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Organisationseinheit der BAM
- 5 Werkstofftechnik (781)
- 5.2 Metallische Hochtemperaturwerkstoffe (211)
- 5.1 Mikrostruktur Design und Degradation (205)
- 5.4 Multimateriale Fertigungsprozesse (157)
- 5.6 Glas (107)
- 5.3 Polymere Verbundwerkstoffe (95)
- 5.5 Materialmodellierung (71)
- 8 Zerstörungsfreie Prüfung (71)
- 7 Bauwerkssicherheit (61)
- 9 Komponentensicherheit (60)
The materials mechanical testing ontology (MTO) was developed by collecting the mechanical testing vocabulary from ISO 23718 standard, as well as the standardized testing processes described for various mechanical testing of materials like tensile testing, Brinell hardness test, Vickers hardness test, stress relaxation test, and fatigue testing. Confirming the ISO/IEC 21838-2 standard, MTO utilizes the Basic Formal Ontology (BFO), Common Core Ontology (CCO), Industrial Ontologies Foundry (IOF), Quantities, Units, Dimensions, and data Types ontologies (QUDT), and Material Science and Engineering Ontology (MSEO) as the upper-level ontologies. Reusing these upper-level ontologies and materials testing standards not only makes MTO highly interoperable with other ontologies but also ensures its acceptance and applicability in the industry. MTO represents the mechanical testing entities in the 230 classes and four main parts: i) Mechanical testing experiments entities like tensile, hardness, creep, and fatigue tests as the subclasses of mseo:Experiment, ii) Mechanical testing quantity concepts such as toughness, elongation, and fatigue strength in the appropriate hierarchies of bfo:Disposition and bfo:Quality classes, iii) Mechanical testing artifacts like indenter as the subclasses of cco:Artifact, and iv) mechanical testing data like the stress-strain, S-N, or creep curves as the subclasses of cco:InformationContentEntity. MTO is publicly available via the KupferDigital GitLab repository.
Nickel-based alloys have been widely used for gas turbine blades owing to their excellent mechanical properties and corrosion resistance at high temperatures. The operating temperatures of modern gas turbines have been increased in pursuit of increased thermal efficiency. Turbine blades are exposed to these high temperatures combined with mechanical stresses, resulting in material damage through creep, fatigue, and other mechanisms. These turbine blades must be regularly inspected and replaced as needed, to prevent the loss of efficiency, breakdown, and catastrophic failure. Repair of the damaged turbine blades is often a more practical and cost-effective option than replacement, as replacement is associated with high costs and loss of material resources. To this end, state-of-the-art repair technologies including different additive manufacturing and brazing processes are considered to ensure efficient repair and optimum properties of repaired components.
In any repaired part, materials property-mismatches and/or inner defects may facilitate the crack initiation and propagation and thus reduce the number of load cycles to failure. Therefore, a fundamental understanding of the fatigue crack growth and fracture mechanisms in joining zones is required to enable the prediction of the remaining life of repaired components and to further improve and adapt the repair technologies.
Fatigue crack growth experiments have been conducted on SEN (Single Edge Notch) specimens joined via brazing, and pre-sintered Preform (PSP) and multi-materials (casted/printed) specimens layered via additive manufacturing (AM). The experiments were performed at 950 °C and various stress ratios. The crack growth was measured using DCPD (Direct Current Potential Drop) method. The stress intensity factors for joined SEN specimens were calculated using the finite element method and then used to derive the fatigue crack growth curves. Metallographic and fractographic analyses were conducted to get insight into the fracture mechanism.
Results show that the experimental technique for fatigue crack growth was successfully adapted and applied for testing joined specimens. Furthermore, the initial tests indicate that the investigated braze filler material provides a lower resistance to crack growth, and bonding defects cause a crack to deviate to the interface of the base material and joining zone. In AM-sandwich specimens, the crack growth rates are significantly reduced when the crack reaches the interface of printed material and casted material. The obtained crack growth data can be used to calibrate a crack growth model, which will further be utilized to predict the remaining life of repaired components.
Experimentally informed multiscale creep modelling of additive manufactured Ni-based superalloys
(2023)
Excellent creep resistance at elevated temperatures, i.e. T / T_m> 0.5, due to γ-γ’ microstructure is one of the main properties of nickel-based superalloys. Due to its great importance for industrial applications, a remarkable amount of research has been devoted to understanding the underlying deformation mechanism in a wide spectrum of temperature and loading conditions. Additive manufactured (AM) nickel-based superalloys while being governed by similar γ-γ’ microstructure, exhibit AM-process specific microstructural characteristics, such as columnar grains, strong crystallographic texture (typically <001> fiber texture parallel to build direction) and compositional inhomogeneity, which in turn leads to anisotropic creep response in both stationary and tertiary phases.
Despite the deep insights achieved recently on the correlation between process parameters and the resulting microstructure, the anisotropic creep behavior and corresponding deformation mechanism of these materials are insufficiently understood so far. One reason for this is the lack of capable material models that can link the microstructure to the mechanical behavior. To overcome this challenge, a multiscale microstructure-based approach has been applied by coupling crystal plasticity (CP) and polycrystal model which enables the inclusion of different deformation mechanisms and microstructural characteristics such as crystallographic texture and grain morphology. The method has been applied to experimental data for AM-manufactured INCONEL-738LC (IN738). The effect of different slip systems, texture, and morphology on creep anisotropy at 850°C has been investigated. Results suggest a strong correlation between superlattice extrinsic stacking fault (SESF) and microtwinning and observed creep anisotropy.
1. Introduction
A normally unwanted process that can arise when converging an electron beam onto, e.g. microparticles, has been called "damage induced by electric field" (DIEF) [1]. By DIEF, the convergent electron beam (CEB) imparts a high amount of energy to the microparticle locally and strongly interacts with its atoms. At a specific current density J, which can be controlled by the convergence angle α, the irradiated material begins to transform. The phenomenon of expelling nanomaterial from microparticles under the influence of a convergent electron beam (CB) in a transmission electron microscope (TEM) has been largely studied [2]. Several types of nanoparticles (NPs) have been observed for different metallic materials and metal oxides after specific CB protocols (P) in the TEM. Thus, DIEF can be used as a promising synthesis method controlled changes of micrometric material to create new nanometric material compositions and morphologies.
While these reactions have been observed in situ at the high acceleration voltages associated with TEM, it remains unclear whether the SEM can also be used to fabricate NPs via DIEF. In contrast to TEM there is no possibility to statically convert the electron beam to a range of α to reach the needed J as in TEM. Instead, the scanning parameters and the magnification can be manipulated so as to find an integrated J. Considering that the scanning electron microscope (SEM) is easier to use, more accessible and cheaper than a TEM, here we explore the possibility to transfer the concepts of DIEF known to operate in the TEM for in situ NP generation SEM.
2. Objectives
The main goal is to determine whether DIEF can be translated to the SEM perform to controlled in situ fabrication of nanoparticles from microparticles, using gold microparticles on amorphous SiO substrate as precursors. We determine what experimental parameters must be taken into account to create SEM-based CBPs for NP creation in the SEM with these materials.
3. Materials & methods
Gold microparticles with diameter of around 1 to 3 µm were deposited on electron transparent amorphous SiO/SiO2 substrate. Using a convergent electron beam protocol (CBP) in a scanning electron microscope (SEM) at an acceleration voltage of 30 kV, the gold microparticles were irradiated until a production of NPs takes place as shown in figure 1. The beam current varied between 16 and 23 nA.
4. Results
Depending on the CBP parameters, either only Au NPs or a mixture of Au and Si NPs are produced. The particle size ranges from a few nm up to 100 nm, and it depends on the distance of the NP to the initial position of the microparticle. Further beam parameters such as the dwell time, the effective irradiated volume and particle size determine whether NPs are produced or if the microparticles only are expelled from the substrate without reacting.
5. Conclusion
The SEM can be used as an instrument for synthesizing nanomaterials via DIEF. Different CBP protocols can be applied for obtaining either gold nanoparticles or silicon + gold nanoparticles
The phenomenon of expelling nanomaterial from microparticles of different materials, such as Au, WO3 or B2O3 under the influence of a convergent electron beam (CB) of a transmission electron microscope (TEM) was reviewed by Ignacio Gonzalez-Martinez [1]. Converging the e-beam in a TEM means that a high amount of energy enters the microparticle at a very local place and interact with the matter. Obviously, during the convergent beam protocol, no imaging with the electron beam is possible, but at the end, nanoparticles with different appearances lie down next to the microparticle while its size is reduced.
Hence, there is a blind spot in the observation, which we want to fill, as we want to help clarify the nature of the expelling phenomenon. One hypothesis that explains the phenomenon is the so-called damage (of the microparticle) induced by an electric field (DIEF). Within this theory, the material is ionized and expelled in form of ionic waves. Our aim is therefore to fabricate specimens with artificial microlandscapes, as schematically exemplified in figure 1a), using the focused ion beam (FIB) and micromanipulators, as experimental setups to follow the paths of the expelled material.
As a first step towards the fabrication of such specimen, we make experimental feasibility studies for each fabrication method, FIB structuring with Ga+ ion beam and micromanipulated microparticle deposition. Bridges (gray regions in Fig. 1) are created by milling a commercially available electron transparent membrane (silicon oxide or carbon) of a Cu-TEM grid. Platinum or carbon walls (blue features in Fig. 1) are built to stand on those bridges. Microparticles (yellow sphere in Fig. 1) of gold or other material are deposited in the center of the bridges.
Figure 2a) shows four square holes (black area) and between them the residual silicon oxide membrane bridges (dark grey). On top of the bridges, walls (light grey) are deposited. The width of the bridges is different, the walls overlap the holes as well as the distance between the walls is very small, so these and other parameters need to be optimized. Figure 2b) shows a square hole (black) with bridges (white) on the right side on top of a carbon membrane (grey). There are still some obstacles which needs to be eliminated. For instance, the deposition process of the walls is not reliable as visible at the wall on top where a hole arises instead of a wall.
These studies are still in progress and the results are further discussed in terms of the applicability for the DIEF experiment in the TEM.
Recent advances in Deep Learning (DL) have significantly impacted the field of materials modelling. DL tools have been recently considered as promising tools to address the complex relationships among processing, microstructure and property of materials. The thermal stability of polycrystalline materials is a highly interesting and complex problem that could be addressed using DL techniques. The Multi-Phase-Field (MPF) method has emerged as a powerful tool for addressing grain growth phenomena from multiple perspectives. Unlike sharp-interface based methods, the MPF approach bypasses the need for detailed information on individual grains. In this work, we use DL to address issues related to MPF simulations of grain growth including numerical efficiency, computing speed, and resource consumption. This presents specific challenges for high-performance computing (HPC) due to the large datasets and complex computations required by both MPF and DL methods. We study various 3D microstructure settings with the goal of accelerating the simulation process while exploring different physical effects. In particular, the impact of grain boundary and triple junction energies on grain growth are to be investigated. The results will be presented in terms of the evolving size and shape distribution of the grains.
Many metallic materials gain better mechanical properties through controlled heat treatments. For example, in age-hardenable aluminium alloys, the strengthening mechanism is based on the controlled formation of nanometre-sized precipitates, which represent obstacles to dislocation movement and consequently increase the strength. Precise tuning of the material microstructure is thus crucial for optimal mechanical behaviour under service condition of a component. Therefore, analysis of the microstructure, especially the precipitates, is essential to determine the optimum parameters for the interplay of material and heat treatment. Transmission electron microscopy (TEM) is utilized to identify precipitate types and orientations in the first step. Dark-field imaging (DF-TEM) is often used to image the precipitates and thereafter quantify their relevant dimensions. Often, these evaluations are still performed by manual image analysis, which is very time-consuming and to some extent also poses reproducibility problems.
Our work aims at a semantic representation of an automatable digital approach for this material specific characterization method under adaption of FAIR data practices. Based on DF-TEM images of different precipitation states of a wrought aluminium alloy, the modularizable, digital workflow of quantitative analysis of precipitate dimensions is described. The integration of this workflow into a data pipeline concept will also be discussed. Using ontologies, the raw image data, their respective contextual information, and the resulting output data of the quantitative image analysis can be linked in a triplestore. Publishing the digital workflow and the ontologies will ensure data reproducibility. In addition, the semantic structure enables data sharing and reuse for other applications and purposes, demonstrating interoperability.
We report about a joint project aiming at the digitalization of a lab course in materials testing. The undergraduate students were asked to prepare samples of a precipitation hardened aluminum alloy and characterize them using hardness and tensile tests. In a first step, we developed the frames for the digital labor notebook using eLabFTW. The primary data and the relevant metadata of each run were saved in a central database and made available for analysis and report issues. The whole set of results produced in a course was made available in the database. This database can be improved and serve as an open repository for data on this specific alloy.
The logical frame for the joint project was provided by the PMD Core Ontology (PMDco), a mid-level ontology that enables the representation and description of processes and process chains in an MSE-specific manner, ensuring full traceability of generated data. For the digitalization of this lab course, the tensile test ontology (TTO) was applied which is designed as a module of the PMDco using strongly related semantic concepts.
Many microstructural features exhibit non-trivial geometries, which can only be derived to a limited extent from two-dimensional images. E.g., graphite arrangements in lamellar gray cast iron have complex geometries, and the same is true for additively manufactured materials and three-dimensional conductive path structures. Some can be visualized using tomographic methods, but some cannot be due to weak contrast and/or lack of resolution when analyzing macroscopic objects. Classic metallography can help but must be expanded to the third dimension. The method of reconstructing three-dimensional structures from serial metallographic sections surely is not new. However, the effort required to manually assemble many individual sections into image stacks is very high and stands in the way of frequent application. For this reason, an automated, robot-supported 3D metallography system is being developed at BAM, which carries out the steps of repeated preparation and image acquisition on polished specimen.
Preparation includes grinding, polishing and optionally etching of the polished surface. Image acquisition comprises autofocused light microscopic imaging at several magnification levels. The image stacks obtained are then pre-processed, segmented, and converted into 3D models, which in the result appear like microtomographic models, but with high resolution at large volume. Contrasting by classical chemical etching reveals structures that cannot be resolved using tomographic methods. The integration of further imaging and measuring methods into this system is underway. Some examples will be discussed in the presentation.
Knowledge representation in the materials science and engineering (MSE) domain is a vast and multi-faceted challenge: Overlap, ambiguity, and inconsistency in terminology are common. Invariant and variant knowledge are difficult to align cross-domain. Generic top-level semantic terminology often is too abstract, while MSE domain terminology often is too specific.
In this presentation, an approach how to maintain a comprehensive and intuitive MSE-centric terminology composing a mid-level ontology–the PMD core ontology (PMDco)–via MSE community-based curation procedures is shown.
The PMDco is designed in direct support of the FAIR principles to address immediate needs of the global experts community and their requirements. The illustrated findings show how the PMDco bridges semantic gaps between high-level, MSE-specific, and other science domain semantics, how the PMDco lowers development and integration thresholds, and how to fuel it from real-world data sources ranging from manually conducted experiments and simulations as well as continuously automated industrial applications.
The surface corrosion behaviour is a key issue which determines whether the material is applicable at a given atmosphere. Medium-entropy alloy FeCrNi alloy was exposed to synthetic air at 1000°C, 1050°C, and 1100 °C for up to 1000 h using a thermobalance. The oxidation rate was parabolic at 1000 and 1050°C, but breakaway occurred at 1100°C after 5 h of aging time. The whole oxide scales formed under the isothermal oxidation tests spalled off and additional oxidation tests were carried out at 1000 °C and 1050°C for 24 h and up to 100 h at 1000°C in a tubular furnace. The corrosion behaviour of the MEA was analysed by scanning electron microscope, energy-dispersive X-ray spectroscopy, and X-ray diffraction and compared to the behaviour of 316 L. The experimental results showed that under all conditions chromium is the main diffusion element resulting in the formation of a Cr2O3 layer at the MEA surface. Spallation of the layer induces the formation of additional oxidation products under the surface of the (spalled off) chromia layer.
The PMD Core Ontology (PMDco) is a comprehensive set of building blocks produced via consensus building. The ontological building blocks provide a framework representing knowledge about fundamental concepts used in Materials Science and Engineering (MSE) today. The PMDco is a mid-level ontology that establishes connections between narrower MSE application ontologies and domain neutral concepts used in already established broader (top-level) ontologies. The primary goal of the PMDco design is to enable interoperability between various other MSE-related ontologies and other common ontologies.
PMDco’s class structure is both comprehensive and extensible, rendering it an efficient tool to structure MSE knowledge. The PMDco serves as a semantic middle-layer unifying common MSE concepts via semantic mapping to other semantic representations using well-known key terms used in the MSE domain. The PMDco enables straight-forward documentation and tracking of science data generation and in consequence enables high-quality FAIR data that allows for precise reproducibility of scientific experiments.
The design of PMDco is based on the W3C Provenance Ontology (PROV-O), which provides a standard framework for capturing the production, derivation, and attribution of resources. Via this foundation, the PMDco enables the integration of data from various data origins and the representation of complex workflows.
In summary, the PMDco is a valuable advancement for researchers and practitioners in MSE domains. It provides a common MSE vocabulary to represent and share knowledge, allowing for efficient collaboration and promoting interoperability between diverse domains. Its design allows for the systematic integration of data and metadata, enabling seamless tracing of science data. Overall, the PMDco is a crucial step towards a unified and comprehensive understanding of the MSE domain in general.
Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material which exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). The linear thermal expansion coefficient of ZrV2O7 is −7.1×10-6 K-. Therefore, it can be used to create composites with controllable expansion coefficients and prevent destruction by thermal shock.
Material characterization, leading to application, requires pure, homogenous samples of high crystallinity via a reliable synthesis route. While there is a selection of described syntheses in the literature, it still needs to be addressed which synthesis route leads to truly pure and homogenous samples. Here, we study the influence of the synthesis methods (solid-state, sol-gel, solvothermal) and their parameters on the sample's purity, crystallinity, and homogeneity. The reproducibility of results and data obtained with scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimetry, and thermogravimetric analysis (DSC/TGA) were analyzed extensively. The sol-gel method proves superior to the solid-state method and produces higher-quality samples over varying parameters. Sample purity also plays an important role in NTE micro and macro-scale characterizations that explain the impact of porosity versus structural changes.
Moreover, we implement ab-initio-based vibrational computations with partially treated anharmonicity (quasi-harmonic approximation, temperature-dependent effective harmonic potentials) in combination with experimental methods to follow and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder, microstructure, and defects. Khosrovani et al. and Korthuis et al., in a series of diffraction experiments, attributed the thermal contraction of ZrV2O7 to the transverse thermal motion of oxygen atoms in V-O-V linkages. In addition to previous explanations, we hypothesize that local disorder develops in ZrV2O7 crystals during heating.
We are working on the experimental ZrV2O7 development and discuss difficulties one might face in the process as well as high-quality sample significance in further investigation. The obtained samples are currently used in the ongoing research of structure analysis and the negative thermal expansion mechanism.
Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material which exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). The linear thermal expansion coefficient of ZrV2O7 is −7.1×10-6 K-. Therefore, it can be used to create composites with controllable expansion coefficients and prevent destruction by thermal shock.
Material characterization, leading to application, requires pure, homogenous samples of high crystallinity via a reliable synthesis route. While there is a selection of described syntheses in the literature, it still needs to be addressed which synthesis route leads to truly pure and homogenous samples. Here, we study the influence of the synthesis methods (solid-state, sol-gel, solvothermal) and their parameters on the sample's purity, crystallinity, and homogeneity. The reproducibility of results and data obtained with scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimetry, and thermogravimetric analysis (DSC/TGA) were analyzed extensively. The sol-gel method proves superior to the solid-state method and produces higher-quality samples over varying parameters. Sample purity also plays an important role in NTE micro and macro-scale characterizations that explain the impact of porosity versus structural changes.
Moreover, we implement ab-initio-based vibrational computations with partially treated anharmonicity (quasi-harmonic approximation, temperature-dependent effective harmonic potentials) in combination with experimental methods to follow and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder, microstructure, and defects. Khosrovani et al. and Korthuis et al., in a series of diffraction experiments, attributed the thermal contraction of ZrV2O7 to the transverse thermal motion of oxygen atoms in V-O-V linkages. In addition to previous explanations, we hypothesize that local disorder develops in ZrV2O7 crystals during heating.
We are working on the experimental ZrV2O7 development and discuss difficulties one might face in the process as well as high-quality sample significance in further investigation. The obtained samples are currently used in the ongoing research of structure analysis and the negative thermal expansion mechanism.
Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material which exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). The linear thermal expansion coefficient of ZrV2O7 is −7.1×10-6 K-1. Therefore, it can be used to create composites with controllable expansion coefficients and prevent destruction by thermal shock.
Material characterization, leading to application, requires pure, homogenous samples of high crystallinity via a reliable synthesis route. While there is a selection of described syntheses in the literature, it still needs to be addressed which synthesis route leads to truly pure and homogenous samples. Here, we study the influence of the synthesis methods (solid-state, sol-gel, solvothermal) and their parameters on the sample's purity, crystallinity, and homogeneity. The reproducibility of results and data obtained with scanning electron microscopy (SEM), X-ray diffraction (XRD), differential scanning calorimetry, and thermogravimetric analysis (DSC/TGA) were analyzed extensively. The sol-gel method proves superior to the solid-state method and produces higher-quality samples over varying parameters. Sample purity also plays an important role in NTE micro and macro-scale characterizations that explain the impact of porosity versus structural changes.
Moreover, we implement ab-initio-based vibrational computations with partially treated anharmonicity (quasi-harmonic approximation, temperature-dependent effective harmonic potentials) in combination with experimental methods to follow and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder, microstructure, and defects. Khosrovani et al. and Korthuis et al., in a series of diffraction experiments, attributed the thermal contraction of ZrV2O7 to the transverse thermal motion of oxygen atoms in V-O-V linkages. In addition to previous explanations, we hypothesize that local disorder develops in ZrV2O7 crystals during heating.
We are working on the experimental ZrV2O7 development and discuss difficulties one might face in the process as well as high-quality sample significance in further investigation. The obtained samples are currently used in the ongoing research of structure analysis and the negative thermal expansion mechanism.
This research deals with the development of the Vickers hardness knowledge graph, mapping the example dataset in them, and exporting the data-mapped knowledge graph as a machine-readable Resource Description Framework (RDF). Modeling the knowledge graph according to the standardized test procedure and using the appropriate upper-level ontologies were taken into consideration to develop the highly standardized, incorporable, and industrial applicable models. Furthermore, the Ontopanel approach was utilized for mapping the real experimental data in the developed knowledge graphs and the resulting RDF files were successfully evaluated through the SPARQL queries.
Low-temperature co-fired ceramics (LTCC) are used to fabricate multilayer circuits which are robust in harsh environments. Thick-film technology is well established for the metallization of circuit boards and microsystems. For specific sensor applications, the combination of LTCC and thin-film technology is advantageous to reach higher structure resolutions. Due to the high roughness of as-fired LTCC surfaces compared with silicon-wafers, the deposition of low-defect- films with narrowly specified properties is challenging. The 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. There is spare literature about thin films on commercial LTCC comparing different material systems or sintering techniques. For developing thin-film sensors on multilayer circuits it is crucial to identify thin-film-compatible commercial LTCC material as well as the crucial surface properties. In this work we evaluate the thin-film capability of different LTCC compositions and surface qualities.
To evaluate the influence of the material composition on the thin film capability, 200 nm Ni-thin films were deposited on three different constrained-sintered LTCC (CT708, CT800 and DP951) by electron beam physical vapour deposition. The effect of surface quality was assessed by thin-film deposition on free-sintered, pressure-assisted sintered, and polished DP951. The thin-films were structured by covering corresponding sections with a UV-curable photo resin and subsequent etching of the uncovered surface, leaving behind the desired structure.
The etched Ni-thin films showed high difference in failure rate and sheet resistance regarding the used LTCC-material. DP951 had the lowest sheet resistance and no failure, whereas CT800 had a high sheet resistance and a failure rate of 40 %. These results are correlated with surface roughness of the LTCC, scanning electron micrographs of the deposited thin-films, and the chemical resistance of the LTCC against commonly used etching media. Contrary to the expectations, no correlation between roughness and thin-film capability was found. The LTCC with high failure rate showed a strong chemical attack by the used etching medium. Additionally, the adhesion of thin-films on DP951 is better than on CT708 and CT800.
Grain boundary (GB) chemical and structural variations can significantly influence materials performance. The former is generally ascribed to the structural gradient between the grain and GB. While GB segregation may be accompanied by chemical and structural variations, clear insights about the GB’s thermodynamic phase behaviour upon coupling between its chemistry and structure is lacking. Using the CALPHAD integrated density-based phase field model, we study the co-evolution of GB’s structure and segregation in Fe-Mn alloys. We found that the GB segregation transition is amplified if its structure can respond to chemical variation. Additionally, the coupling between GB structural and segregation evolution was found to enable co-existence of the spinodally formed low- and high-Mn phases within the GB. In the light of atomistic simulations, we expand on investigating the correlation between the parameters that characterise the GB density map with GB properties.
Several recent studies have revealed that the phase decomposition in medium- and high-entropy alloys is triggered by solute segregation at grain boundaries. The chemically complex nature of these alloys already clues that such segregation in materials should be something more than the interaction between solutes and grain boundary, but also affected by the solute-solute interactions during the segregation. In fact, experiments indicate the significance of such solute-solute interaction. Yet, the mechanisms of co-segregation in multi-component alloys are rather challenging to explore and rarely studied quantitatively. Recently, a CALPHAD-integrated density-based phase-field model has been proposed for studying grain boundary phenomena. Several applications of this model have shown its expansive capacity for investigating grain boundary segregation and phase behavior. In this talk, the applications of this model to studying co-segregation phenomena and grain boundary phase diagrams in multi-component alloys are presented ––the term ‘co-segregation’ here refers to co-evolution and any mutual interplay among the solutes and grain boundary during the segregation. In particular, the iron-based ternary and quaternary alloys are discussed. I show how a grain boundary may have its own miscibility gap and how this immiscibility can influence the co-segregation behavior. As an alternative to grain boundary phase diagrams, rather suited for binary and ternary alloys, a new concept of co-segregation maps for screening and segregation design in multi-component alloys is presented. Applying the co-segregation maps, the nonlinear Mn and Cr co-segregation in Fe-Co-Mn-Cr is discussed.
Tensile Test Ontology (TTO)
(2023)
This is the stable version 2.0.1 of the PMD ontology module of the tensile test (Tensile Test Ontology - TTO) as developed on the basis of the 2019 standard ISO 6892-1: Metallic materials - Tensile Testing - Part 1: Method of test at room temperature.
The TTO was developed in the frame of the PMD project. The TTO provides conceptualizations valid for the description of tensile test and corresponding data in accordance with the respective standard. By using TTO for storing tensile test data, all data will be well structured and based on a common vocabulary agreed on by an expert group (generation of FAIR data) which will lead to enhanced data interoperability. This comprises several data categories such as primary data, secondary data and metadata. Data will be human and machine readable. The usage of TTO facilitates data retrieval and downstream usage. Due to a close connection to the mid-level PMD core ontology (PMDco), the interoperability of tensile test data is enhanced and data querying in combination with other aspects and data within the broad field of material science and engineering (MSE) is facilitated.
The TTO class structure forms a comprehensible and semantic layer for unified storage of data generated in a tensile test including the possibility to record data from analysis, re-evaluation and re-use. Furthermore, extensive metadata allows to assess data quality and reproduce experiments. Following the open world assumption, object properties are deliberately low restrictive and sparse.
Wind turbine rotor blades are produced as aerodynamic, three-dimensionally formed sandwich shell structures using mainly glass fiber reinforced plastics (GFRP). The GFRP used today have the potential to withstand the harsh operating conditions of rotor blades over the projected service life of 20 years. Premature damages that occur can be traced primarily back to design and/or manufacturing imperfections, as well as unusually high load scenarios (for instance lightning strikes, or strong winds combined with system control errors). Therefore, rotor blades have to be repaired several times (on average 2-3 times) during their projected service life. Approximately 70% of these are repairs of small- to medium-sized sandwich shells, carried out by technicians directly accessing the blade by suspended roping at the wind turbine location. The goal is to execute repairs that will last over the remaining service life, i.e. be sustainable.
Within the framework of a research project carried out at BAM, Division 5.3 Polymer Matrix Composites, Department 5 for Materials Engineering, not only was the geometric shape (round vs. square in relation to the top view) varied, but also the layup of the scarf repair structure, variables that have not been studied systematically to-date. Sub-component scale sandwich shell specimens with representative repairs were used in this work in addition to coupon-scale specimens that are more commonly seen in literature. These sub-component shell specimens were tested using a unique shell test bench under loading conditions representative of wind turbine blade shell operating conditions with respect to fatigue strength. Using non-destructive testing methods (field strain measurement and thermography), damage development and distribution was monitored and analyzed in-situ. As a result, a concept was developed in which the repaired areas showed at least equivalent if not higher fatigue strength than the reference shells that were not repaired.
Une transition mondiale vers des systèmes énergétiques plus durables, abordables et fiables a été initiée par l’accord de Paris et l’Agenda 2030 des Nations unies pour un développement durable. Il s’agit là d’un défi industriel majeur car les systèmes et infrastructures énergétiques résilients au changement climatique exigent de se positionner pour le long terme. Se pencher sur le comportement dans la durée des matériaux structurels - principalement des métaux et des alliages - s’impose alors comme une nécessité. Dans cette optique, « La corrosion : un défi pour une société durable »présente une série de cas montrant l’importance de la tenue à la corrosion et de la protection anticorrosion des métaux et des alliages pour le développement de systèmes durables, économiques et fiables de production d’énergie.
In our current view, 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) aims to develop 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 the creation and distribution of 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.
In our current view, 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) aims to develop 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 the creation and distribution of 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 hohen Betriebstemperaturen während des Einsatzes von Radialverdichterrädern in Abgasturboladern führen zu einer Änderung der ursprünglich eingestellten Mikrostruktur in der warmfesten Aluminiumlegierung EN AW-2618A (Überalterung). Grund dafür sind thermische Belastungen, die nahe der Aushärtetemperatur liegen und diese kurzzeitig sogar überschreiten können. Die Alterungsmechanismen wurden zusammen mit den Themen niederzyklische (LCF) und thermomechanische Ermüdung (TMF) sowie Kriechen bis max. 190 °C in vorangegangenen Forschungsvorhaben untersucht. Kaum untersucht war bisher das Verhalten der Legierung unter hochzyklischer Beanspruchung (HCF) sowie der Einfluss von Kerben und Lastkollektiven. Da zukünftig mit weiter steigenden Betriebstemperaturen für Radialverdichter zu rechnen ist, wurde in diesem Forschungsvorhaben das HCF-Verhalten bei 230 °C untersucht und somit bei einer Prüftemperatur, die deutlich oberhalb der Aushärtetemperatur liegt. Das Ziel des Projektes war der Aufbau einer geeigneten experimentellen Datenbasis, das Verständnis der relevanten mikrostrukturellen Prozesse sowie die Weiterentwicklung und Anpassung geeigneter Modelle und Bewertungsmethoden.
Das experimentelle Untersuchungsprogramm umfasste neben einer Basischarakterisierung des HCF-Verhaltens am Ausgangszustand T61 gezielte mechanische Versuche zur Isolierung der Einflussfakto-ren Mittelspannung (𝑅 = −1, 𝑅 = 0,1), Werkstoffüberalterung (T61, 10 h/230 °C, 1000 h/230 °C), Prüftemperatur (20 °C, 230 °C), Prüffrequenz (0,2 Hz, 20 Hz) sowie Kerbwirkung und variable Amplituden. Darauf aufbauend wurden die in den vorangegangenen Projekten entwickelten Modelle und Bewertungsmethoden angepasst und weiterentwickelt, um die genannten thermischen und mechanischen Belastungen in der Lebensdauerbewertung abzubilden.
The essence of dynamic failure is closely linked to the formation of adiabatic shear bands (ASB), which result from the localization of shear strain under high deformation speeds accompanied by a rapid temperature increase. Understanding this phenomenon is crucial in view of safety issues when impacts of fast rotating machine components (i.e. aircraft turbine blades) may occur. Our contribution addresses both the experimental evidence and characterization of ASBs due to high-speed impact tests at the Split HOPKINSON pressure bar (SHPB) setup and the finite element analysis to determine the parameters of the underlying constitutive model, which is closely related to JOHNSON-COOK (JC) material model.
Experimental investigations were performed on notched shear specimens made of the fine -grained structural steel S690QL and the displacements in the regions affected by shear localization were measured with subset-based local Digital Image Correlation (DIC). The displacement fields, obtained in the SHPB tests, were considered as an objective to validate and to identify the constitutive parameters with. The JC model could reasonably reproduce the displacement distribution. In order to overcome the issues with mesh dependency we provide a nonlocal extension based on the implicit gradient model approach.
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 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.
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.
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.