de) to store FAIR data in accordance with a standard-compliant ontological representation (‘application ontology’) of a tensile test of metals at room temperature (ISO 6892-1:2019-11) will be presented. This includes the path from developing an ontology in accordance with the respective standard, converting ordinary data obtained from standard tests into the interoperable RDF format, up to connecting the ontology and data. The semantic connection of the ontology and data leads to interoperability and an enhanced ability of querying. For further reusability of data and knowledge semantically stored, the PMD core ontology (PMDco) was developed, which is a mid-level ontology in the field of MSE. The semantic connection of the tensile test application ontology to the PMDco is also presented. Moreover, Ontopanel, a tool for domain experts facilitating visual ontology development and mapping for FAIR data sharing in MSE, is introduced briefly.
Towards interoperability: Digital representation of a material specific characterization method
(2023)
Certain metallic materials gain better mechanical properties through controlled heat treatments. In age-hardenable aluminum alloys, the strengthening mechanism is based on the controlled formation of nanometer sized precipitates, which hinder dislocation movement. Analysis of the microstructure and especially the precipitates by transmission electron microscopy allows identification of precipitate types and orientations. Dark-field imaging is often used to image the precipitates and quantify their relevant dimensions.
The present work aims at the digital representation of this material-specific characterization method. Instead of a time-consuming, manual image analysis, a digital approach is demonstrated. The integration of an exemplary digital workflow for quantitative precipitation analysis into a data pipeline concept is presented. Here ontologies enable linking of contextual information to the resulting output data in a triplestore. Publishing digital workflow and ontologies ensures the reproducibility of the data. The semantic structure enables data sharing and reuse for other applications and purposes, demonstrating interoperability.
Der Beitrag behandelt verschiedene Themen aus dem H2Safety@BAM-Kompetenzfeld Sensorik, Analytik und zertifizierte Referenzmaterialien (SensRef) mit Schwerpunkt auf Mess- und Prüfverfahren, die verschiedene Analyseverfahren, Sensortechnologien und Ultraschallwellen nutzen. Ein Teil davon ist das Euramet-Vorhaben "MefHySto" zur Metrologie der Wasserstoffspeicherung. Des Weiteren werden Verfahren zur Erkennung von freigesetztem Wasserstoff und zur Bestimmung des Wasserstoff-Luftverhältnisses mithilfe von Gassensoren behandelt. Ein weiterer Aspekt ist die zerstörungsfreie Fehlstellenerkennung mit einem integrierten Zustandsüberwachungssystem, das auf geführten Ultraschallwellen basiert und zur Überwachung der Lebensdauer von Composite-Behältern (Wasserstoffspeicher) dient. Zudem wird die Anwendung faseroptischer Sensorik zur Schadenfrüherkennung an Wasserstoffspeichern diskutiert. Dabei werden erkennbare Dehnungsänderungen an Druckbehältern als Indikatoren genutzt.
Packaging containers for dangerous goods that include aggressive liquids require that any packaging material that is based on high-density polyethylene has a high degree of stability and durability. This work is focused on testing the environmental stress cracking of the high-density polyethylenes used for such containers in contact with crop protection formulations, in particular, two model liquids established in Germany as standardized test media representatives for crop protection formulations containing the various admixtures typical for such products. One of the liquids is water-based and contains mostly surface-active ingredients, while the other is solvent-based and includes some emulsifiers. Originally established for pin impression tests, these model liquids and their individual components were here used for the first time as environmental media in the Full Notch Creep Test, which addresses the resistance against environmental stress cracking. The Full Notch Creep Test was carried out on five high-density polyethylene types with both model liquids, and also on one selected material with its components. The evaluation was focused on the fracture surface structures, which were visualized by a scanning electron microscope and by optical in situ imaging of the notch opening. While the water-based model liquid and its surface-active individual components induced environmental stress cracking with the characteristic pattern for a craze-crack mechanism and so-called brittle fracture on the surface, the solvent-based model liquid and its soluble ingredients exhibited rather ductile failure behavior, caused by the plasticizing effect on the polymer that reduced the yield stress of the high-density polyethylene.
For both cases, fracture surface analysis, together with side views of the crack opening, showed a clear relation between surface pattern, notch deformation (e.g., by blunting), or crack opening due to crack growth with time to failure and the solubility of the liquids in high-density polyethylene.
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.
This dataset consists of indentation data measured with a conospherical tip in a Hysitron-Bruker TI980 Nanoindenter on the surface of a <100> Silicon wafer and a polished cross-sectional cut of a Zr65Cu25Al10 bulk metallic glass.
It is associated with the following publication:
Birte Riechers, Catherine Ott, Saurabh Mohan Das, Christian H. Liebscher, Konrad Samwer, Peter M. Derlet and Robert Maass "On the elastic microstructure of bulk metallic glasses" Materials and Design xxx, (2023) 111929. https://doi.org/10.1016/j.matdes.2023.111929
All experimental information can be found in this paper and in the accompanying supplementary information.
This electronic version of the data was published on the "Zenodo Data repository" found at http://zenodo.org/deposit in the community "Bundesanstalt fuer Materialforschung und -pruefung (BAM)".
The authors have copyright to these data. You are welcome to use the data for further analysis, but are requested to cite the original publication whenever use is made of the data in publications, presentations, etc.
Any questions regarding the data can be addressed to birte.riechers@bam.de who would also appreciate a note if you find the data useful.
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.
The elastic properties (Young's modulus, shear modulus) of austenitic stainless steel AISI 316L were investigated between room temperature and 900 °C in an additively manufactured variant (laser powder bed fusion, PBF‑LB/M) and from a conventional process route (hot rolled sheet). The moduli were determined using the dynamic resonance method. The data set includes information on processing parameters, heat treatments, grain size, specimen dimensions and weight, Young’s and shear modulus as well as their measurement uncertainty.
The dataset was generated in an accredited testing lab using calibrated measuring equipment. The calibrations meet the requirements of the test procedure and are metrologically traceable. The dataset was audited as BAM reference data.
The elastic properties (Young's modulus, shear modulus) of Ni-based alloy Inconel IN718 were investigated between room temperature and 800 °C in an additively manufactured variant (laser powder bed fusion, PBF‑LB/M) and from a conventional process route (hot rolled bar). The moduli were determined using the dynamic resonance method. The data set includes information on processing parameters, heat treatments, grain size, specimen dimensions and weight, Young’s and shear modulus as well as their measurement uncertainty.
The dataset was generated in an accredited testing lab using calibrated measuring equipment. The calibrations meet the requirements of the test procedure and are metrologically traceable. The dataset was audited as BAM reference data.
The elastic properties (Young's modulus, shear modulus) of titanium alloy Ti-6Al-4V were investigated between room temperature and 400 °C in an additively manufactured variant (laser-based directed energy deposition with powder as feedstock, DED-LB/M) and from a conventional process route (hot rolled bar). The moduli were determined using the dynamic resonance method. The data set includes information on processing parameters, heat treatments, microstructure, grain size, specimen dimensions and weight, Young’s and shear modulus as well as their measurement uncertainty.
The dataset was generated in an accredited testing lab using calibrated measuring equipment. The calibrations meet the requirements of the test procedure and are metrologically traceable. The dataset was audited as BAM reference data.
Oxide thermoelectric semiconducting materials like p-type calcium cobaltite Ca3Co4O9 are investigated as oxidation- and temperature-resistant thermoelectric materials for thermoelectric generators (TEGs). To realize TEGs in planar film technology, the powder aerosol deposition (PAD) method is emerging recently. PAD is a method to obtain dense ceramic films directly from the synthesized starting powders without a subsequent high temperature step.
In the present work, Ca3Co4O9 (CCO) powders are processed by PAD to ceramic films at room temperature. The thermoelectric properties of the films (film thickness 10 – 20 µm) are characterized from room temperature to 900°C. Additionally, the layer morphology and texture of the films will be investigated.
As result, the Seebeck coefficient of the CCO-PAD film is comparable to pressed and sintered CCO-bulk materials during the 1st heating cycle to 900°C. The morphology of the films after the thermal treatment shows strong aligned crystallites resulting in a strong texture of the films. The electrical conductivity increases strongly during the 1st heating cycle to 900°C and stays almost constant afterwards. Compared to CCO-bulks, the films provide higher electrical conductivity which could be explained by the oriented crystal growth in-plane direction of the film.
The relationship between thermoelectric properties and layer morphology as a function of thermal annealing parameters will be further investigated.
Self-healing agents have the potential to restore mechanical properties and extend service life of composite materials. Thermoplastic healing agents have been extensively investigated for this purpose in epoxy matrix composites due to their strong adhesion to epoxy and their ability to fill in microcracks. One of the most
investigated thermoplastic additives for this purpose is poly(ethylene-co-methacrylic acid) (EMAA). Despite the ability of thermoplastic healing agents to restore mechanical properties, it is important to assess how the addition of thermoplastic healing agents affect properties of the original epoxy material. In this work, EMAA was added to epoxy resin and the effect of the additive on fracture toughness of epoxy was evaluated. Results indicate that although added in low concentrations, EMAA can affect fracture toughness.
Low-temperature co-fired ceramics (LTCC) are used to fabricate robust multilayer circuits. Typically, thick-film technology is applied for metallization. For specific sensor applications, thin films are deposited directly on the as-fired LTCC-surface. These deposited thin films are structured either by lift-off or by etching. The latter is less error-prone and thus preferred in industry provided the selected materials allow it.
200 nm Ni-thin films were deposited on three different commercial constrained-sintered LTCC (CT708, CT800 and DP951) by electron beam physical vapour deposition. The thin-films were structured by covering corresponding sections with a UV-curable photo resisn and subsequent etching of the uncovered surface, leaving behind the desired structure. The etched Ni-thin film showed high difference in failure rate and sheet resistance regarding the used LTCC-material. DP951 had the lowest sheet resistance and no failure, whereas the CT800 had a failure rate of 40 %. The LTCC with high failure rate showed a strong chemical attack by the used etching medium. To address this phenomenon, the chemical resistance of the three different commercial LTCC (CT708, CT800 and DP951) against four different commonly used etching media (sulphuric acid, phosphoric acid, aqua regia, and hydrofluoric acid) is investigated. The dissolved ions are analyzed by ICP-OES to correlate the LTCC-composition and its chemical resistance.
Destructive and non-destructive 3D-characterization of inner metal structures in ceramic packages
(2023)
Ceramic multilayer packages provide successful solutions for manifold
applications in telecommunication, microsystem, and sensor technology. In such packages, three-dimensional circuitry is generated by combination of structured and metallized ceramic layers by means of tape casting and multilayer technology. During development and for quality assurance in manufacturing, characterization of integrity, deformation, and positioning of the inner metal features is necessary.
Visualization with high resolution and material contrast is needed.
Robot-assisted 3D-materialography is a useful technique to characterize such multimaterial structures. In that, many sections of the specimen are polished and imaged automatically. A three-dimensional representation of the structure is created by digital combination of the image stack. A quasi non-destructive approach is to perform X-ray computer tomography (CT) with different beam energies. The energies are chosen to achieve a good imaging of either the metal features, or the ceramic matrix of the structure. The combination of the respective tomograms results in a high contrast representation of the entire structure. Both methods were tested to characterize Ag and Ag/Pd conductors in a ceramic multilayer package. The results were compared in terms of information content, effort, and applicability of the methods.
The increasing importance of resource availability and closed-loop material cycles are driving materials research to reduce alloying content in conventional materials or even substitute them with more sustainable alternatives. Intermetallic iron aluminide alloys (FeAl) present a potential alternative. Many alloy concepts for improved high-temperature properties or ductility have already been successfully implemented in casting technologies on a laboratory scale. However, successful testing of FeAl alloys on an industrial scale was still pending at the beginning of the project.
Therefore, the aim of the project was to develop simulation based casting concepts for industrial casting processes using the base alloy Fe-26Al-4Mo-0.5Ti-1B and to narrow down process limits by means of hot cracking tests. Findings were transferred into practice-oriented guidelines for casting of iron aluminides, which is accessible to future applicants in SMEs. The focus was placed on centrifugal casting combined with investment casting or die casting. In addition to numerous design and casting process parameters, heat treatments and alloying additions (Al, Mo, B) were varied to determine the influence of alloying elements on castability, microstructure and mechanical properties. Data from microstructure analyses (microscopic imaging, determination of grain sizes as well as phase compositions and volume fractions, fractography), mechanical tests (hardness measurements, compression tests, ambient and high-temperature tensile tests, creep tests) as well as measurements of thermophysical properties could be generated on the base alloy. Correlations of materials data with process variables allowed conclusions to be drawn on strengthening mechanisms and ductility of the alloy and how they can be controlled in terms of processing and component design. Successful casting of highly complex components with thin wall thicknesses and optimised alloy compositions points out prospects for new fields of application.
3D printing or additive manufacturing in space is of great value for long-term human spaceflight missions and space stations, conveniently offering access to a ‘virtual warehouse’ of tools and spare parts on the push of a button. The process only needs one type of feedstock such as powder or filament and only as much material as the final part requires, giving it a huge weight benefit over traditional subtractive methods.
While 3D printers are already operational on the ISS since 2014, the utilized processes are only capable of manufacturing relatively low strength parts from polymers not suitable for many tools or critical components. To gain access to high quality metal prints, a modified Laser Powder Bed Fusion (LPBF) process was developed to stabilize the critical powder bed in microgravity through a gas flow [2]. This setup was able to generate a (miniature) steel wrench during parabolic flights, but a reliable layer deposition has raised challenges due to the combination of gas flow parameters with microgravity conditions. Furthermore, the quality and density of the powder bed, which is critical for the process, cannot be examined afterward on the ground. This is due to hyper gravity phases during the flight that are influencing the properties of the powder bed.
In this paper, the challenges of the layer deposition are revised, and the subsequent evolution of the recoating system explained. Later, the challenges of an in-situ quality control, evaluation, and quantification of the properties of the powder bed are examined. As a solution, a high-resolution line-scanner is proposed and its implementation int the compact LPBF system demonstrated. Its ability to measure common defects such as ridges in the deposited layer is shown in experiments at normal gravity. As an illustration, Figure 1 shows an extreme case of the formation of ridges.
The increasing importance of resource availability and closed-loop material cycles are driving materials research to reduce alloying content in conventional materials or even substitute them with more sustainable alternatives. Intermetallic iron aluminide alloys (FeAl) present a potential alternative. Many alloy concepts for improved high-temperature properties or ductility have already been successfully implemented in casting technologies on a laboratory scale. However, successful testing of FeAl alloys on an industrial scale was still pending at the beginning of the project.
Therefore, the aim of the project was to develop simulation-based casting concepts for industrial casting processes using the base alloy Fe-26Al-4Mo-0.5Ti-1B and to narrow down process limits by means of hot cracking tests. Findings were transferred into practice-oriented guidelines for casting of iron aluminides, which is accessible to future applicants in SMEs. The focus was placed on centrifugal casting combined with investment casting or die casting. In addition to numerous design and casting process parameters, heat treatments and alloying additions (Al, Mo, B) were varied to determine the influence of alloying elements on castability, microstructure and mechanical properties. Data from microstructure analyses (microscopic imaging, determination of grain sizes as well as phase compositions and volume fractions, fractography), mechanical tests (hardness measurements, compression tests, ambient and high-temperature tensile tests, creep tests) as well as measurements of thermophysical properties could be generated on the base alloy. Correlations of materials data with process variables allowed conclusions to be drawn on strengthening mechanisms and ductility of the alloy and how they can be controlled in terms of processing and component design. Successful casting of highly complex components with thin wall thicknesses and optimised alloy compositions points out prospects for new fields of application.
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 aim of the task area Materials Data Infrastructure (TA-MDI) of the consortium Materials Science and Engineering (MatWerk) of National Research Data Infrastructure (NFDI) is to shape scientific datasets obtained through the Participant Projects (PPs) from a data management perspective conforming to the FAIR principles, making use of the FAIR Digital Object (FAIR DO) concept, including structured metadata and storage solutions. As an example, they apply PP18 (BAM) as a use case to demonstrate the proposed technical workflow.
Reference datasets in the MSE domain represent specific material properties, e.g., structural, mechanical, … characteristics. A reference dataset must fulfill high-quality standards, not only in precision of measurement but also in a comprehensive documentation of material, processing, and testing history (metadata). This Infrastructure Use Case (IUC) of the consortium Materials Science and Engineering (MatWerk) of National Research Data Infrastructure (NFDI) aims to develop, together with BAM and other Participant Projects (PP), a framework for generating reference material datasets using creep data of a single crystal Ni-based superalloy as a best practice example. In a community-driven process, we aim to encourage the discussion and establish a framework for identifying reference material datasets. In this poster presentation, we highlight our current vision and activities and intend to stimulate the discussion about the topic reference datasets and future collaborations and work.
Die HÜTTE ist ein Kompendium und Nachschlagewerk für unterschiedliche Aufgabenstellungen. Durch Kombination der Einzeldisziplinen dieses Wissenskreises kann das multidisziplinäre Grundwissen für die verschiedenen Technikbereiche und Ingenieuraufgaben zusammengestellt werden.
Die HÜTTE enthält in drei Bänden - orientiert am Stand von Wissenschaft und Technik und den Lehrplänen der Technischen Universitäten und Hochschulen - die Grundlagen des Ingenieurwissens.
Band 3 enthält die Elektro- und informationstechnische Grundlagen.
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 %, respectively. Due to the added complexity of the structure factor, much 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.
In nickelbasierten Superlegierungen, die für Gasturbinenschaufeln verwendet werden, sind bei hohen Betriebstemperaturen und -belastungen Kriechschäden, Ermüdung, Korrosion und Oxi-dation zu beobachten. Die betroffenen Turbinenschaufeln müssen ersetzt oder repariert werden, um Effizienzverluste und ein eventuelles Bauteilversagen zu vermeiden. In letzter Zeit wurden additive Fertigungs- und Lötverfahren für die Reparatur und das Fügen von Nickelbasiswerk-stoffen entwickelt, um die Einschränkungen der traditionellen Reparaturverfahren zu überwinden. Für eine auslegungsrelevante Bewertung des Risswachstumsverhaltens in den Fügezonen, die durch diese neuen Technologien erzeugt werden, sind Rissfortschrittsuntersuchungen erfor-derlich. Entsprechende Untersuchungen an gefügten Proben werden in diesem Beitrag vorge-stellt. Die Rissfortschrittsversuche werden an gefügten SEN-Proben (Single Edge Notch) bei einem Spannungsverhältnis von 0,1 und einer Temperatur von 950 °C durchgeführt. Das Riss-wachstum wird mit der DCPD-Methode (Direct Current Potential Drop) überwacht, und die ge-messenen Potenzialsignale werden anhand der optisch vermessenen Risslänge und einer Finite-Elemente-Analyse kalibriert. Der Spannungsintensitätsfaktor (SIF) für die gefügte SEN-Geometrie wird mit Hilfe von Finite-Elemente-Analysen berechnet. Auf diese Weise können Rissfortschrittskurven aus den experimentellen Daten abgeleitet werden.
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.
The KupferDigital project aims to develop digital methods, tools, and data space infrastructures for digitalizing the entire life cycle of copper materials. The mechanical testing process is one of the main chains of such life cycles which generates lots of important testing data about the mechanical properties of the materials and their related materials and testing metadata. To train the digitalization of the mechanical testing process, different kinds of copper alloys were provided for this project, and their mechanical properties were measured by typical methods like Brinell and Vickers hardness and tensile testing. The primary raw testing data as well as the secondary datasets of these tests are provided. The detailed materials specifications, the utilized mechanical testing methods, and provided datasets are described in the content file. The test data files of heterogeneous structures are processed by the KupferDigital digital tools to be converted to standardized machine-readable data files.
Due to their unique physico-chemical properties, nanoparticles are well established in research and industrial applications. A reliable characterization of their size, shape, and size distribution is not only mandatory to fully understand and exploit their potential and develop reproducible syntheses, but also to manage environmental and health risks related to their exposure and for regulatory requirements. To validate and standardize methods for the accurate and reliable particle size determination nanoscale reference materials (nanoRMs) are necessary. However, there is only a very small number of nanoRMs for particle size offered by key distributors such as the National Institute of Standards and Technology (NIST) and the Joint Research Centre (JRC) and, moreover, few provide certified values. In addition, these materials are currently restricted to polymers, silica, titanium dioxide, gold and silver, which have a spherical shape except for titania nanorods. To expand this list with other relevant nanomaterials of different shapes and elemental composition, that can be used for more than one sizing technique, we are currently building up a platform of novel nanoRMs relying on iron oxide nanoparticles of different shape, size and surface chemistry. Iron oxide was chosen as a core material because of its relevance for the material and life sciences.
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.
Als elektrische Durchschlagfestigkeit bezeichnet man die elektrische Feldstärke, bei der es zur Entladung durch ein isolierendes Medium kommt. Im Falle von Festkörpern ist dies ein zerstörender Prozess. Bei der messtechnischen Bestimmung der Durchschlagfestigkeit haben neben den verwendeten Messgeräten auch die eingesetzten Elektroden, die Form des Prüfkörpers und das Isoliermedium, in dem die Prüfung stattfindet, einen signifikanten Einfluss auf die ermittelten Messwerte. Im Vortrag werden die Einflüsse erläutert und anhand von Messreihen aus der Literatur und der eigenen Forschung quantifiziert. Aufgrund der vorgestellten Effekte wird klar, dass es sich bei elektrischer Durchschlagfestigkeit nicht um absolute Materialkennwerte handelt, sondern vielmehr um systemabhängige Größen.
A new patented dynamic mechanical analysis (DMA) is presented, where the tensile, bending- or torsional stiffness of a media can be characterized in-situ during the phase transition from liquid to solid. An epoxy system, e.g. Hexion L285/H287, is filled into an elastomer container, such as a silicone tube. This can be mounted into a conventional OMA and, based on a linear viscoelastic approach, the storage modulus (E';G'), the loss modulus (E'';G'') and the loss angle tan(δ) can be measured at constant temperature as a function of time in order to investigate the liquid to sol-gel to solid transition. With this new method, the stiffness increase as a result of the cure process can be directly measured more precisely than with a rheometer in a shear plate set-up, because using an elastomer container gives a defined cross section for calculating the Young's modulus.
Lithium-ion batteries (LIBs) are one technology to overcome the challenges of climate and energy crisis. They are widely used in electric vehicles, consumer electronics, or as storage for renewable energy sources. However, despite innovations in batteries' components like cathode and anode materials, separators, and electrolytes, the aging mechanism related to metallic aluminum current collector degradation causes a significant drop in their performance and prevents the durable use of LIBs.[1] Glow-discharge optical emission spectroscopy (GD-OES) is a powerful method for depth-profiling of batteries' electrode materials. This work investigates aging-induced aluminum deposition on commercial lithium cobalt oxide (LCO) batteries' cathodes. The results illustrate the depth-resolved elemental distribution from the cathode surface to the current collector. An accumulation of aluminum is found on the cathode surface by GD-OES, consistent with results from energy-dispersive X-ray spectroscopy (EDX) combined with focused ion beam (FIB) cutting. In comparison to FIB-EDX, GD-OES allows a fast and manageable depth-profiling. Results from different positions on an aged cathode indicate an inhomogeneous aluminum film growth on the surface. The conclusions from these experiments can lead to a better understanding of the degradation of the aluminum current collector, thus leading to higher lifetimes of LIBs.
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.
Fully-reversed fatigue behavior of scarf joint repairs for wind turbine blade shell applications
(2022)
To enable a quick and cost-effective return to service for wind turbine blades, localized repairs can be executed by technicians in the field. Scarf repairs, shown to be highly efficient with a smooth load transition across angled joint walls and a restored aerodynamic profile, are the focus of this work. The failure mechanisms of these structures were examined under quasi-static tensile and fully-reversed cyclic loading. While the scarf ratio was held constant at 1:50, the repair layup was varied between large-to-small and small-to-large. The effect of the presence of resin pockets and the fiber orientation mismatch between parent and repair material on the restored strength of BIAX ±45° glass fiber reinforced polymer scarf joint structures was studied.
In failure analysis, micro-fractographic analysis of fracture surfaces is usually performed based on practical knowledge which is gained from available studies, own comparative tests, from the literature, as well as online databases. Based on comparisons with already existing images, fracture mechanisms are determined qualitatively. These images are mostly two-dimensional and obtained by light optical and scanning electron imaging techniques. So far, quantitative assessments have been limited to macrocopically determined percentages of fracture types or to the manual measurement of fatigue striations, for example. Recently, more and more approaches relying on computer algorithms have been taken, with algorithms capable of finding and classifying differently structured fracture characteristics. For the Industrial Collective Research (Industrielle Gemeinschaftsforschung, IGF) project “iFrakto” presented in this paper, electron-optical images are obtained, from which topographic information is calculated. This topographic information is analyzed together with the conventional 2D images. Analytical algorithms and deep learning are used to analyze and evaluate fracture characteristics and are linked to information from a fractography database. The most important aim is to provide software aiding in the application of fractography for failure analysis. This paper will present some first results of the project.
Die Steigerung der Leistung und des thermodynamischen Wirkungsgrades von Verbrennungsmotoren führt zu erhöhten Anforderungen an die Festigkeit abgasführender Komponenten wie z. Bsp. Abgasturbolader. Als Folge erhöhter thermomechanischer Wechselbeanspruchungen (TMF) im Betrieb kommt es an den mechanisch und/oder thermisch höchst beanspruchten Stellen der Bauteile zur Bildung von Rissen, wodurch die Lebensdauer der Komponenten begrenzt wird. Derzeit werden bei Turboladern heißgehende Bauteile mit detektierten Rissen zumeist prophylaktisch ersetzt, da die weitere Ausbreitung der Risse während des Betriebs nicht vorhergesagt werden kann. Um diese aufwändige und un- ökonomische Praxis zu vermeiden, wurde im vorliegenden Forschungsvorhaben eine rechnerische Bewertungsmethode auf Basis der experimentellen und numerischen Bruchmechanik erarbeitet, mit deren Hilfe bereits in der Auslegungsphase oder während des Betriebs die (restliche) Lebensdauer der abgasführenden Komponenten vorhergesagt werden kann. Damit wird erstmalig die quantitative Vorhersage der Rissentwicklung bei TMF-Beanspruchungsbedingungen unter Berücksichtigung großer zyklischer viskoplastischer Verformungen ermöglicht.
Zentrales Ergebnis des Vorhabens ist eine automatisierte Berechnungsprozedur auf der Basis spezieller Finite-Elemente-Techniken (FEM), womit sowohl der Pfad als auch die Größe eines Risses als Funktion der Anzahl der Lastwechsel in Bauteilen unter TMF-Bedingungen berechnet werden kann. Als geeigneter Beanspruchungsparameter zur Bewertung des Rissfortschritts unter TMF wurde die zyklische Rissöffnungsverschiebung ΔCTOD verwendet. Das Werkstoffverhalten des betrachteten austenitischen Gusseisens Ni-Resist D-5S wurde mit einem validierten viskoplastischen, temperaturabhängigen Materialmodell modelliert, das zur Berücksichtigung große Verzerrungen und Rotationen am Riss erweitert wurde. Für die genaue Berechnung des ΔCTOD bei TMF wurden effiziente FEM-Techniken erarbeitet. Zur Simulation der Rissausbreitung wurde ein automatischer FEM-Algorithmus mit inkrementeller adaptiver Neuvernetzung entwickelt, bei dem die Verformungen und inelastischen Zustandsvariablen jeweils vom alten auf das neue Netz übertragen werden. Dieser Algorithmus wurde im Software-Paket ProCrackPlast implementiert, das in Verbindung mit dem kommerziellen FEM-Code Abaqus zur Lösung dreidimensionaler Rissprobleme zur Verfügung steht. Ziel der umfangreichen experimentellen Arbeiten war es, an isothermen LCF und anisothermen TMF-Versuchen mit gekerbten Flachzugproben (SENT) das Risswachstum im Temperaturbereich von 20 °C bis 700 °C zu ermitteln. Mit Hilfe begleitender 2D FEM Simulationen wurden anhand dieser Datenbasis die Rissfortschrittskurven des Werkstoffs unter Anwendung des ΔCTOD-Konzepts bestimmt und in geeigneter, parametrisierter Form den Nutzern zur Verfügung gestellt. Die Versuche an SENT-Proben wurden mit der entwickelten Software ProCrackPlast als 3D Modell simuliert. Der Vergleich der 2D und 3D Simulationen ergab einen systematischen Unterschied im CTOD und CTOD, der mit Hilfe eines Übertragungsfaktors korrigiert wurde. Der Vergleich der 3D Berechnungen mit den Experimenten zeigte eine zufriedenstellende Übereinstimmung der er- reichten Risslänge mit der Zahl der Lastzyklen im gesamten Temperaturbereich, wobei die numerische Prognose meist auf der konservativen / sicheren Seite lag. Die Übertragbarkeit der Ergebnisse der 2D Parameteridentifikation auf 3D Risskonfigurationen mit Mixed-Mode Beanspruchung ist mit zusätzlichen Versagenshypothesen verbunden, die aufgrund fehlender Versuchsdaten im Vorhaben nicht endgültig geklärt werden konnten. Zur Validierung des Gesamtkonzeptes wurden LCF-Proben mit einem bauteil- typischen Oberflächenriss experimentell und numerisch untersucht. In der Simulation konnte die komplexe Form und Größe der Rissentwicklung zufriedenstellend (richtig) vorhergesagt werden. Die Leis- tungsfähigkeit der erarbeiteten rechnerische Bewertungsmethode wurde an weiteren TMF-Beispielen vorgestellt und diskutiert. Die Software ProCrackPlast und die viskoplastische Materialroutine wurden dem Anwenderkreis des Vorhabens zusammen mit einem Nutzer-Handbuch und Verifikationsbeispielen zur Verfügung gestellt.
Das Ziel des Forschungsvorhabens ist erreicht worden.
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.
Due to combined cyclic mechanical and thermal loading during operation, the material of exhaust gas conducting components of combustion engines is exposed to thermomechanical fatigue (TMF). This leads to formation and growth of cracks, especially at the most highly stressed points of these components. In order to better predict the service life of cracked components before failure, it is necessary to identify a crack propagation law for the material used. Isothermal crack propagation tests have been carried out at several temperatures with a typical cast iron to identify such a law. The crack length is measured by the potential drop method. The compliance method, fractography and thermographic camera measurements have been used to validate and calibrate the potential drop measurements. Each of the isothermal tests has been simulated using a specially developed FEM-algorithm based on remeshing and remapping. This algorithm has been implemented in python and ABAQUS. Thereby, the crack tip region is modeled by collapsed Quad8 elements. From the individual simulations, the cyclic crack tip opening displacement (ΔCTOD) is extracted and regarded as a potential fracture mechanics parameter which controls the crack growth rate. By combining the data from the experiments and the simulations, the crack propagation law has been identified. Finally, anisothermal crack propagation tests have been performed for validation of the crack growth law.
Die zunehmende geopolitische Bedeutung der Ressourcenverfügbarkeit sowie die Anforderungen an einen geschlossenen Materialkreislauf treiben die Materialforschung voran, um konventionelle Werkstoffe mit weniger kritischen Zusätzen zu legieren oder sogar vollständig mit nachhaltigeren Alternativen zu substituieren. Eine potenzielle Alternative stellen die intermetallischen Eisenaluminid-Legierungen (FeAl) dar. Im Labormaßstab wurden bereits viele Legierungskonzepte für verbesserte Hochtempera- tureigenschaften oder Duktilität erfolgreich gießtechnisch umgesetzt. Eine erfolgreiche Erprobung von FeAl-Legierungen im industriellen Maßstab stand zu Beginn des Projekts aber weiterhin aus. Ziel des Vorhabens war daher die Entwicklung von simulationsgestützten Gießkonzepten in industrienahe Gießprozesse anhand der Modelllegierung Fe-26Al-4Mo-0,5Ti-1B und die Eingrenzung der prozesstechnischen Verfahrensgrenzen durch Warmrissversuche. Erkenntnisse hieraus wurden in einen praxisorientierten, für zukünftige Anwender in KMUs zugänglichen Handlungskatalog für die gießgerechte Auslegung von Bauteilen aus Eisenaluminiden überführt. Fokus wurde insbesondere auf das Feinguss- und Kokillengussverfahren im Schleuderguss gesetzt. Neben zahlreicher Konstruktions- und Gießprozessparameter wurden auch Wärmebehandlungen und Legierungszusätze (Al, Mo, B) variiert, um den Einfluss von Legierungselementen auf Gießbarkeit, Mikrostruktur und mechanische Kennwerte zu be- stimmen. Eine umfangreiche Basis an Daten aus Mikrostrukturanalysen (Mikroskopische Bildgebung, Bestimmung von Korngrößen sowie Phasenzusammensetzungen und -anteilen, Fraktographie), mechanischen Tests (Härtemessungen, Druckversuch, Zugversuch, Warmzugversuch, Kriechversuch) sowie Messungen thermophysikalischer Eigenschaften konnte für die Modelllegierung erzeugt werden. Korrelationen dieser Informationen mit Prozessvariablen erlaubten Schlussfolgerungen zu Härtungsmechanismen und Duktilität in der Legierung und wie sie prozesstechnisch in Gieß- und Bauteilauslegung gesteuert werden können. Der erfolgreiche Abguss von hochkomplexen Bauteilgeometrien mit dünnen Wandstärken sowie optimierte Legierungszusammensetzungen zeigen Perspektiven auf neue Anwendungsfelder auf.
Das Ziel des Forschungsvorhabens ist erreicht worden.
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.
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.
Das hochaktuelle Thema der Integration und Wiederverwendung von Wissen und Daten aus Herstellung, Bearbeitung und Charakterisierung von Materialien ('Digitalisierung von Materialien') wird in den Projekten Innovationsplattform MaterialDigital (PMD, materialdigital.de) und Materials-open-Lab (Mat-o-Lab, matolab.org) adressiert. In diesem Beitrag werden die Weiterentwicklungen in diesen Projekten hinsichtlich der Speicherung von Zugversuchsdaten gemäß einer normenkonformen (DIN EN ISO 6892-1:2019-11) ontologischen Repräsentation vorgestellt. Das umfasst den Weg von der Entwicklung einer Ontologie nach Norm, der Konvertierung von Daten aus Standardtests in das interoperable RDF-Format bis hin zur Verknüpfung von Ontologie und Daten. Letztendlich können die entsprechenden Daten in einem Triple Store abgelegt und abgefragt werden.
Komponenten von Fahrrädern werden im Betrieb vorwiegend schwingend beansprucht. Typische Werkstoffe sind Stahl, Aluminiumlegierungen, Messing, CFK und thermoplastische Kunststoffe. Da es sich, unabhängig von der Preiskategorie, um konstruktiven Leichtbau handelt, werden einige Bauteile betriebsfest mehr oder weniger weit oberhalb der Dauerfestigkeit ausgelegt. Die im normalen Betrieb auftretenden Schäden sind daher weit überwiegend Schwingbrüche. Andere Schadensmechanismen wie z.B. Korrosion spielen quantitativ eine untergeordnete Rolle. Schwingbrüche treten nach einer Periode unbemerkten Risswachstums oft ohne Vorwarnung und ohne makroskopische Verformung auf. Im Falle von sicherheitsrelevanten Komponenten wie Rahmen, Gabeln, Lenkern, Sattelstützen, Kurbelarmen oder Pedalen kann dies zu erheblichen Personenschäden führen, die den Wert des ursächlichen Bauteilschadens weit überschreiten.
Über einen langjährigen Zeitraum wurden gebrochene Komponenten aus dem Alltag und aus Gerichtsverfahren analysiert. Das Hauptaugenmerk lag hierbei auf der fraktographischen Analyse, teilweise wurden die zu Grunde liegenden Schadensursachen ermittelt. Einflussfaktoren sind beispielsweise konstruktive Kerben an ungünstigen Stellen, aber auch Werkstoffwahl und Fertigungsqualität spielen eine Rolle. In den meisten Fällen wurde jedoch die konstruktive Lebensdauer überschritten. Diese wird praktisch nie mitgeteilt, und eine wiederkehrende Prüfung sicherheitsrelevanter Bauteile findet nicht statt.
Im Sinne der Vermeidung von Schäden und Unfällen könnte darauf hingewirkt werden, für sicherheitsrelevante Komponenten Lebensdauern besser abzuschätzen und von der Laufleistung abhängige Sichtprüfungen zu empfehlen.
Small-angle scattering data analysis round robin - Anonymized results, figures and Jupyter notebook
(2023)
The intent of this round robin was to find out how comparable results from different researchers are, who analyse exactly the same processed, corrected dataset.
This zip file contains the anonymized results and the jupyter notebook used to do the data processing, analysis and visualisation. Additionally, TEM images of the samples are included.
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.
Laser powder bed fusion (PBF-LB/M) of metallic alloys is a layer wise additive manufacturing process which provides significant scope for more efficient designs of components, benefiting performance and weight, leading to efficiency improvements for various sectors of industry. However, to benefit from these design freedoms, knowledge of the high produced induced residual stress and mechanical property anisotropy associated with the unique microstructures is critical. X-ray and neutron diffraction are considered the benchmark for non-destructive characterization of surface and bulk internal residual stress. The latter, characterized by the high penetration power in most engineering alloys, allows for the use of diffraction angle close to 90° enabling a near cubic sampling volume to be specified. However, the complex microstructures of columnar growth with inherent crystallographic texture typically produced during PBF-LB/M of metallics present significant challenges to the assumptions typically required for time efficient determination of residual stress. These challenges include the selection of an appropriate set of diffraction elastic constants and a representative strain-free reference for the material of interest. In this presentation advancements in the field of diffraction-based residual stress analysis of L-PBF Inconel 718 will be presented. The choice of an appropriate set of diffraction-elastic constants depending on the underlying microstructure will be described.
In diesem Artikel werden die verschiedenen additiven Fertigungsverfahren und ihre Anwendungsmöglichkeiten vorgestellt. Der Fokus liegt hierbei auf Silikatkeramik. Für jedes 3D Druckverfahren werden die Möglichkeiten mit Silikatkeramik, Hochleistungskeramik und Dentalkeramik aufgezeigt. Auf den Nutzen der verschiedenen 3D Druckverfahren für industrielle Anwendungen, den privaten Bereich, sowie die Verwendung für Kunst und Design wird eingegangen. Das Potenzial der Additiven Fertigung wird auch für den Bereich der Keramik in der dentalen Anwendung bewertet.
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.
Das zyklische plastische Verformungsverhalten von additiv gefertigtem Edelstahl AISI 316L wurde in dehnungsgeregelten Kurzzeitfestigkeitsversuchen (LCF-Versuchen) untersucht. Dabei wurden zwei Wärmebehandlungszustände betrachtet: Beim ersten Zustand war die fertigungsbedingte zelluläre Struktur vorhanden, während sie durch die zweite Wärmebehandlung aufgelöst wurde. Untersuchungen im Transmissions-Elektronen-Mikroskop (TEM) zeigten, dass die zyklische Verformung die Zellstruktur lokal zerstörte und Gleitbänder entstanden, was die Entfestigung in diesem Fall erklärt. Für Material ohne Zellstrukturen resultierten nach zyklischer Verformung ähnliche Versetzungsstrukturen wie in konventionell gefertigtem (warmgewalzten) Material.
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.
Seit Beginn der Luftfahrt Anfang des letzten Jahrhunderts ist die Menschheit auf der Suche nach neuen Materialien, die das Abenteuer Fliegen sicherer, angenehmer, schneller und rentabler gestalten. Hochentropielegierungen sind solche vielversprechenden Materialien. Die richtige Analytik hilft dabei, besser zu verstehen, wie deren Zusammensetzung und atomare Anordnung die makroskopischen Eigenschaften beeinflusst.
Der Beitrag beinhaltet Themen vom H2Safety@BAM-Kompetenzfeld Sensorik, Analytik und zertifizierte Referenzmaterialien (SensRef) mit Fokus auf Mess- und Prüfverfahren mit verschiedenen Sensortechnologien und Ultraschallwellen:
Metrologie zur Wasserstoffspeicherung - Euramet-Vorhaben "MefHySto",
Erkennung von freigesetztem Wasserstoff sowie die Bestimmung des Wasserstoff-Luftverhälntisses mit Gassensoren, zerstörungsfreie Fehlstellenerkennung mit integriertem Zustandsüberwachungssystem basierend auf geführten Ultraschallwellen zur Lebensdauerüberwachung von Composite-Behältern (Wasserstoffspeicher) sowie faseroptische Sensorik zur Schadenfrüherkennung von Wasserstoffspeichern aufgrund erkennbarer Dehnungsänderungen an Druckbehältern.
Within NFDI-MatWerk (“National Research Data Infrastructure for Material Sciences”/ “Nationale Forschungsdateninfrastruktur für Materialwissenschaften und Werkstofftechnik“), the Task Area Materials Data Infrastructure (TA-MDI) will provide tools and services to easily store, share, search, and analyze data and metadata. Such a digital materials environment will ensure data integrity, provenance, and authorship. The MatWerk consortium aims to develop specific solutions jointly with Participant Projects (PPs), which are scientific groups or institutes covering different domains, from theory and simulations to experiments. The Data Exploitation Methods group of the Karlsruhe Institute of Technology-Steinbuch Centre of Computing, as part of TA-MDI, is developing specific solutions in close collaboration with three PPs.
PP07, together with the University of Stuttgart, aims at the image-based prediction of the material properties of stochastic microstructures using large-scale supercomputers. PP13, in cooperation with the University of Saarland, focuses on tomographic methods at various scales in materials research. PP18, together with the Federal Institute for Materials Research and Testing (“Bundesanstalt für Materialforschung und -prüfung”), aspires to define the criteria for materials reference datasets and usage analytics.
The requirements and goals are comparable for each PP: their research outputs, which are scientific datasets, should conform to the FAIR (Findable, Accessible, Interoperable, Reusable) principles. We aim to shape them from a data management perspective making use of the FAIR Digital Object concept, including structured metadata and storage solutions. The results will be a blueprint which will act as a reference for future datasets. Even though the collaboration is in an early stage, the initial steps already show the added value of this approach.
This research has been supported by the Federal Ministry of Education and Research
(BMBF) – funding code M532701 / the Deutsche Forschungsgemeinschaft (DFG, German
Research Foundation) - project number NFDI 38/1, project no. 460247524.
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.
Investigation of degradation of the aluminum current collector in lithium-ion batteries by GD-OES
(2022)
Lithium-ion batteries (LIBs) are one technology to overcome the challenges of climate and energy crisis. They are widely used in electric vehicles, consumer electronics, or as storage for renewable energy sources. However, despite innovations in batteries' components like cathode and anode materials, separators, and electrolytes, the aging mechanism related to metallic aluminum current collector degradation causes a significant drop in their performance and prevents the durable use of LIBs. Glow-discharge optical emission spectroscopy (GD-OES) is a powerful method for depth-profiling of batteries' electrode materials. This work investigates aging-induced aluminum deposition on commercial lithium cobalt oxide (LCO) batteries' cathodes. The results illustrate the depth-resolved elemental distribution from the cathode surface to the current collector. An accumulation of aluminum is found on the cathode surface by GD-OES, consistent with results from energy-dispersive X-ray spectroscopy (EDX) combined with focused ion beam (FIB) cutting. In comparison to FIB-EDX, GD-OES allows a fast and manageable depth-profiling. Results from different positions on an aged cathode indicate an inhomogeneous aluminum film growth on the surface. The conclusions from these experiments can lead to a better understanding of the degradation of the aluminum current collector, thus leading to higher lifetimes of LIBs.
Trace elements play an important role in the fine-tuning of complex material properties. This study focuses on the correlation of microstructure, lattice misfit and creep properties. The compositionally complex alloy Al10Co25Cr8Fe15Ni36Ti6 (in at. %) was tuned with high melting trace elements Hf and W. The microstructure consists of a γ matrix, γ' precipitates and the Heusler phase and it is accompanied by good mechanical properties for high temperature applications. The addition of 0.5 at.% Hf to the Al10Co25Cr8Fe15Ni36Ti6 alloy resulted in more sharp-edged cubic γ′ precipitates and an increase in the Heusler phase amount. The addition of 1 at.% W led to more rounded γ′ precipitates and the dissolution of the Heusler phase. The shapes of the γ' precipitates of the alloys Al9.25Co25Cr8Fe15Ni36Ti6Hf0.25W0.5 and Al9.25Co25Cr8Fe15Ni36Ti6Hf0.5W0.25, that are the alloys of interest in this paper, create a transition from the well-rounded precipitates in the alloy with 1% W containing alloy to the sharp angular particles in the alloy with 0.5% Hf. While the lattice misfit has a direct correlation to the γ' precipitates shape, the creep rate is also related to the amount of the Heusler phase. The lattice misfit increases with decreasing corner radius of the γ' precipitates. So does the creep rate, but it also increases with the amount of Heusler phase. The microstructures were investigated by SEM and TEM, the lattice misfit was calculated from the lattice parameters obtained by synchrotron radiation measurements.
The Global Exploration Strategy of the International Space Exploration Coordination Group (ISECG) describes a timeframe of 2020 and beyond with the ultimate aim to establish a human presence on Mars towards the 2040ies. The next steps lie on the Moon with a focus on the coming 10 years. Early lunar surface missions will establish a capability in support of lunar science and prepare and test mission operations for subsequent human exploration of Mars and long-duration human activities on the Moon.
Given the extreme costs involved in the shipping of material from Earth, a prerequisite for future human exploration is the manufacturing of elements directly on the Moon’s surface. Unlike the equipment, which at the beginning will have to be brought from Earth, raw materials and energy could be available following the concept of In-Situ Resource Utilization. The ESA OSIP PAVING THE ROAD (PAVER) study investigates the use of a laser to sinter regolith into paving elements for use as roadways and launch pads thus mitigating dust issues for transport and exploration vehicles.
The ESA-funded study examines the potential of using a laser (12 kW CO2 laser with spot beam up to 100 mm) for layer sintering of lunar and martian regolith powders to manufacture larger 3D elements and provide know-how for the automatic manufacture of paving elements in the lunar environment. The project contributes to the first step toward the establishment of a lunar base and will lead to the construction of equipment capable of paving areas and manufacturing 3D structures.
PAVER project sets the starting point for an examination of the larger context of lunar exploration. Mission scenarios will look at different phases of lunar exploration: Robotic Lunar Exploration, Survivability, Sustainability, and Operational Phase. A proposed Technology Roadmap investigates the mission scenario and analyses how, and to which extent, laser melting/sintering will play a role in the various phases of exploration. The paper contextualizes laser sintering within selected mission scenarios and discusses the different kinds of infrastructure that can be produced at each phase of the mission. The outcome of the study includes the detailing of the TRL steps in the project and an outline of a timeline for the different elements. Covered aspects include terrain modelling such as operation pads, roadways, or towers, non-pressurized building structures to protect machinery, and habitat envelopes, to protect and shield humans against dust, micrometeoroids, and radiation.
Powder bed technologies are amongst the most successful Additive Manufacturing (AM) techniques. Powder bed fusion and binder jetting especially are leading AM technologies for metals and polymers, thanks to their high productivity and scalability. The application of these techniques to most ceramics has been difficult so far, because of the challenges related to the deposition of homogeneous powder layers when using fine powders. In this context, the “layerwise slurry deposition” (LSD) has been developed as a layer deposition method which enables the use of powder bed AM technologies also for advanced ceramic materials. The layerwise slurry deposition consists of the layer-by-layer deposition of a ceramic slurry by means of a doctor blade, in which the slurry is deposited and dried to achieve a highly packed powder layer. This offers high flexibility in the ceramic feedstock used, especially concerning material and particle size. The LSD technology can be combined with binder jetting to develop the so-called “LSDprint” process for the additive manufacturing of ceramics. The LSDprint technology combines the high-speed printing of binder jetting with the possibility of producing a variety of high-quality ceramics with properties comparable to those achieved by traditional processing. In this presentation, the LSD process will be introduced and several examples of application ranging from silicate to high-performance ceramics will be shown. Recent developments towards the scale-up and industrialization of this process will be discussed, alongside future perspectives for the multi-material additive manufacturing.
At the Workshop "Neutron and Synchrotron Monitoring in Aerospace Advanced Manufacturing" at the Institute of Materials Physics in Space, German Aerospace Center (DLR) in Cologne, we presented on the opportunities and our experiences of using a powder based additive manufacturing process for in-space manufacturing applications in microgravity.
The Global Exploration Strategy of the International Space Exploration Coordination Group (ISECG) describes a timeframe of 2020 and beyond with the ultimate aim to establish a human presence on Mars towards the 2040ies. The next steps lie on the Moon with a focus on the coming 10 years. Early lunar surface missions will establish a capability in support of lunar science and prepare and test mission operations for subsequent human exploration of Mars and long-duration human activities on the Moon.
Given the extreme costs involved in the shipping of material from Earth, a prerequisite for future human exploration is the manufacturing of elements directly on the Moon’s surface. Unlike the equipment, which at the beginning will have to be brought from Earth, raw materials and energy could be available following the concept of In-Situ Resource Utilization. The ESA OSIP PAVING THE ROAD (PAVER) study investigates the use of a laser to sinter regolith into paving elements for use as roadways and launch pads thus mitigating dust issues for transport and exploration vehicles.
The ESA-funded study examines the potential of using a laser (12 kW CO2 laser with spot beam up to 100 mm) for layer sintering of lunar and martian regolith powders to manufacture larger 3D elements and provide know-how for the automatic manufacture of paving elements in the lunar environment. The project contributes to the first step toward the establishment of a lunar base and will lead to the construction of equipment capable of paving areas and manufacturing 3D structures.
PAVER project sets the starting point for an examination of the larger context of lunar exploration. Mission scenarios will look at different phases of lunar exploration: Robotic Lunar Exploration, Survivability, Sustainability, and Operational Phase. A proposed Technology Roadmap investigates the mission scenario and analyses how, and to which extent, laser melting/sintering will play a role in the various phases of exploration. The paper contextualizes laser sintering within selected mission scenarios and discusses the different kinds of infrastructure that can be produced at each phase of the mission. The outcome of the study includes the detailing of the TRL steps in the project and an outline of a timeline for the different elements. Covered aspects include terrain modelling such as operation pads, roadways, or towers, non-pressurized building structures to protect machinery, and habitat envelopes, to protect and shield humans against dust, micrometeoroids, and radiation.
As part of a joint project involving the Fraunhofer Institute for Silicate Research (ISC), the Friedrich Schiller University of Jena, the Clausthal University of Technology and the Federal Institute for Materials Research and Testing (BAM), digital tools are to be created for the development of new types of glass materials. Current processes for the production of glasses with improved properties are usually very cost- and energy-intensive due to the low degree of automation and are subject to long development cycles. The use of robotic synthesis processes in combination with self-learning machines is intended to overcome these problems in the long term. The development of new types of glass can then not only be accelerated considerably, but also be achieved with much less effort.
In this talk, data generation via a robotic high-throughput glass melting system is presented, which should be the experimental basis for the ontology developed within the project GlasDigital.
Although the slow crack growth in glass is dominated by stress-corrosion phenomena, it also should reflect the underlaying intrinsic fracture behavior controlled by glass chemistry and structure. To investigate such underlaying phenomena, crack growth velocity in alkali silicate glasses was measured in vacuum across 10 orders of magnitude with double cantilever beam technique. Measured and literature crack growth data were compared with calculated intrinsic fracture toughness data obtained from Young’s moduli and theoretical fracture surface energy. Data analysis reveals slight correlation with the packing density and significant deviations from the intrinsic brittle fracture behavior. These deviations do not follow simple compositional trends. Two opposing processes may explain this finding: a decrease in the apparent fracture surface energy due to stress-induced chemical changes at the crack tip and its increase due to energy dissipation during fracture.
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.
Efforts towards digitalization in the material science and technology community have enhanced in the last years. In 2019 the German digitalization initiative platform „MaterialDigital“1 (MD) has been started. Numerous projects concerning digitalization, including the copper related project „KupferDigital“ (copper digital) have been initiated under the umbrella of MD. The initiative strives to
address numerous issues concerning data access, exchange, security, provenance and sovereignty. Heterogeneous data origin, storage and evaluation often result in problems concerning comparability and reproducibility of scientific and technological results. In many cases material data are recorded, but the methods of testing are insufficiently described, or such information is not communicated along with the raw data. The material data can also have numerous different formats such as paper printouts, pdfs, excel sheets or csv-files. Hence, gathering and integrating material data from different sources is challenging for potential users like materials scientists and engineers, especially if there are contradictory data where the reasons for contradictions is not clear due their vague description. In order to address these problems, data should comply to the so called „FAIR“ principle which calls for data to be findable, accessible, interoperable, and reusable (FAIR)2 and hence be accessible via so-called decentralized but interconnected data spaces. By using knowledge representation withontologies, data can be enriched with meaning and the methods of the testing procedures can be accurately provided. In this presentation we want to introduce our approach to such knowledge representation based on a high-throughput alloy development process for Cu-based alloys³ along with characterization techniques such as hardness testing and microstructural characterization (e.g. EBSD – Electron Backscattered Diffraction).
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.
Kern des Projektes KupferDigital ist es, einen Demonstrator für ein digitales Datenökosystem zu erstellen, der der Digitalisierung der Materialforschung und der metallverarbeitenden Industrie als zukunftsfähige Plattform zur Verfügung stehen soll. Das Projekt KupferDigital entwickelt Methoden und Konzepte, um den Lebenszyklus am Beispiel von Kupfer – von der Erzgewinnung bis zum Recycling – digital zu erfassen. Grundlage ist die Entwicklung sogenannter Ontologien. Diese können als eine Art Wissensnetz verstanden werden. Sie dienen als gemeinsame Standards für die Beschreibung von Werkstoffen und technischen Vorgängen. Sie helfen bei der digitalen Erfassung von Prozessschritten sowie von Materialeigenschaften. Parallel dazu werden Konzepte für Datenstrukturen, die Speicherung und den Austausch von Werkstoffdaten über neu zu definierende Schnittstellen erarbeitet.
Über die Bereitstellung digitalisierter Lebenszyklen von Kupfer wird die Industrie bei der Pro-duktentwicklung befähigt, neue Werkstoffentwicklungen frühzeitig zu bewerten, beispielsweise unter dem Gesichtspunkt der Nachhaltigkeit. Kupfer kommt hier eine aktuelle Bedeutung zu, weil es für die digitale Transformation sowie die Energie- und Mobilitätswende von fundamentaler Bedeutung ist und somit von hohem gesellschaftlichem Wert. Die Projektziele sind sowohl auf weitere metallische Struktur- und Funktionswerkstoffe als auch auf andere Industriebereiche übertragbar.
Die Projektergebnisse werden im Rahmen der Aktivitäten der Innovationsplattform MaterialDigital allen Interessierten zur Verfügung gestellt.
3D-printed landing pads on the moon: Paving the road for large area sintering of lunar regolith.
A prerequisite for lunar exploration and beyond is the manufacturing of objects directly on the moon, given the extreme costs involved in the shipping of material from Earth. Looking at processes, raw materials, and energy sources, equipment will certainly have to be brought from Earth at the beginning. Available on the moon are lunar regolith as raw material and the sun as an energy source. One of the first steps towards the establishment of a lunar base is the creation of infrastructure elements, such as roads and landing pads.
We’ll introduce you to the ESA-project PAVER that demonstrates the sintering and melting of lunar regolith simulant material to produce large scale 3D printed elements that could be used during human and robotic lunar explorations.
Additive manufacturing methods such as laser powder bed fusion (LPBF) allow geometrically complex parts to be manufactured within a single step. However, as an aftereffect of the localized heat input, the rapid cooling rates are the origin of the large residual stress (RS) retained in as-manufactured parts. With a view on the microstructure, the rapid directional cooling leads to a cellular solidification mode which is accompanied by columnar grown grains possessing crystallographic texture. The solidification conditions can be controlled by the processing parameters and the scanning strategy. Thus, the process allows one to tailor the microstructure and the texture to the specific needs. Yet, such microstructures are not only the origin of the mechanical anisotropy but also pose metrological challenges for the diffraction-based RS determination. In that context the micromechanical elastic anisotropy plays an important role: it translates the measured microscopic strain to macroscopic stress. Therefore, it is of uttermost importance to understand the influence of the hierarchical microstructures and the texture on the elastic anisotropy of LPBF manufactured materials.
This study reveals the influence of the build orientation and the texture on the micro-mechanical anisotropy of as-built Inconel 718. Through variations of the build orientation and the scanning strategy, we manufactured specimens possessing [001]/[011]-, [001]-, and [011]/[111]-type textures. The resulting microstructures lead to differences in the macroscopic mechanical properties. Even further, tensile in-situ loading experiments during neutron diffraction measurements along the different texture components revealed differences in the microstrain response of multiple crystal lattice planes. In particular, the load partitioning and the residual strain accumulation among the [011]/[111] textured specimen displayed distinct differences measured up to a macroscopic strain of 10 %. However, the behavior of the specimens possessing [001]/[011]-and [001]-type texture was only minorly affected. The consequences on the metrology of RS analysis by diffraction-based methods are discussed.
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.
Präsentation der Aktivitäten an der BAM im Bereich Additive Fertigung unter Mikrogravitationsbedingungen für Anwendungen im Weltraum beim Arbeitsgruppentreffen der AG Werkstoffe & Prozesse vom Netzwerk Space2Motion.
A main source of current challenges in materials science and engineering is the ever-increasing complexity in materials chemistry and processing resulting in complex microstructures, making the assessment of process-microstructure-property-performance relations difficult, even unmanageable. Here the computational materials science is facing the same situation. In this talk, I share a viewpoint that the complexities in chemistry, processing and microstructures can be circumscribed by integrating existing knowledges of bulk thermodynamics and kinetics to the unknown thermodynamics and kinetics of microstructure elements. To this end, I discuss several successful examples on grain boundary segregation engineering how this scientific advance can be conducted. A roadmap is proposed, beginning to form on generalizing the concept of phase diagrams.