TY - CONF A1 - Winckelmann, Alexander T1 - Investigation of degradation of the aluminum current collector in lithium-ion batteries by glow-discharge optical emission spectroscopy N2 - 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. T2 - European Winter Conference on Plasma Spectrochemistry (EWCPS 2023) CY - Ljubljana, Slovenia DA - 29.01.2023 KW - Lithium-ion batteries KW - Aging mechanisms KW - Depth-profiling PY - 2023 AN - OPUS4-56992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Investigation of degradation of the aluminum current collector in lithium-ion batteries by GD-OES N2 - 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. T2 - Empa Group Meeting CY - Dübendorf, Switzerland DA - 22.11.2022 KW - Lithium Ion Batteries KW - GD-OES KW - FIB KW - SEM KW - EDX PY - 2022 AN - OPUS4-56584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Channammagari, Harichandana A1 - Sahr, Rabea A1 - Trappe, Volker T1 - Experimentelle, Analytisch-Numerische Untersuchung des thermischen Ausdehnungsverhaltens von Faser-Kunststoff-Verbunden N2 - Im Rahmen des Forschungsvorhabens PROVING wurde eine Methode zur rechnerischen Bestimmung thermomechanischer Eigenspannungen in CFK entwickelt. Ziel ist die Berücksichtigung des thermischen Ausdehnungsverhaltens bei der Bestimmung des dreidimensionalen in-situ-Spannungszustands der Matrix für den strukturellen Nachweis. Die Eigenspannungen werden über mikromechanische Modellierung und FEM berechnet; die zugrunde liegenden Ausdehnungsfunktionen wurden experimentell validiert. N2 - As part of the PROVING research project, a method for calculating thermomechanical residual stresses in CFRP was developed. The aim is to take thermal expansion behavior into account when determining the three-dimensional in-situ stress state of the matrix for structural verification. The residual stresses are calculated using micromechanical modeling and FEM; the underlying expansion functions have been experimentally validated. T2 - 43. Vortrags- und Diskussionstagung Werkstoffprüfung 2025 CY - Dresden, Germany DA - 27.11.2025 KW - Thermische Eigenspannungen KW - Mikromechanik KW - Faser-Kunststoff-Verbunde KW - FEM PY - 2025 SN - 978-3-88355-454-9 VL - 2025 SP - 154 EP - 159 PB - DGM CY - Sankt Augustin AN - OPUS4-65112 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sahr, Rabea T1 - Experimentelle, Analytisch-Numerische Untersuchung des Thermischen Ausdehnungsverhaltens von Faser-Kunststoff-Verbunden N2 - Im Rahmen des Forschungsvorhabens PROVING wurde eine Methode zur rechnerischen Bestimmung thermomechanischer Eigenspannungen in CFK entwickelt. Ziel ist die Berücksichtigung des thermischen Ausdehnungsverhaltens bei der Bestimmung des dreidimensionalen in-situ-Spannungszustands der Matrix für den strukturellen Nachweis. Die Eigenspannungen werden über mikromechanische Modellierung und FEM berechnet; die zugrunde liegenden Ausdehnungsfunktionen wurden experimentell validiert. T2 - 43. Vortrags- und Diskussionstagung Werkstoffprüfung 2025 CY - Dresden, Germany DA - 27.11.2025 KW - Thermische Eigenspannungen KW - Mikromechanik KW - Faser-Kunststoff-Verbunde KW - FEM PY - 2025 AN - OPUS4-65118 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waurischk, Tina A1 - Deubener, J. A1 - Müller, Ralf T1 - Internal friction and energy dissipation during fracture in silicate glasses N2 - To obtain a deeper insight into the nature of energy dissipation during fracture, the internal friction of 13 borosilicate, aluminosilicate, soda-lime, and lead-containing glasses, for which inert crack growth data are known, was measured using dynamic mechanical thermal analysis. For asymmetrically bent glass beams, the loss tangent, tan δ, was determined between 0.2 and 50 Hz at temperatures between 273 K and the glass transition temperature, Tg. It was found that the area under the tan δ vs T·Tg−1 curve correlates with the crack growth exponent, n, in the empirical v = v0·KIn relation between crack growth velocity, v, and stress intensity, KI, which indicates that n correlates with the degree of energy dissipation of sub-Tg relaxation phenomena. KW - Glass KW - Internal friction KW - Crack growth PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-651371 DO - https://doi.org/10.1063/5.0255432 SN - 0021-9606 VL - 162 IS - 19 SP - 1 EP - 9 PB - AIP Publishing AN - OPUS4-65137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pan, Z. A1 - Waurischk, Tina A1 - Duval, A. A1 - Müller, Ralf A1 - Deubener, J. A1 - Krishnan, N. M. A. A1 - Wondraczek, K. A1 - Wondraczek, L. T1 - Precise Real‐Time Measurement of Liquid Viscosity Using Digital Video Data N2 - Quantitative knowledge of liquid viscosity is of fundamental importance in many areas of materials synthesis and processing. However, the determination of viscosity often relies on specialized experimental equipment, offline experimentation, or invasive procedures, in particular when required in extreme conditions such as at high temperature, high pressure, and in confined or corrosive environments. Here, this study proposes and validates a fast and simple method that mimics the intuitive perception of liquid flow within a quantitative framework. For this, this study employs digital video observation to derive quantitative values of the shear viscosity of liquids, with high precision and rapid acquisition rates. The technique involves capturing liquid dynamics after minor mechanical stimulation. Processed imaging data are indexed by similarity and referenced to a digital database generated with a finite element model, from which values of viscosity are obtained in line. The approach is tested on water at room temperature and on a high‐temperature glass melt. Covering a viscosity range of four orders of magnitude, both yield convincing agreement with tabulated reference data at low computational cost. KW - Glass KW - Liquid Viscosity KW - Digital Video Data KW - Finite Element Method PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-651363 DO - https://doi.org/10.1002/aisy.202500297 SN - 2640-4567 VL - 7 IS - 12 SP - 1 EP - 12 PB - Wiley VHC-Verlag AN - OPUS4-65136 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Channammagari, Harichandana T1 - From Micromechanics to Macro Validation: A New Approach for Aerospace Structures N2 - Given the high experimental effort required to verify fiber‑reinforced polymer composites (FRP) in aviation, the PROVING project (Production, Optimization, and Virtual Verification for Generative Manufacturing Processes) aims to establish a streamlined and robust verification methodology based on analytical and numerical approaches. As a foundation for this virtual verification process, BAM contributed extensive material testing for parameter identification, feeding directly into the material models and probabilistic methods. Beyond the experiments, an analytical‑numerical model was developed to more accurately determine the in‑situ stress state within the composite matrix. Since damage initiation in FRP is largely driven by inter-fiber failure, the three‑dimensional matrix stress state is essential for structural verification. In addition to external loading, thermomechanical residual stresses arising from the mismatched thermal expansion of fibers and matrix contribute to the stress state. Within PROVING, a calculation method was developed that incorporates the thermomechanical behavior of carbon‑fiber‑reinforced polymers (CFRP) into the verification process with minimal experimental effort. The method determines matrix thermal residual stresses using micromechanical modeling combined with finite element analysis. T2 - 29. Nationales SAMPE Symposium CY - Aachen, Germany DA - 02.04.2025 KW - Virtual Verification KW - Micromechanics KW - FEA PY - 2025 AN - OPUS4-65187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sonntag, Nadja T1 - Dwell-Fatigue and Cyclic Softening of Grade P92 Steel under LCF and TMF Conditions N2 - Tempered martensite-ferritic steels, such as the grade P92 steel studied in this contribution, exhibit pronounced macroscopic cyclic softening under isothermal low-cycle fatigue (LCF) and non-isothermal thermomechanical fatigue (TMF) conditions, which is considered to be the predominant degradation mechanism in high-temperature fatigue in this and other material groups. However, such softening processes are highly complex since microscopic (e.g., recovery) and macroscopic (e.g., crack initiation and growth), as well as global and local effects superimpose, especially under creep-fatigue conditions. In this contribution, we discuss the cyclic deformation and softening behavior of P92 in strain-controlled LCF, in-phase (IP) TMF, and out-of-phase (OP) TMF tests with and without dwell times in the temperature range from 300 °C to 620°C. EBSD-based dislocation analysis on various fatigued material states confirms the continuous redistribution and annihilation of geometrically necessary dislocations in all studied states, which can be quantitatively correlated with macroscopic softening despite different damage mechanisms for different test types. Deviations from this correlation are observed for OP TMF and LCF with dwell times, i.e., for conditions where optical microscopy reveals pronounced crack-oxidation interactions at the specimen surfaces. T2 - LCF9 - Ninth International Conference on Low Cycle Fatigue CY - Berlin, Germany DA - 21.06.2022 KW - LCF KW - TMF KW - EBSD PY - 2022 DO - https://doi.org/10.48447/LCF9-2022-111 AN - OPUS4-55128 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Viguier, B. T1 - Creep of single-crystals of nickel-base gamma-alloy at high temperatures N2 - Porosity in single-crystal nickel-base superalloys is removed by hot isostatic pressing (HIP) at temperatures above gamma’-solvus where the material is very soft and ductile. For example, single-crystal nickel-base superalloy CMSX-4 is HIPed at temperature 1288 °C, which is slightly higher than the gamma’-solvus temperature of this alloy equal to about 1280 °C. It is assumed that pore shrinking during HIP is mostly due to dislocation creep. Such a modelling of HIP of CMSX-4 was started in our group on the base of results of creep tests of [001] single-crystals at 1288 °C [1]. However, it was found later [2] that the alloy CMSX-4 shows very strong creep anisotropy at 1288 °C. Therefore, for calibration of the creep law, creep tests of different orientations under different stress levels are required at the HIP temperature. This was the main task of present work. Single-crystals of CMSX-4 of axial orientations [001], [011], [123] and [111] were cast by VIAM Moscow and tested by BAM Berlin under creep conditions at 1288 °C and stress levels between 4 MPa and 16 MPa. At all stress levels, the creep rate increases by an order of magnitude when changing the orientation from [001] to [111] with [011] and [123] orientations in between. Such a character of creep anisotropy corresponds to the orientation dependence of the Schmid factor for octahedral glide. The crystal viscoplasticity model developed in [1] was improved to better represent the time induced softening observed during creep. The creep tests for different stresses and orientations as well as pore closure were simulated. The results of pore closure simulation are compared with measurements of porosity decrease during Hiping. T2 - 15th International Conference on Creep and Fracture of Engineering Materials and Structures CY - Online meeting DA - 14.06.2021 KW - Nickel-base superalloys KW - Creep KW - Single-Crystal PY - 2021 AN - OPUS4-53935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Fedelich, Bernard ED - Cailletaud, G. ED - Cormier, J. ED - Eggeler, G. ED - Maurel, V. ED - Nazé, L. T1 - Crystal orientation and elastic properties N2 - The elastic constants are the most basic mechanical properties of a material and are needed for any structural analysis of a component. For example, they have a major influence on the eigenfrequencies of vibrating parts. Single crystals of Ni-base superalloys are strongly anisotropic, which means that the observed properties are orientation dependent. Tensor algebra is then required to mathematically formulate the elastic properties and their relations to the crystal orientation. Hence, this chapter first summarizes some basic definitions and calculation rules for Rotation matrices, including the definition of the Euler angles, which are most commonly used to define the relative orientations of the crystal and the component. Parts of this chapter closely follow the lines of the excellent exposition of the topic by Olschewski. KW - Nickel-base superalloys KW - Elasticity PY - 2022 SN - 978-0-12-819357-0 SP - 41 EP - 67 PB - Elsevier Inc. AN - OPUS4-53435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kianinejad, Kaveh A1 - Darvishi Kamachali, Reza A1 - Khedkar, Abhinav A1 - Manzoni, Anna Maria A1 - Agudo Jácome, Leonardo A1 - Schriever, Sina A1 - Saliwan Neumann, Romeo A1 - Megahed, Sandra A1 - Heinze, Christoph A1 - Kamrani, Sepideh A1 - Fedelich, Bernard T1 - Creep anisotropy of additively manufactured Inconel-738LC: Combined experiments and microstructure-based modeling N2 - The current lack of quantitative knowledge on processing-microstructure–property relationships is one of the major bottlenecks in today’s rapidly expanding field of additive manufacturing. This is centrally rooted in the nature of the processing, leading to complex microstructural features. Experimentally-guided modeling can offer reliable solutions for the safe application of additively manufactured materials. In this work, we combine a set of systematic experiments and modeling to address creep anisotropy and its correlation with microstructural characteristics in laser-based powder bed fusion (PBF-LB/M) additively manufactured Inconel-738LC (IN738LC). Three sample orientations (with the tensile axis parallel, perpendicular, and 45° tilted, relative to the building direction) are crept at 850 °C, accompanied by electron backscatter secondary diffraction (EBSD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) investigations. A crystal plasticity (CP) model for Ni-base superalloys, capable of modeling different types of slip systems, is developed and combined with various polycrystalline representative volume elements (RVEs) built on the experimental measurements. Besides our experiments, we verify our modeling framework on electron beam powder bed fusion (PBF-EB/M) additively manufactured Inconel-738LC. The results of our simulations show that while the crystallographic texture alone cannot explain the observed creep anisotropy, the superlattice extrinsic stacking faults (SESF) and related microtwinning slip systems play major roles as active deformation mechanisms. We confirm this using TEM investigations, revealing evidence of SESFs in crept specimens. We also show that the elongated grain morphology can result in higher creep rates, especially in the specimens with a tilted tensile axis. KW - Additive manufactured Ni-base superalloys KW - Creep KW - Crystal plasticity KW - Superlattice extrinsic stacking faults PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601576 DO - https://doi.org/10.1016/j.msea.2024.146690 SN - 0921-5093 VL - 907 SP - 1 EP - 16 PB - Elsevier B.V. AN - OPUS4-60157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gesell, Stephan T1 - Numerical calculation of ΔCTOD for thermomechanical fatigue crack growth N2 - The cyclic crack tip opening displacement ΔCTOD is a promising loading Parameter to quantify the crack propagation under thermomechanical fatigue (TMF). In this work, suitable techniques are investigated and compared for an accurate calculation of ΔCTOD under TMF loading using a viscoplastic temperature dependent material model. It turned out that collapsed special crack tip elements give the best results. An efficient FEM-technique is developed to simulate the incremental crack growth by successive remeshing, whereby the deformations and internal state variables are mapped from the old mesh onto the new one. The developed techniques are demonstrated and discussed for two-dimensional examples like TMF-specimens. 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. T2 - ESIS Technical Meeting on Numerical Methods (TC8) CY - Online meeting DA - 06.04.2021 KW - Crack tip opening displacement KW - Thermomechanical fatigue KW - Crack growth PY - 2021 AN - OPUS4-52410 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ganesh, Rahul A1 - Gesell, Stephan A1 - Kuna, M. A1 - Fedelich, Bernard A1 - Kiefer, B. T1 - Numerical calculation of ΔCTOD for thermomechanical fatigue crack growth N2 - The cyclic crack tip opening displacement ΔCTOD is a promising loading Parameter to quantify the crack propagation under thermomechanical fatigue (TMF). In this work, suitable techniques are investigated and compared for an accurate calculation of ΔCTOD under TMF loading using a viscoplastic temperature dependent material model. It turned out that collapsed special crack tip elements give the best results. An efficient FEM-technique is developed to simulate the incremental crack growth by successive remeshing, whereby the deformations and internal state variables are mapped from the old mesh onto the new one. The developed techniques are demonstrated and discussed for two-dimensional examples like TMF-specimens. 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. N2 - Zur Bewertung des Rissfortschritts unter thermomechanischer Ermüdung (TMF) ist die zyklische Rissöffnungsverschiebung ΔCTOD ein aussichtsreicher bruchmechanischer Beanspruchungsparameter. In dieser Arbeit werden unter Anwendung eines viskoplastischen, temperaturabhängigen Materialmodells geeignete FEM-Techniken für die akkurate Berechnung des ΔCTOD bei TMF erprobt und verglichen. Als beste Technik hat sich die Verwendung kollabierter Rissspitzenelemente erwiesen. Es wurde ein effizienter FEM-Algorithmus zur Simulation der Rissausbreitung mit inkrementeller Neuvernetzung entwickelt, bei dem die Verformungen und inelastischen Zustandsvariablen jeweils vom alten auf das neue Netz übertragen werden. Die erarbeiteten Techniken werden am Beispiel von zweidimensionalen Strukturen und TMF-Proben vorgestellt und diskutiert. Dabei werden wesentliche Kontrollparameter der Simulation wie optimale Grösse der Rissspitzenelemente, Länge des Rissinkrementes in Relation zur plastischen Zone und dem ΔCTOD-Wert empfohlen. T2 - 53. Tagung des Arbeitskreises "Bruchmechanik und Bauteilsicherheit" CY - Online meeting DA - 18.02.2021 KW - Crack tip opening displacement KW - Thermomechanical fatigue KW - Crack growth PY - 2021 SP - 1 EP - 10 PB - DVM (Deutscher Verband für Materialforschung und -prüfung) CY - Berlin AN - OPUS4-52519 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ganesh, R. A1 - Gesell, Stephan A1 - Fedelich, Bernard A1 - Kuna, Meinhard A1 - Kiefer, B. T1 - Procrackplast: Eine Software zur Simulation des 3D-Risswachstums unter großen plastischen Deformationen T1 - Procrackplast: A software for simulating 3D crack growth under large plastic deformation N2 - The finite element software ProCrackPlast is developed for the automated simulation of fatigue crack growth in arbitrarily loaded three-dimensional components with large scale plastic deformations, in particular under cyclic thermomechanical (TMF) loading. ProCrackPlast is developed by extending the software Procrack, created at TU Freiberg for linear-elastic crack growth simulations. The pre-processing, FEM analysis, and the post-processing in ProCrackPlast are done by the commercial software ABAQUS. ProCrackPlast resorts to a crack growth procedure which adaptively updates the crack in finite increments based on the fracture-mechanical parameter, cyclic crack tip opening displacement ΔCTOD . Features of this software along with two application examples of fatigue crack growth in a typical cast steel, Ni-Resist, are presented in this paper to show its capability and performance. N2 - Es wird die Finite-Element-Software ProCrackPlast vorgestellt, die eine automatische Simulation der Ermüdungsrissausbreitung in beliebig belasteten dreidimensionalen Bauteilen mit größeren plastisch verformten Bereichen ermöglicht, insbesondere bei thermomechanischer Wechselbelastung (TMF). ProCrackPlast entstand durch Erweiterung des Programs ProCrack, das an der TU Freiberg für linear-elastische inkrementelle Rissfortschrittsanalysen entwickelt wurde. Das Pre-Processing, die FEM Analyse und das Post-Processing werden mit Hilfe der kommerziellen FE-Software ABAQUS durchgeführt. ProCrackPlast beruht auf einem Algorithmus, mit dem der Rissfortschritt adaptiv in endlichen Inkrementen unter Verwendung des bruchmechanischen Parameters der zyklischen Rissöffnungsverschiebung ΔCTOD gesteuert wird. Die Funktionseigenschaften dieser Software werden anhand von zwei Anwendungsbeispielen zum Ermüdungsrisswachstum für einen typischen Stahlguss, Ni-Resist, exemplarisch dargestellt, um die Möglichkeiten und Leistungsfähigkeit von ProCrackPlast zu demonstrieren. T2 - 54. Tagung des Arbeitskreises "Bruchmechanik und Bauteilsicherheit" CY - Online meeting DA - 22.02.2021 KW - Automated finite element analysis KW - Automatische Finite Element Simulation KW - Thermomechanical fatigue KW - Crack growth KW - Thermomechanische Ermüdung KW - Rissausbreitung PY - 2022 SP - 205 EP - 214 PB - Deutscher Verband für Materialforschung und -prüfung e.V. AN - OPUS4-54435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ferrari, Bruno T1 - Microstructural evolution of PBF-LB/M Inconel 718 during solution-aging heat treatments - an in-situ x-ray diffraction study N2 - Inconel 718 (IN718) is a traditional age-hardenable nickel-based alloy that has been increasingly processed by additive manufacturing (AM) in recent years. In the as-solidified condition, IN718 exhibits chemical segregation and the undesired Laves phase, requiring a solution annealing (SA) prior to aging. The material produced by AM does not respond to the established thermal routines in the same way as conventionally produced IN718, and there is still no consensus on which routine yields optimal results. This work aims to provide a fundamental understanding of the heat treatment (HT) response by continuously monitoring the microstructural evolution during SA via time-resolved synchrotron x-ray diffraction, complemented by ex-situ scanning electron microscopy (SEM). The samples were produced by laser powder bed fusion to a geometry of 10x20x90 mm³, from which Ø1x5 mm³ cylindric specimens were extracted. Two different scanning strategies – incremental 67° rotations, Rot, and alternating 0°/67° tracks, Alt – were used, leading to two different as-built conditions. 1-hour SAs were carried out in the beamline ID22 of the ESRF at 50 KeV. Two SA temperatures, SA1 = 1020 °C, and SA2 = 1080 °C were tested for each scanning strategy. Data were processed using the software PDIndexer. In the as-built state, all samples showed typical subgrain columnar cell structures with predominant Nb/Mo segregation and Laves phase at the cell walls, as seen by SEM. The Alt scan induced higher intensity on the Laves peaks than the Rot scan, suggesting a greater content of Laves. Chemical homogenization in the SA was largely achieved during the heating ramp (Fig. 1). SA2 eliminated the Laves peaks just before reaching 1080 °C, and mitigated differences between Rot and Alt samples. On the other hand, SA1 induced the precipitation of the generally detrimental δ phase, also observed by SEM. Furthermore, the Rot scan showed higher δ peak intensities than the Alt scan, indicating a higher content of δ in the latter. No signs of recrystallization were observed in any of the investigated SAs. T2 - FEMS EUROMAT 2023 CY - Frankfurt a. M., Germany DA - 03.09.2023 KW - Additive Manufacturing KW - X-Ray Diffraction KW - Inconel 718 KW - Heat Treatments KW - Microstructure PY - 2023 AN - OPUS4-58392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Santos Baltieri, Ricardo T1 - Luminescence Thermometry in Pure TeO₂ Glasses Doped with Er3+/Yb3+ and Eu3+: Remote Sensing Capability Across the Biological Temperature Range N2 - The development of non-contact and remote temperature sensors based on rare-earth (RE3+)-doped glasses is crucial for emerging applications in biomedical diagnostics and microscale thermal monitoring. In this study, we explore the fundamental thermometric properties of pure tellurite (TeO2) glasses doped with either Er3+/Yb3+ or Eu3+ ions in a wide range of temperature. The Er3+/Yb3+-co-doped system was analyzed through upconversion emission thermometry, particularly involving thermally coupled levels 2H11/2 and 4S3/2. The intensity ratio between these levels exhibits a clear temperature dependence from 100 K to 530 K, with an inversion near 160 K and optimal sensitivity above 250 K. At 300 K, the relative sensitivity (SR) reached 1.1% K−1, and the absolute sensitivity peaked at 6.5 × 10−3 K−1 at 460 K. Figure on the left is the Er3+ upconversion luminescence dependency on temperature, in the center is the excitation spectra of Eu3+ with temperature, and on the right is the comparison between calculated and measured temperature for Eu3+ samples. In parallel, the excitation spectra of Eu3+-doped TeO2 glasses were acquired from 100 K to 520 K, revealing three thermally responsive spectral regions. These transitions exhibited temperature-dependent intensity inversions, enabling the use of excitation-based thermometry. Notably, one of the regions provided the most accurate temperature predictions, with a relative sensitivity of 0.5% K−1 at 300 K. Both systems benefit from the high optical transparency, chemical stability, and low phonon energy of pure TeO2 glass, making them ideal candidates for remote sensing platforms, such as fiber-optic tips or implantable probes. While the Er3+/Yb3+ system provides robust upconversion emission for conventional thermometry, the Eu3+ system introduces an innovative excitation-based strategy, broadening the applicability of RE3+-doped tellurite glasses for optical thermometry. Acknowledgements This work was supported by the São Paulo Research Foundation (FAPESP – N. 2020/11038-2, 2023/05994-6, 2024/04675-7) and National Council for Scientific and Technological Development (CNPq - 304718/2023-8). T2 - Shift 2025 Conference CY - Tenerife, Spain DA - 13.10.2025 KW - Lanthanide KW - Optical thermometry KW - Energy conversion PY - 2025 AN - OPUS4-65195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Darvishi Kamachali, Reza T1 - Melting upon Coalescence of Solid Nanoparticles N2 - The large surface-to-volume ratio of nanoparticles is understood to be the source of many interesting phenomena. The melting temperature of nanoparticles is shown to dramatically reduce compared to bulk material. Yet, at temperatures below this reduced melting point, a liquid-like atomic arrangement on the surface of nanoparticles is still anticipated to influence its properties. To understand such surface effects, here, we study the coalescence of Au nanoparticles of various sizes using molecular dynamics simulations. Analysis of the potential energy and Lindemann index distribution across the nanoparticles reveals that high-energy, high-mobility surface atoms can enable the coalescence of nanoparticles at temperatures much lower than their corresponding melting point. The smaller the nanoparticles, the larger the difference between their melting and coalescence temperatures. For small enough particles and/or elevated enough temperatures, we found that the coalescence leads to a melting transition of the two nominally solid nanoparticles, here discussed in relation to the heat released due to the surface reduction upon the coalescence and the size dependence of latent heat. Such discontinuous melting transitions can lead to abrupt changes in the properties of nanoparticles, important for their applications at intermediate temperatures. KW - Nanoparticles KW - Molecular Dynamics KW - Surface-induced Melting PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552183 DO - https://doi.org/10.3390/solids3020025 VL - 3 IS - 2 SP - 361 EP - 373 PB - MDPI AN - OPUS4-55218 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Darvishi Kamachali, Reza T1 - On the origin of embrittlement in Mn containing and Zn-coated steels N2 - Grain boundary embrittlement in medium-Mn steels and liquid metal embrittlement (LME) in Zn-coated high strength steels are among key challenges on the way of safe application of sustainable steels for automotive industry. Using a novel density-based model for grain boundaries, we reveal that the affinity of a grain boundary to attract Mn and Zn atoms result in a segregation transition accompanied by interfacial structural changes. In case of the Zn, the simulations show that the amount of segregation abruptly increases with decreasing temperature, while the Zn content in the alloy, required for triggering the segregation transition, decreases. The results are discussed in the context of CALPHAD-integrated density-based grain boundary phase diagrams. T2 - DPG 2024 CY - Berlin, Germany DA - 17.03.2024 KW - Phase-Field Simulation KW - CALPHAD KW - Steels KW - Density-based Thermodynamics PY - 2024 AN - OPUS4-60743 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Leo, Reinhold T1 - Duplex stainless steels - Compatibility for high-pressure hydrogen applications N2 - Duplex Stainless Steels (DSS) are an essential component used in the construction of transportation pipelines because of their many distinctive qualities. The choice of DSS for a particular hydrogen application mainly depends on its susceptibility level to Hydrogen Assisted Cracking (HAC). Several mechanisms have been proposed to describe the occurring microscale processes behind HAC, and these include metastable phase transformation, Hydrogen Enhanced Localized Plasticity (HELP), and Hydrogen Enhanced Decohesion (HEDE). This contribution describes the path to ascertain if DSS is suitable for high-pressure gaseous hydrogen applications. The interplay between several critical factors that result in HAC was examined using high-pressure gaseous hydrogen charging, Electron Backscatter Diffraction (EBSD), tensile testing and hydrogen concentration measurements using Carrier Gas Hot Extraction (CGHE). T2 - Third German-African Green Hydrogen Forum 2025 CY - Bernburg (Saale), Germany DA - 23.09.2025 KW - Hydrogen Assisted Cracking KW - High Pressure Hydrogen KW - Duplex Stainless Steels KW - Hollow Specimen Technique PY - 2025 AN - OPUS4-64302 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kianinejad, Kaveh A1 - Fedelich, Bernard A1 - Darvishi Kamachali, Reza A1 - Schriever, Sina A1 - Manzoni, Anna Maria A1 - Agudo Jácome, Leonardo A1 - Megahed, Sandra A1 - Kamrani, Sepideh A1 - Saliwan Neumann, Romeo T1 - Experimentally informed multiscale creep modelling of additive manufactured Ni-based superalloys N2 - 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. T2 - EUROMAT 23 CY - Frankfurt a. M., Germany DA - 04.09.2023 KW - IN738LC KW - Creep anisotropy KW - Crystal plasticity PY - 2023 AN - OPUS4-58263 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koerdt, Andrea T1 - The impact and potential of halophilic microorganisms on alternative fuels N2 - As more industrial interests focusing on using salt caverns and repurposed gas or petroleum reservoirs for alternative fuel storage, i.e. CO2/H2, the question raises whether microorganisms may impact the infrastructure, gas purity and storage condition over time. Environments with high salinity (> 1.5 Meq of NaCl) are resided by halophiles (salt-loving microorganisms). To compensate for the intensive osmotic stress, they have resorted to two main adaptation strategies: 1) production of compatible solutes and 2) accumulation of intracellular KCl. Microbial community analysis of several high salinity environments revealed a number of recurring genera, including Halomonas and Halanaerobium. However, the impact of halophiles on the overall integrity and stability of the storage facilities remain largely unknown. To evaluate the suitability and stability of saline storage facilities, several model halophilic microorganisms, such as members of Halomonas, will be selected as testing subjects. First, the impact of halophiles on the infrastructure will be determined using an integrative approach by combining a number of techniques, including electrochemistry, TOF-SIMS, SEM/FIB/EDS and FIB-TEM. Second, the abilities of halophiles to alter the fuel composition (i.e. increase/decrease the fractions of H2) will be monitored using gas chromatography by growing them under high pressure. As a result of climate change and the accompanying mandatory shift to renewable energy resources, microorganisms will continue to play an important role in the energy sector, both to their benefit and detriment. Thus, it is important to achieve a certain level of understanding regarding the activities and mechanisms of halophiles prior to large-scaled excursions. T2 - ISMOS-8 CY - Online meeting DA - 07.06.2021 KW - Microbiologically influenced corrosion KW - Hydrogen KW - Gas storage KW - Contamination PY - 2021 AN - OPUS4-52891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Camargo, Andrea A1 - Arai, Marylyn Setsuko T1 - Upconversion nanoparticles for chemical, physical and biological sensing: from functionalization to point-of-care devices N2 - Among several applications, versatile upconversion nanoparticles (UCNPs) which can convert lower-energy infrared radiation into higher-energy visible or ultraviolet light, have emerged as one of the most powerful tools in the field of chemical, physical and biological sensing. The use of UCNPs in fluorescent sensors allows non-invasive, highly sensitive, and selective detection methods, which are particularly beneficial in environments requiring minimal interference and high precision for analytes that can range from metal ions to biomolecules. In this lecture, an overview and the state of the art will be given, accompanied by examples of our recent contributions to key areas such as chronic disease diagnostics, bacterial sensing, and multifunctionally responsive nanoplatforms: (1) An Enhanced Luminescence Lateral-Flow Assay (ELLA) designed for rapid (< 15 min) and early detection of acute kidney injury biomarkers in urine samples, using a commercial cell phone camera, will be presented. The platform is based on Er³⁺- and Tm³⁺-doped UCNPs whose emissions intensities are 40-fold enhanced by an Au-coated mesoporous silica shell, enabling the accurate detection of KIM-1 and NGAL biomarkers with detection limits as low as 0.23 ng/mL; (2) Also, a multifunctional nanoplatform that combines Tm³⁺-doped UCNPs with a Cu(I) complex for applications in oxygen sensing, optical thermometry, and emission colour tuning will be presented. The platform utilizes Luminescent Resonance Energy Transfer (LRET) to achieve efficient energy transfer, enabling red emission from the Cu(I) complex while allowing the use of the UCNP’s original emissions for thermometry. The dual functionality allows sensitive O2 detection and temperature measurements, with relative sensitivities of up to 1% K⁻¹; (3) The critical challenge of rapid bacterial detection and differentiation was addressed by the development of a novel UCNP-based sensor. By functionalizing UCNPs with the antibiotics - vancomycin for Gram-(+) and polymyxin-B for Gram-(-), and using Au nanoparticles as intensity quenchers, the sensor leverages a ratiometric "turn-on" mechanism for selective detection of the bacteria, through changes in the green/red (G/R) ratio for Er-UCNP@PEG4-Van, and blue/red (B/R) ratio for Tm-UCNP@PEG4-Poly. By this approach, differentiation was possible over a wide concentration range of bacteria (0.05 to 5 x 105 CFU/mL) with high correlation with actual bacterial counts (r = 0.99 for S. aureus, r = 0.91 for E. coli); (4) Recently, we have demonstrated a water dispersable ratiometric pH-nanosensor based on host-guest interaction of Tm3+/Yb3+ co-doped UCNPs functionalized with b-cyclodextrin (b-CD) and a pH-responsive nitrobenzoxadiazol dye modified with adamantane (NBD-Ad). The sensor shows a ratiometric emission response (blue/red) over a pH range of 8.0 – 11.0 with high reproducibility, excellent reusability and selectivity, even in the presence of interferents. Together, the presented examples highlight the versatility and potential of UCNPs to develop novel sensors, offering measurable advances in diagnostics, environmental monitoring, and beyond. T2 - Shift2025 - Spectral shaping for biomedical and energy applications CY - Tenerife, Spain DA - 13.10.2025 KW - Upconverting nanoparticles KW - Fluorescent sensors KW - Point-of-care devices PY - 2025 AN - OPUS4-65282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Camargo, Andrea T1 - Enhanced emission of Nd3+ by localized silver nanocluster growth via direct laser writing in Ga-fluoride phosphate glasses N2 - Gallium fluoride phosphate glasses are promising materials for optical applications in the visible to near infrared spectra due to their wide transmission window and ability to accommodate optically active dopants. In this study, melt quenched glasses in the compositional system 25Ga(PO₃)₃–20ZnF₂–30BaF₂–(25–x–y)SrF₂–xAgNO₃–yNdF₃ (x = 0 -10 mol%, y = 0 or 1 mol%) were studied and fully characterized by conventional and spectroscopic techniques to understand the interaction of silver species and Nd³⁺ ions. In Ag+ doped samples, the observation of a broad emission band in the visible spectrum evidences the overlapping presence of Ag⁺, Ag nanoclusters (NCs), and [Ag₂]²⁺ species. In the sample doped with 10 mol% Ag⁺, the development of a dark yellow color and alterations in the emission profile suggest the formation of Ag nanoparticles. In an attempt to control and increase the formation of Ag nanoclusters in a localized way, the glasses with 3 and 5 mol% Ag+ were subjected to direct laser writing (DLW) with femtosecond laser pulses at variable inscription intensities and scan speeds. As expected, the approach led to localized growth of Ag-NCs with precise spatial control and as a consequence, the Nd³⁺ emissions in the NIR region (e.g. at1060 nm) were significantly enhanced in laser-structured regions as compared to unmodified areas, evidencing efficient energy transfer from silver species to Nd³⁺ ions. These results demonstrate that DLW, applied for the first time in these glasses, enables precise spatial control over silver nanocluster formation, offering a viable route to process optical glasses for photonic applications. T2 - XXIII - B-MRS Meeting CY - Salvador, Brazil DA - 28.09.2025 KW - Fluoride phosphate glasses KW - Direct laser writting KW - Neodymium KW - Silver nanoclusters PY - 2025 AN - OPUS4-65281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Anker, A. S. A1 - Balazs, D. M. A1 - Beyer, F. L. A1 - Bienert, Ralf A1 - Bouwman, W. G. A1 - Breßler, Ingo A1 - Breternitz, J. A1 - Brok, E. S. A1 - Bryant, G. A1 - Clulow, A. J. A1 - Crater, E. R. A1 - De Geuser, F. A1 - Giudice, A. D. A1 - Deumer, J. A1 - Disch, S. A1 - Dutt, S. A1 - Frank, K. A1 - Fratini, E. A1 - Gilbert, E. P. A1 - Hahn, Marc Benjamin A1 - Hallett, J. A1 - Hohenschutz, Max A1 - Hollamby, M. J. A1 - Huband, S. A1 - Ilavsky, J. A1 - Jochum, J. K. A1 - Juelsholt, M. A1 - Mansel, B. W. A1 - Penttilä, P. A1 - Pittkowski, R. K. A1 - Portale, G. A1 - Pozzo, L. D. A1 - Ricardo de Abreu Furtado Garcia, P. A1 - Rochels, L. A1 - Rosalie, Julian A1 - Saloga, P. E. J. A1 - Seibt, S. A1 - Smith, A. J. A1 - Smith, G. N. A1 - Annadurai, V. A1 - Spiering, G. A. A1 - Stawski, Tomasz A1 - Taché, O. A1 - Thünemann, Andreas A1 - Toth, K. A1 - Whitten, A. E. A1 - Wuttke, J. T1 - The human factor - Results of a small-angle scattering data analysis round robin N2 - 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. KW - Round robin KW - Sall-angle scattering KW - Nanostructure quantification KW - Nanostructure KW - SAXS KW - MOUSE KW - X-ray scattering KW - Size distribution KW - Nanoparticles PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571342 DO - https://doi.org/10.48550/arXiv.2303.03772 SP - 1 EP - 23 PB - Cornell University CY - Ithaca, NY AN - OPUS4-57134 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shasmal, Nilanjana T1 - Effects of Direct femtosecond laser writing on chloroborosilicate glasses doped with Eu3+/Eu2+ and CdS quantum dots N2 - Femtosecond (fs) direct laser writing (DLW) is a promising technique for developing nano-inhomogeneous materials with advanced optical properties and for fabricating novel photonic devices such as integrated waveguides, ultrafast optical switches, phase plates, and 3D optical memory. In this study, DLW was applied to chloroborosilicate glasses that were singly and co-doped with Eu and CdS quantum dots (QDs). The glasses were laser-treated within a very narrow range of experimental conditions, resulting in laser-inscribed sites exhibiting enhanced emission, similar to the glass-ceramics crystallized from the as-prepared glass. In the regions crystalized by DLW a significant reduction of Eu3+ to Eu2+ was verified by photoluminescence spectroscopy. However, the characteristics of the emission bands of Eu2+ changed markedly in the laser-treated sites as compared to the emission spectra of the same glass crystallized by heat treatment. A considerable redshift and splitting of the emission band were observed, attributed to changes in the surrounding environment of the rare earth (RE) ions which was, in turn, attributed to an alteration in the coordination number of Ba2 + and/or Eu2+ as a result of the high-power laser treatment. Although there was an issue with homogeneity of the glass in the micro-level, which restricts some of the aspects of the DLW, these findings suggest the potential for structural modifications through laser treatment, which could be harnessed to create new functionalities for advanced optical applications. T2 - ICG 2025 (27th International Congress on Glass) CY - Kolkata, India DA - 20.01.2025 KW - Femtosecond direct laser writing KW - DLW KW - CdS quantum dots KW - Eu/CdS co-doped glass PY - 2025 AN - OPUS4-65285 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Ávila Calderón, Luis A1 - Shakeel, Y. A1 - Schriever, Sina A1 - Gedsun, A. A1 - Forti, M. A1 - Jordan, Hans A1 - Han, Ying A1 - Baer, O. A1 - Aversa, R. A1 - Olbricht, Jürgen A1 - Hammerschmidt, T. A1 - Hickel, T. A1 - Skrotzki, Birgit T1 - NFDI-MatWerk/IUC02 Data schema for creep data of Ni-based superalloys including a comprehensive documentation of test results and metadata N2 - This data schema was developed within the infrastructure use case IUC02: “Framework for curation and distribution of reference datasets” of the consortium NFDI-MatWerk. It intends to define a structured approach for collecting all required information on a creep experiment using the established terminology of the respective test standard ISO 204:2022 and additional terminology agreed upon by the domain experts. The individual entries are grouped according to their content type and sub-summarized under respective headlines, thereby suggesting a basic categorization and a related hierarchy of concepts. This hierarchy can be similarly applied to other test methods and different metallic (and other) materials. In version 1.1 some editorial and formal changes were made. KW - NFDI-MatWerk KW - Digitalisierung KW - Referenzdaten KW - Kriechen KW - Ni-based Superalloys PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611629 DO - https://doi.org/10.5281/zenodo.11668375 PB - Zenodo CY - Geneva AN - OPUS4-61162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Ávila Calderón, Luis T1 - Mechanisches Verhalten von additiv gefertigtem nichtrostendem Stahl X2CrNiMo17-12-2 (AISI 316L) und Vergleich zur konventionell gefertigten Variante T1 - Mechanical behavior of additively manufactured stainless steel X2CrNiMo17-12-2 (AISI 316L) and comparison with a conventionally manufactured variant N2 - Die additive Fertigung (AM) metallischer Werkstoffe ist eine Technologie, die zunehmend Gegenstand von Forschungsaktivitäten und industrieller Anwendung ist. Dennoch steht sie noch vor Herausforderungen, um eine breite Nutzung in sicherheitsrelevanten Anwendungen zu erreichen. Die Hauptgründe für die Verzögerung des technologischen Durchbruchs zugunsten von AM-Metallen gegenüber konventionell hergestellten Varianten sind das Fehlen eines tieferen Verständnisses der Prozess-Struktur-Eigenschafts-Beziehungen und die begrenzte Verfügbarkeit von Daten zu den Materialeigenschaften. In diesem Kontext stellt diese Arbeit einen Beitrag sowohl zum Verständnis der Prozess-Struktur-Eigenschafts-Beziehungen als auch zur Verbesserung der Datenlage von 316L dar, einem häufig als Konstruktionswerkstoff in verschiedenen Hochtemperaturbauteilen verwendeten Werkstoff. Die Arbeit legt den Fokus auf die mittels Laser-Pulverbettschmelzen hergestellte Werkstoffvariante, PBF-LB/M/316L. Eine konventionell hergestellte Variante, HR/316L, wurde auch untersucht. Bei PBF-LB/M/316L wurde zusätzlich der Effekt ausgewählter Wärmebehandlungen ausgewertet. Die Untersuchung umfasste die Charakterisierung der mechanischen Eigenschaften und der Verformungs- und Schädigungsmechanismen bei erhöhten Prüftemperaturen bei LCF und Kriechen, wo die Daten und Wissenslage am spärlichsten ist. Außerdem hat die untersuchte PBF-LB/M/316L-Wersktoffvariante einen geringen Porositätsgrad. Somit hat diese Arbeit die Mikrostruktur stärker in den Fokus genommen als die meisten bisher in der Literatur verfügbaren Studien. Die mechanische Prüfkampagne umfasste Zugversuche zwischen Raumtemperatur und 650 °C, LCF-Versuche zwischen Raumtemperatur und 600 °C sowie Kriechversuche bei 600 °C und 650 °C. In Ermangelung konkreter Richtlinien und Normen wurde die Charakterisierung zumeist anhand der bestehenden internationalen Prüfnormen und Probengeometrien durchgeführt. Aus jedem dieser Prüfverfahren wurden die entsprechenden Festigkeits- und Verformungskennwerte ermittelt. Darüber hinaus wurde mit Hilfe gezielter mikrostruktureller Untersuchungen ein Beitrag zum Verständnis des Zusammenhangs zwischen der Mikrostruktur und den mechanischen Eigenschaften in Bezug auf die Verformungs- und Schädigungsmechanismen geleistet. Die Dehngrenze von PBF-LB/M/316L ist etwa doppelt so hoch wie die von HR/316L und dieser Trend setzt sich mit ansteigender Prüftemperatur fort. Die Bruchdehnung ist bei allen Prüftemperaturen geringer. PBF-LB/M/316L weist über den größten Teil der Ermüdungslebensdauer vor allem bei Raumtemperatur höhere zyklische Spannungen als HR/316L auf. Ausschließlich bei den kleinsten Dehnungs-schwingbreiten sind die Ermüdungslebensdauer ausgeprägt kürzer. Das Wechselverformungsverhalten von PBF-LB/M/316L ist durch eine Anfangsverfestigung gefolgt von einer kontinuierlichen Entfestigung charakterisiert, welche bis zum Auftreten der zum Versagen führenden Entfestigung stattfindet. Die Kriechbruchzeiten und die Dauer jeder Kriechphase sind bei allen Kombinationen von Prüfparametern bei PBF-LB/M/316 kürzer als bei HR/316L. Die Spannungsabhängigkeit von PBF-LB/M/316L ist im Vergleich zu HR/316L geringer und die Duktilität beim Kriechen kleiner. Die minimale Kriechrate wird bei allen geprüften Parameterkombinationen bei deutlich geringeren Kriechdehnungen erreicht. Eine Wärmebehandlung bei 450 °C / 4 h bewirkt keine wesentliche Änderungen der Mikrostruktur und Zugversuchseigenschaften. Eine zusätzliche Wärmebehandlung bei 900 °C / 1 h verursacht eine Abnahme der Dehngrenze des PBF-LB/M/316L. Diese blieb aber immer noch um den Faktor 1,5x höher als bei HR/316L. Die Verformungsmerkmale wurden kaum davon beeinflusst. Bezüglich des Kriechverhaltens hat die Wärmebehandlung bei 900 °C / 1 h längere sekundäre und tertiäre Kriechstadien bewirkt und die Kriechdehnung hat sich signifikant erhöht. Die Bruchbilder unterscheiden sich generell nicht nur aber vor allem mit ansteigender Prüftemperatur, bei der bei PBF-LB/M/316L oft interkristalline Rissbildung beobachtet wurde. Die Zellstruktur trägt als der Hauptfaktor zu den unterschiedlichen mechanischen Eigenschaften im Vergleich zur HR/316L-Variante bei. Darüber hinaus spielen mutmaßlich die Kornmorphologie, die Stapelfehlerenergie und der Stickstoffgehalt eine Rolle. N2 - Metal additive manufacturing (AM) is a technology that is increasingly the subject of research activities and industrial applications. However, it still faces challenges to achieve widespread use in safety-relevant applications. The main reasons for the delay of this technological breakthrough in favor of AM metals over conventionally manufactured variants are the lack of a deeper understanding of process-structure-property relationships and the limited availability of data on material properties. In this context, this work contributes to both achieving a better understanding of process-structure-property relationships and the improvement of data for 316L, an alloy frequently used as a structural material in various high-temperature components. The work focuses on a material variant produced by laser pow-der bed fusion, PBF-LB/M/316L. A conventionally produced variant, HR/316L, was also investigated. For PBF-LB/M/316L, the effect of selected heat treatments was also evaluated. The investigation included the characterization of the mechanical properties and the related deformation and damage mechanisms at elevated test temperatures in LCF and creep, where data and knowledge are scarce. The PBF-LB/M/316L variant studied has a low degree of porosity. Thus, this work is more focused on the microstructure than most studies available in the literature. The mechanical test campaign included tensile tests between room temperature and 650 °C, LCF tests between room temperature and 600 °C, and creep tests at 600 °C and 650 °C. In the absence of concrete guidelines and standards for testing of AM metals, the characterization mostly took place using existing international test standards and specimen geometries. From each of the test methods, corresponding strength, and deformation characteristic values were determined. In addition, targeted microstructural investigations contributed to understanding the relationship between the microstructure and the mechanical properties in terms of deformation and damage mechanisms. The proof stress of PBF-LB/M/316L is about twice that of HR/316L. This trend remains with increasing test temperature. The elongation after fracture is lower at all test temperatures. Regarding LCF, PBF-LB/M/316L exhibits higher cyclic stresses than HR/316L for most of the fatigue life, especially at room temperature. Exclusively at the smallest strain amplitudes, the fatigue lives of PBF-LB/M/316L are markedly shorter than in HR/316L. The cyclic stress-strain deformation behavior of PBF-LB/M/316L features an initial strain hardening followed by a continuous softening, which occurs until the softening leading to failure takes place. The creep rupture times and the duration of each creep stage are shorter for PBF-LB/M/316 than for HR/316L for all combinations of test parameters. The stress dependence of PBF-LB/M/316L is lower, and the creep ductility is smaller compared to HR/316L. The minimum creep rate is reached at significantly lower creep extensions for all parameter combinations tested. A heat treatment at 450 °C / 4 h did not cause significant changes in the microstructure and tensile behavior. An additional heat treatment at 900 °C / 1 h caused a decrease in the proof stress of PBF-LB/M/316L. However, it still remained higher than the one of HR/316L by a factor of 1.5x. The deformation characteristics were hardly affected. Regarding the creep behavior, this latter heat treatment at 900 °C / 1 h caused longer secondary and tertiary creep stages, and the creep strain increased significantly. The fracture characteristics generally differed, which happened not only but especially with increasing test temperature, where intergranular cracking often took place in PBF-LB/M/316L. The cellular structure is considered the main factor contributing to the different mechanical properties compared to the HR/316L variant. In addition, grain morphology, stacking fault energy, and nitrogen content might play a role. KW - AGIL KW - Additive Fertigung KW - Laser-Pulverbettschmelzen KW - Mikrostrukturentwicklung KW - 316L KW - LCF KW - Kriechen KW - Additive Manufacturing KW - Microstructure KW - Mechanical Properties KW - Mechanische Eigenschaften PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597143 DO - https://doi.org/10.14279/depositonce-19828 SP - 1 EP - 190 CY - Berlin AN - OPUS4-59714 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis T1 - Low cycle fatigue behavior of DED-L Ti-6AL-4V N2 - Laser powder-based directed energy deposition (DED-L) is a technology that offers the possibility for 3D material deposition over hundreds of layers and has thus the potential for application in additive manufacturing (AM). However, to achieve broad industrial application as AM technology, more data and knowledge about the fabricated materials regarding the achieved properties and their relationship to the manufacturing process and the resulting microstructure is still needed. In this work, we present data regarding the low-cycle fatigue (LCF) behavior of Ti-6Al-4V. The material was fabricated using an optimized DED-L process. It features a low defect population and excellent tensile properties. To assess its LCF behavior two conventionally manufactured variants of the same alloy featuring different microstructures were additionally tested. The strain-controlled LCF tests were carried out in fully reversed mode with 0.3 % to 1.0 % axial strain amplitude from room temperature up to 400°C. The LCF behavior and failure mechanisms are described. For characterization, optical microscopy (OM), scanning electron microscopy (SEM), and micro-computed tomography (µCT) were used. The low defect population allows for a better understanding of the intrinsic material’s properties and enables a fairer comparison against the conventional variants. The fatigue lifetimes of the DED-L material are nearly independent of the test temperature. At elevated test temperatures, they are similar or higher than the lifetimes of the conventional counterparts. At room temperature, they are only surpassed by the lifetimes of one of them. The principal failure mechanism involves multiple crack initiation sites. T2 - Ninth International Conference on Low Cycle Fatigue (LCF9) CY - Berlin, Germany DA - 21.06.2022 KW - AGIL KW - Additive Manufacturing KW - Ti-6Al-4V KW - Low-Cycle-Fatigue KW - Microstructure PY - 2022 AN - OPUS4-55123 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bhadeliya, Ashok A1 - Rehmer, Birgit A1 - Fedelich, Bernard A1 - Olbricht, Jürgen A1 - Skrotzki, Birgit A1 - Jokisch, T. ED - Zimmermann, M. T1 - Rissfortschrittsuntersuchungen an gefügten Nickelbasiswerkstoffen bei hoher Temperatur N2 - 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. T2 - Tagung „Werkstoffprüfung 2022“ CY - Dresden, Germany DA - 27.10.2022 KW - Lötverbindung KW - Rissfortschritt KW - SEN-Probe KW - Gefügte Nickelbasislegierungen PY - 2022 SN - 978-3-88355-430-3 VL - 2022 SP - 67 EP - 72 AN - OPUS4-57090 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bhadeliya, Ashok T1 - High temperature fatigue crack growth in nickel-based alloys joined by brazing and additive manufacturing N2 - 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. T2 - DGM Arbeitskreis Mechanisches Werkstoffverhalten bei hoher Temperatur im FachausschussWerkstoffverhalten unter mechanischer Beanspruchung CY - Munich, Germany DA - 10.10.2023 KW - Fatigue crack growth KW - Joined nickel-based alloys PY - 2023 AN - OPUS4-60908 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis T1 - Creep Behavior of Stainless Steel 316L Manufactured by Laser Powder Bed Fusion N2 - This contribution presents the results of an experimental study on the creep behavior of an austenitic 316L stainless steel produced by laser powder bed fusion (PBF-LB/M/316L) with an emphasis on understanding the effects of microstructure on the creep mechanisms. Hot tensile tests and constant force creep tests at 600 °C and 650 °C, X-ray computed tomography, as well as optical and electron microscopy were performed. The produced PBF-LB/M/316L exhibits a low void population (< 0.01 %) resulting from the manufacturing parameters used and which allowed us to understand the effects of other microstructural aspects on creep behavior, e.g., grain morphology and dislocation substructure. A hot‑rolled variant of 316L was also tested as a reference. T2 - International Materials Science and Engineering Congress - MSE 2024 CY - Darmstadt, Germany DA - 24.09.2024 KW - AGIL KW - Additive Fertigung KW - Mikrostruktur KW - Mikrostrukturentwicklung KW - Kriechen KW - Kriechschädigung PY - 2024 AN - OPUS4-61169 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Harald T1 - Tour de table - BAM N2 - Kurzübersicht über die neuen Aktivitäten zu Nanomaterialien in 2021. T2 - Nano-Behördenklausur der Bundesoberbehörden 2021 CY - Online meeting DA - 17.11.2021 KW - Nano KW - Nanomaterial KW - Nanopartikel KW - Bundesoberbehörden PY - 2021 AN - OPUS4-53827 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Gesell, Stephan A1 - Fedelich, Bernard A1 - Rehmer, Birgit A1 - Uhlemann, Patrick A1 - Skrotzki, Birgit A1 - Ganesh, R. A1 - Dude, D. P. A1 - Kuna, M. A1 - Kiefer, B. T1 - TMF-Rissverlaufsberechnung für ATL-Heißteile N2 - 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. KW - Abgasturbolader Heißteile KW - Numerische Simulation KW - Rissverlauf PY - 2023 VL - 1320 SP - 1 EP - 137 PB - Forschungsvereinigung Verbrennungskraftmaschinen (FVV) CY - Frankfurt am Main AN - OPUS4-56960 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bayerlein, Bernd T1 - Towards Interoperability: Digital Representation of a Material Specific Characterization Method N2 - Certain metallic materials gain better mechanical properties through controlled heat treatments. For example, in age-hardenable aluminum alloys, the strengthening mechanism is based on the controlled formation of nanometer sized precipitates, which represent obstacles to dislocation movement. Precise tuning of the material structure is critical for optimal mechanical behavior in the application. Therefore, analysis of the microstructure and especially the precipitates is essential to determine the ideal parameters for the interplay of material and heat treatment. Transmission electron microscopy (TEM) is utilized to identify precipitate types and orientations in a first step. Dark-field imaging (DF-TEM) is often used to image the precipitates and to 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, an automatable, digital approach is demonstrated. Based on DF-TEM images of different precipitation states of a wrought aluminum alloy, a modularizable digital workflow for quantitative precipitation analysis is presented. The integration of this workflow into a data pipeline concept will also be discussed. Thus, by using ontologies, the raw image data, their respective contextual information, and the resulting output data from the quantitative precipitation analysis can be linked in a triplestore. Publishing the digital workflow and the ontologies will ensure the reproducibility of the data. In addition, the semantic structure enables data sharing and reuse for other applications and purposes, demonstrating interoperability. The presented work is part of two digitization initiatives, the Platform MaterialDigital (PMD, materialdigital.de) and Materials-open-Laboratory (Mat-o-Lab). T2 - MSE 2022 CY - Darmstadt, Germany DA - 27.09.2022 KW - Interoperability KW - Ontology KW - Precipitation Analysis PY - 2022 AN - OPUS4-55892 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Skrotzki, Birgit T1 - Aging processes in precipitation hardened aluminum alloys N2 - The mechanical strength of wrought high-strength aluminum alloys is essentially based on precipitation hardening, possibly in combination with prior forming, e. g. by stretching. Important parameters for achieving an optimum combination of hardness, strength, ductility, toughness, and further properties such as corrosion resistance are age-hardening temperature and time. During thermal (mechanical) treatment, nucleation and growth of precipitates takes place, leading to the desired degree of hardening. In aluminum alloys, precipitation sequences are usually passed through, i. e. a sequence of metastable precipitates is formed before the stable phase can precipitate. The optimum combination of properties is therefore based on a certain (optimum) microstructure, which can, however, change during the use of a component, since the microstructure is not stable. This happens in particular when the operating temperatures are close to the aging temperature and/or the operating times are sufficiently long. An external mechanical load may accelerate the processes. The presentation gives some examples for this. T2 - Materials Science and Engineering Congress MSE 2022 CY - Darmstadt, Germany DA - 27.9.2022 KW - Aluminium alloy KW - Precipitation hardening KW - Aging KW - Degradation PY - 2022 AN - OPUS4-55877 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonrado T1 - Low-Cycle Fatigue Behavior of Laser Powder Bed Fused Inconel 718 at Room and High Temperature N2 - The nickel-base superalloy Inconel 718 (IN718) is one of the most commonly used Ni-based superalloys for high temperature structural applications for its remarkable strength, as well as creep, fatigue, and corrosion resistance up to 650 °C. While IN718 has traditionally been employed as cast or wrought material, it is difficult to machine because of its high strength and toughness. The additive manufacturing of IN718 components made by metal AM has thus gained extensive attention to produce expensive near-net shaped components of high-temperature alloys such as IN718, for it saves material and costs in processing and machining steps. Among all metal additive manufacturing (AM) technologies, laser powder bed fusion (PBF-LB/M) is the most widespread, IN718 being one of the most common alloys produced with it. However, high cooling rates associated to the PBF-LB/M process, hinders the primary strengthening phases γ’’ and γ’ to form, as these cooling rates induce a dislocation cellular substructure, at which walls primary Laves phases bind segregating Nb, Ti and Mo. Many of the therefore needed heat-treatment strategies can then promote Laves-phase transformation into the stable δ phase along the cell and grain boundaries. Laves and δ phases, as well as grain-boundary primary carbides may have adverse effects on mechanical properties. The mostly needle-shaped δ phase was namely found to have a detrimental effect on creep rupture life while no direct effect on LCF fatigue life was evident. In this work room- and high-temperature (650 °C) low-cycle fatigue behavior of PBF-LB/M IN718 is investigated in the four-step heat-treated state and compared to wrought IN718. The microstructure of both materials is characterized across length scales via microscopy methods. The fatigue life at room temperature of the PBF-LB/M IN718 material is slightly lower than that for the wrought material, which is reversed at 650 °C. The cyclic stress response for both materials is marked by cyclic softening that is more pronounced at higher test temperatures. Multiple secondary cracks form at high strain amplitudes, at both room and high temperatures. High testing temperatures enhance specially crack formation at the transitions of regions between elongated grains and columns of stacked grains with ripple patterns in the PBF-LB/M material. Additional to this behavior, pronounced crack branching and deflection indicate that the cracks are controlled by sharp micromechanical gradients. T2 - EUROMAT 2025 CY - Granada, Spain DA - 14.09.2025 KW - Additive manufacturing KW - Low-cycle fatigue KW - Microstructural characterization KW - Ni-base superalloy PY - 2025 AN - OPUS4-64354 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Ávila Calderón, Luis A1 - Han, Ying A1 - Matzak, Kathrin A1 - Olbricht, Jürgen A1 - Skrotzki, Birgit T1 - NFDI-MatWerk/IUC02 data schema for elevated temperature tensile data of Ni-based superalloys N2 - Strength characteristics, such as proof strength and tensile strength, of metallic materials are usually measured at room temperature. However, for high-temperature materials, the values at operational temperatures are equally important for analyzing the mechanical behavior of components or for designing purposes. Elevated temperature tensile tests (often referred to as hot tensile tests) generally enable the measurement of the same material parameters as those obtained at room temperature. Typically, tensile and proof strength, elongation after fracture, and reduction of area are analyzed, with the focus often being on proof strength. The attached data schema for elevated temperature tensile tests was developed within the German NFDI-MatWerk initiative (https://nfdi-matwerk.de/). It builds on a previously published creep data schema and follows a reference data methodology that has also been previously outlined. The presented schema constitutes a structured approach for collecting all relevant information on an elevated temperature tensile test experiment. Overall, this development, as defined in the previously published data schema for creep data, aims to provide a comprehensive hierarchical data description that can be implemented in data management platforms (such as electronic laboratory notebooks), facilitate consistent quality assessment across different users and data providers, and promote the alignment of datasets to the FAIR principles by providing easy interoperability and full reusability. The presented schema was initially developed for datasets of Ni-based high-temperature alloys. However, thanks to its modular structure, it can also be applied to tensile tests of various metallic and other materials. Although the focus is on elevated temperature tensile testing, the data schema also offers a solid foundation for documenting room temperature tensile tests. In such cases, an adjustment of the requirement profile might be necessary, and categories or entries specific to mechanical testing at elevated temperatures, such as “temperature-measuring system”, “specified temperature”, or “soaking time”, become irrelevant. Overall, a detailed approach was followed to ensure the collection of all relevant information, including both metadata and test results. This includes, for example, comprehensive descriptions of the material’s manufacturing history and of the laboratory equipment, and basic strength and deformation characteristic values. The resulting data schema aims to support the description and identification of high-quality datasets, which may qualify as reference data of materials. Our current definition of reference data of materials has been published elsewhere. It should be noted, however, that not all research datasets —depending on their origin and purpose— require this full level of detail. Nevertheless, the presented data schema can support data providers in evaluating the completeness and value of their datasets. This version of the data schema covers elevated temperature tensile tests on both single- and polycrystalline specimen materials. The terminology is aligned with DIN EN ISO 6892-1 and DIN EN ISO 6892-2. It is designed to record the use of temperature measurement using thermocouples and the use of contacting extensometer systems. The requirement profile refers to the highest quality class of reference data, taken from calibrated instruments, and which shall enable the following usages: 1. Checking one's own elevated temperature tensile test results on nominally similar material 2. Verification of own testing set-up (e.g., by testing the same or a similar material) 3. Using the data as input data for simulations in the context of design or alloy development KW - NFDI MatWerk KW - Referenzdaten KW - Zugversuch KW - CMSX-6 KW - Datenschema KW - NFDI MatWerk KW - CMSX-6 KW - Data schema KW - Reference data KW - Tensile test PY - 2025 UR - https://doi.org/10.5281/zenodo.17846436 DO - https://doi.org/10.5281/zenodo.17846435 PB - Zenodo CY - Geneva AN - OPUS4-65190 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Skrotzki, Birgit T1 - Interlinking Structured Data about Aging and Fattigue of an Aluminum Alloy N2 - In typical material oriented research projects numerous types and sources of data need to get connected to form the final outcome. The data-structures have to be described in a manner semantically concise enough so that all participants share the meaning and at the same time flexible enough to allow connecting findings and facts that have not been connected before. The present contribution describes the approach that is being taken in a public funded research project with two cooperating research institutes. The aim of the data-management solution is to describe and interlink three main entity types: material entities like a test specimen that is under observation, immaterial entities like a fatigue life model and processes that generate and transform the immaterial and material entities. The shared understanding of what is described by the data is achieved by referring to existing linked data resources. In addition a common thesaurus that is subject to ongoing discussion is used for concepts and terms that need precision beyond publicly available concept descriptions. The data associated with the entities and processes and entities is rather small and well structured. The entities and processes covered by the vocabularies are typical to laboratories performing fatigue testing and microstructure analysis. Through the interlinking of the entities and processes it becomes possible to intuitively understand the knowledge that is accumulating in the database. For example it is easy to trace the history of a creep test specimen starting from the chemical composition that has been analyzed for the heat, continuing with the heat treatment of the material, going into the creep test itself with the associated creep data and finally finding the transmission electron microscopy images that have been taken from the crept sample. The presented approach is prototypical way to tackle the sustainable management of structured open research data. Open questions remain for example with the management of attributions, the acceptance of an increased effort in data creation and the access control to specific regions of the data. On the other hand the approach sketches what added value can be created, if the community adopts and contributes to the linked data principles. T2 - LCF9 CY - Berlin, Germany DA - 21.6.2022 KW - Data management KW - Data linking KW - Thesaurus PY - 2022 AN - OPUS4-55159 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suarez Ocano, Patricia T1 - Influence of heat-treatment-induced microstructural evolution on the Low Cycle Fatigue behavior of 316L stainless steel fabricated by Laser Powder Bed Fusion N2 - Additive manufacturing, particularly the laser powder bed fusion (PBF-LB/M) process, has gained significant attention in recent years due to its ability to produce complex geometries with enhanced mechanical properties. Among the various materials used, 316L stainless steel is highly favored for cyclically loaded components due to its exceptional mechanical strength, high-temperature performance, and corrosion resistance, making it widely applicable across various industries. 316L SS fabricated by PBF-LB/M (PBF-LB/M/316L) exhibits a unique hierarchical microstructure, with high density of low-angle grain boundaries (LAGBs), nano-dispersed silicates, chemical micro-segregations, and solidification-induced cellular structures. Particularly, the submicron-sized cellular features enriched with chromium (Cr) and molybdenum (Mo), along with high dislocation densities, contribute to a superior strength-ductility balance compared to conventionally manufactured 316L SS. The dispersed silicate particles act also as a strengthening phase, impeding dislocation movement and enhancing plastic deformation resistance. This study explores the effect of heat treatments on the low-cycle fatigue (LCF) behavior of PBF-LB/M/316L at room temperature (RT) and 600 °C. First, three heat treatment conditions were applied to the as-built material: 450 °C for 4 hours (HT450/4), 800 °C for 3 hours (HT800/3), and 900 °C for 1 hour (HT900/1) to investigate their influence on microstructural evolution. Microstructural analysis revealed that the HT450/4 condition preserved the cellular structure with high dislocation density, while the HT800/3 condition showed partial dissolution of cells together with reduction in segregated elements along the cell walls and a reduced dislocation density. The HT900/1 condition resulted in complete segregation and cellular structure dissolution with comparable dislocation density to HT800/3 while maintaining the crystallographic texture and grain morphology. Intermetallic χ phase was mostly observed at the grain boundaries in HT800/3, but not in HT900/1. Fully reversed LCF tests were conducted under strain-controlled conditions with a strain amplitude of 0.8 %. Tests were interrupted at specific intervals to analyze the interaction between hierarchical microstructural features and deformation mechanisms in the three heat-treated conditions. Due to the pronounced dislocation cell structures and elemental segregation, the microstructure of the HT450/4 condition significantly impact deformation and damage mechanisms during cyclic loading, which in turn, differ from the conventional produced counterparts. The results provide insights into the relationship between microstructural features and fatigue performance, highlighting key deformation and failure mechanisms under cyclic loading. T2 - FEMS 2025 EUROMAT 18th European Congress and Exhibition on Advanced Materials and Processes CY - Granada, Spain DA - 14.09.2025 KW - Additive manufacturing KW - 316L stainless steel KW - Heat treatments KW - Low Cycle Fatigue KW - Microstructure PY - 2025 AN - OPUS4-64238 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schilling, Markus A1 - Skrotzki, Birgit T1 - Full dataset of several mechanical tests on an S355 steel sheet as reference data for digital representations N2 - The dataset provided in this repository comprises data obtained from a series of characterization tests performed to a sheet of typical S355 (material number: 1.0577) structural steel (designation of steel according to DIN EN 10025-2:2019). The tests include methods for the determination of mechanical properties such as, e.g., tensile test, Charpy test and sonic resonance test. This dataset is intended to be extended by the inclusion of data obtained from further test methods. Therefore, the entire dataset (concept DOI) comprises several parts (versions), each of which is addressed by a unique version DOI. The data were generated in the frame of the digitization project Innovationplatform MaterialDigital (PMD) which, amongst other activities, aims to store data in a semantically and machine understandable way. Therefore, data structuring and data formats are focused in addition to aspects in the field of material science and engineering (MSE). Hence, this data is supposed to provide reference data as basis for experimental data inclusion, conversion and structuring (data management and processing) that leads to semantical expressivity as well as for MSE experts being generally interested in the material properties and knowledge. KW - S355 steel sheet KW - Mechanical testing KW - Tensile test KW - Charpy test KW - Microstructure analysis KW - Digital representation KW - Data management KW - Data format PY - 2022 DO - https://doi.org/10.5281/zenodo.6778336 PB - Zenodo CY - Geneva AN - OPUS4-55141 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Jentzsch, Stefan A1 - Stock, Daniel A1 - Häcker, Ralf A1 - Skrotzki, Birgit A1 - Darvishi Kamachali, Reza A1 - Klingbeil, Dietmar A1 - Kindrachuk, Vitaliy T1 - Split Hopkinson Pressure Bar (SHPB) investigations of steel S355 specimens and complementary characterization methods N2 - The workbook SHPB_S355.xlsx contains in the main spreadsheet S355_TestOverview an overview on the S355 specimens, which were tested in Split Hopkinson Pressure Bar (SHPB) and complementary quasi-static (QS) tests. The tests were conducted with notched hat-shaped specimens without a notch offset (S355_TestOverview/column geometry: “no offset”) and a small notch offset of x=0.35 mm (S355_TestOverview/column geometry: “offset”), cf. Fig. 1 [1]. Furthermore, for selected specimens, links are provided to DIC and bar strain measurement files as well as to evaluations from further characterization methods (microhardness, EBSD). For the boundary conditions at the SHPB projectile impact, the pressures of the compressor p, driving the projectile, and the associated projectile impact velocities are provided in SHPB_S355.xlsx. The DIC displacement measurements are provided in FurtherMeasurements/DIC with frame output times in the file labels, which are associated with an imaginary trigger at the left end of the shortened incident bar (length 300 mm), which is considered within the SHPB simulation setup, see [1]. Furthermore, the DIC reference coordinate systems are provided as COS.jpg files in the respective DIC folders. Starting from the strain signals at the bars, captured by strain gauges at the incident (file name BC_Inc) and transmission bar (BC_Trans), displacement boundary conditions (which are provided for the tests in FurtherMeasurements/BarDisplBCs) are calculated by eq. (12) in [1], incorporating the acoustic velocity equal to 4639 m/s at the bars and a correction factor. Fig. 1 shows the shear specimen geometry (lengths in mm) with the offset of the notches x. For the quasi-static tests force(displacements)-values are directly provided in FurtherMeasurements/Fu_curves, which are considered from the relative displacements of the specimens, evaluated by DIC. The Vickers microhardness (HV 0.01) distribution across the shear localization zone was assessed by QNESS 60A+ EVO (DIN EN ISO 6507-1) for quasi-statically and dynamically tested specimens, applying the small notch offset, such that the specimens did not fail in the localization region. Therefore, raw data is provided in FurtherMeasurements/Microhardness. For fitting the microhardness distribution perpendicularly to the shear bands (as i.e. provided for the SHPB specimen in [1]), representative microhardness profiles were considered. Similarly for specimens with the small notch offset, EBSD data on dynamic and quasi-static tests is provided in FurtherMeasurements/EBSD. The grain size distributions for positions at the notch and the undeformed region are included in the subdirectory ./GrainLists_Shortened and EBSD images in the PowerPoint Presentations. Further information as the sizes and misorientations of the single grains, is incorporated in the subfolders ./GrainLists_FurtherInf. KW - Adiabatic shear bands KW - Split Hopkinson pressure bar KW - Digital image correlation PY - 2025 DO - https://doi.org/10.5281/zenodo.17591439 PB - Zenodo CY - Geneva AN - OPUS4-64842 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bayerlein, Bernd T1 - Digital Transformation in Materials Science:Insights from Platform MaterialDigital N2 - In the digital transformation of materials science and engineering, existing processes are being closely examined to optimize and extend them using technologies such as the Semantic Web, while adhering to the FAIR principles. The challenge is to identify and adapt these technologies to significantly improve daily operations, covering the entire cycle of data generation, collection, storage to its processing and use. This presentation presents different approaches developed within the Platform MaterialDigital (PMD) and related initiatives, each addressing specific challenges of digitalization and demonstrating their benefits. These will be illustrated by a case study on age-hardenable aluminium alloys in different aging states, based on a comprehensive dataset of microstructural and mechanical properties. In this context, ontologies are essential for organizing data into interoperable semantic structures, thereby enabling the representation of concepts and their relationships. The PMD Core Ontology (PMDco) serves as a higher semantic layer that connects domain-specific ontologies [1]. The PMDco provides MSE-specific bridging concepts that enhance data mapping and integration capabilities. This approach facilitates the linking of results from natural language processing of a corpus of microscopy abstracts, which supported the development of a microscopy ontology. In addition, the presentation highlights how modular, digital workflows can improve the reproducibility of transmission electron microscopy image processing and analysis [2]. It also shows how freely available mechanical and microstructural datasets are semantically integrated and made searchable through PMDco, facilitating correlation analysis [3]. Looking ahead, the integration of these components has the potential to advance and sustain MSE practices. T2 - MSE Congress 2024 - Materials Science and Engineering CY - Darmstadt, Germany DA - 24.09.2024 KW - Semantic Interoperability KW - FAIR data management KW - Digtial Representation PY - 2024 AN - OPUS4-61137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Skrotzki, Birgit T1 - Interconnecting data repositories: The Platform MaterialDigital (BMBF) N2 - Presentation of the Platform MaterialDigital. Presentation of the needs and challenges in materials science and engineering. T2 - 3rd EMMC International Workshop - EMMC CY - Online meeting DA - 02.03.2021 KW - Digitization KW - Standardization KW - Ontology PY - 2021 AN - OPUS4-52247 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Skrotzki, Birgit A1 - Schriever, Sina T1 - BAM reference data - Results of ASTM E139-11 creep tests on a reference material of Nimonic 75 nickel-base alloy N2 - Results of creep tests on a certified reference material at T = 600°C and a tensile creep load of 160 MPa are provided. The evaluated results include the times to reach 2% and 4% creep strain, respectively, and the creep rate after 400 h. The data were audited and are BAM reference data. KW - Reference data KW - Creep KW - Nickel-base alloy KW - Nimonic 75 KW - Reference material BCR-425 PY - 2021 DO - https://doi.org/10.5281/zenodo.5106606 PB - Zenodo CY - Geneva AN - OPUS4-52970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beygi Nasrabadi, Hossein A1 - Skrotzki, Birgit T1 - Ontology-oriented modeling of the Vickers hardness knowledge graph N2 - 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. T2 - ICMMM 2023: 10th International Conference on Mechanics, Materials and Manufacturing CY - Washington, D.C., USA DA - 18.08.2023 KW - Ontology KW - Knowledge graph KW - Data mapping KW - Vickers hardness KW - FAIR data PY - 2023 AN - OPUS4-58100 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Beygi Nasrabadi, Hossein A1 - Skrotzki, Birgit T1 - Tensile test ontology (TTO) N2 - Tensile Test Ontology (TTO) has developed for representing the Tensile testing process, testing equipment requirements, test pieces charactristics, and related testing parameters and their measurement procedure according to DIN EN ISO 6892-1 standard. Versions info: V2 developed using BFO+CCO top-level ontologies. V3 developed using PROVO+PMDco top-level ontologies. Repositories: GitLab: https://gitlab.com/kupferdigital/process-graphs/tensile-test GitHub: https://github.com/HosseinBeygiNasrabadi/Tensile-Test-Ontology-TTO- MatPortal: https://matportal.org/ontologies/TTO IndustryPortal: https://industryportal.enit.fr/ontologies/TTO KW - Ontology KW - Tensile testing PY - 2024 UR - https://gitlab.com/kupferdigital/process-graphs/tensile-test UR - https://github.com/HosseinBeygiNasrabadi/Tensile-Test-Ontology-TTO- UR - https://matportal.org/ontologies/TTO UR - https://industryportal.enit.fr/ontologies/TTO PB - GitLab CY - San Francisco, CA, USA AN - OPUS4-60545 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė A1 - Bustamante, Joana A1 - Mieller, Björn A1 - Stawski, Tomasz A1 - George, Janine A1 - Knoop, F. T1 - High-quality zirconium vanadate samples for negative thermal expansion (NTE) analysis N2 - 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. T2 - TDEP2023: Finite-temperature and anharmonic response properties of solids in theory and practice CY - Linköping, Sweden DA - 21.08.2023 KW - NTE KW - Sol-gel KW - Solid-state KW - Ab-initio KW - TDEP PY - 2023 AN - OPUS4-58135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė A1 - Bustamante, Joana A1 - Mieller, Björn A1 - Stawski, Tomasz A1 - George, Janine A1 - Knoop, F. T1 - High-quality zirconium vanadate samples for negative thermal expansion (NTE) analysis N2 - 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. T2 - 4th International Symposium on Negative Thermal Expansion and Related Materials (ISNTE-4) CY - Padua, Italy DA - 04.07.2023 KW - NTE KW - Sol-gel KW - Solid-state KW - Ab-initio KW - TDEP PY - 2023 AN - OPUS4-58132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė A1 - Bustamante, Joana A1 - Mieller, Björn A1 - Stawski, Tomasz A1 - George, Janine A1 - Knoop, F. T1 - High-quality zirconium vanadate samples for negative thermal expansion (NTE) analysis N2 - 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. T2 - 16th International conference on materials chemistry (MC16) CY - Dublin, Ireland DA - 03.07.2023 KW - NTE KW - Sol-gel KW - Solid-state KW - Ab-initio KW - TDEP PY - 2023 AN - OPUS4-58134 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė A1 - George, Janine A1 - Mieller, Björn A1 - Stawski, Tomasz T1 - ZrV2O7 negative thermal expansion (NTE) material N2 - Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material that exhibits significant isotropic contraction over a broad temperature range (~150°C < T < 800°C). Therefore, it can be used to create composites with controllable expansion coefficients and prevent thermal stress, fatigue, cracking, and deformation at interfaces. We implement interdisciplinary research to analyze such material. We study the influence of the synthesis methods and their parameters on the sample's purity, crystallinity, and homogeneity. Moreover, we implement ab initio-based vibrational computations with partially treated anharmonicity in combination with experimental methods to follow temperature-induced structural changes and rationalize the negative thermal expansion in this material, including the influence of the local structure disorder. T2 - SALSA Make and Measure Conference CY - Berlin, Germany DA - 13.09.2023 KW - NTE KW - Composites KW - TEM PY - 2023 AN - OPUS4-58367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Evans, Alexander T1 - Manufacturing a safer world: Diffraction based residual stress analysis for metal additive manufacturing N2 - Metal Additive Manufacturing (AM) technologies such as Laser Powder Bed Fusion (LPBF) are characterized by layer wise construction, which enable advancements of component design, with associated potential gains in performance and efficiency. However, high magnitude residual stresses (RS) are often a product of the rapid thermal cycles typical of the layerwise process. Therefore, a deep understanding of the formation of RS, the influence of process parameters on their magnitude and the impact on mechanical performance is crucial for widespread application. The experimental characterisation of these RS is essential for safety related engineering application and supports the development of reliable numerical models. Diffraction-based methods for RS analysis using neutrons and high energy X-rays enable non-destructive spatially resolved characterisation of both surface and bulk residual stresses in complex components. This presentation will provide an overview of recent research by the BAM at large scale facilities for the characterization of residual stresses in LPBF metallic alloys as a function of process parameters. In addition, the challenges posed by the textured and hierarchical microstructures of LPBF materials on diffraction-based RS analysis in AM materials will be discussed. This will include the question of the d0 reference lattice spacing and the appropriate choice of the diffraction elastic constants (DECs) to calculate the level of RS in LPBF manufactured alloys. T2 - 11th INternational Conference on Residual Stress (ICRS11) CY - Online meeting DA - 28.03.2021 KW - Residual stress analysis KW - Neutron diffraction KW - X-ray diffraction KW - Additive manufacturing KW - Laser powder bed fusion KW - AGIL PY - 2022 AN - OPUS4-54676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Evans, Alexander T1 - Ageing behaviour of laser powder bed fused 316L: a powder to failure approach N2 - Laser powder bed fusion (LPBF) is an additive manufacturing process for materials which inherently tends to yield various degrees of metastable hierarchical microstructures, defects and high residual stresses in the as-built condition depending on the process parameters. The understanding of the evolution of these typical features during heat treatment and subsequent thermal and mechanical ageing is crucial for the wider acceptance for safety critical structures. A multi-disciplinary research project at BAM studying the development of the microstructure, defects, residual stresses typical of LPBF 316L and their evolution during thermal and mechanical ageing has led to insights into the stability of these inherent features. This presentation aims to give a broad overview of the project with a few specific cases of investigation. Firstly, the formation of residual stresses, the nature of the initial microstructure, the tensile properties and a modelling approach to understand the anisotropy will be presented. This will be followed by examples of studies of their evolution during heat treatment, long term thermal exposure, and room temperature and high temperature mechanical testing compared to a baseline of conventional wrought variant of the same alloy. T2 - International Conference on Additive Manufacturing 2021 (ICAM 2021) CY - Online meeting DA - 01.11.2021 KW - Ageing KW - Additive manufacturing KW - Laser powder bed fusion KW - AGIL PY - 2021 AN - OPUS4-54106 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Markötter, Henning T1 - Tomographic Imaging Capabilities with hard X-Rays at BAMline (Bessy II) N2 - The BAMline at the synchrotron X-ray source BESSY II (Berlin, Germany) is supporting researchers especially in materials science. As a non-destructive characterization method, synchrotron X-ray imaging, especially tomography with hard X-Rays, plays an important role in structural 3D characterization. The imaging capabilities allow for in-situ and operando experiments. In this presentation the equipment, data handling pipeline as well as various examples from material science are presented. T2 - Correlative Materials Characterization Workshop 2023 CY - Brno, Czech Republic DA - 09.11.2023 KW - Tomography KW - X-ray imaging KW - Li-ion battery PY - 2023 AN - OPUS4-58958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Making materials (digital) - Keramik N2 - Der Vortrag gibt einen Überblick über die Materialklasse Keramik, insbesondere Technische Keramik. Nach einem kurzen Überblick über typische Anwendungen und Werkstoffe wird die keramische Prozesskette erläutert. Am Beispiel von Festigkeit wird der für Keramik typische, enge Zusammenhang zwischen Technologie, Mikrostruktur und Eigenschaften herausgearbeitet. Daraus werden Anforderungen für eine erfolgreiche Digitalisierung abgeleitet. T2 - Workshop "STREAM" - Semantische Repräsentation, Vernetzung und Kuratierung von qualitätsgesicherten Materialdaten CY - Darmstadt, Germany DA - 26.09.2022 KW - Keramik KW - Festigkeit KW - Überblick PY - 2022 AN - OPUS4-55859 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Evans, Alexander T1 - Entwicklung der Mikrostruktur der mechanischen Eigenschaften und der Eigenspannungen in L-PBF 316L N2 - Die additive Fertigung (AM) metallischer Werkstoffe mittels Laser Powder Bed Fusion (L-PBF) ermöglicht einzigartige hierarchische Mikrostrukturen, die zu Verbesserungen bestimmter mechanischer Eigenschaften gegenüber konventionell hergestellten Varianten derselben Legierung führen können. Allerdings ist das L-PBF-Verfahren häufig durch das Vorhandensein hoher Eigenspannungen gekennzeichnet, die es zu verstehen und zu mindern gilt. Daher ist das Verständnis der Mikrostrukturen, der Eigenspannungen und der daraus resultierenden mechanischen Eigenschaften entscheidend für eine breite Akzeptanz bei sicherheitskritischen Anwendungen. Die BAM hat ein multidisziplinäres Forschungsprogramm gestartet, um diese Aspekte bei LPBF 316L zu untersuchen. Der vorliegende Beitrag stellt einige der wichtigsten Ergebnisse vor: der Einfluss von Prozessparametern auf die Mikrostruktur, der Einfluss von Mikrostruktur und Textur auf die Festigkeit, Kriechverhalten und Schädigung und die Stabilität von Eigenspannungen und Mikrostruktur unter Wärmebehandlungsbedingungen. T2 - DGM 3. Fachtagung Werkstoffe und Additive Fertigung CY - Dresden, Germany DA - 11.05.2022 KW - Mechanische Eigenschaften KW - Additive Fertigung KW - L-PBF 316L KW - Entwicklung KW - Mikrostruktur KW - Eigenspannung PY - 2022 AN - OPUS4-55786 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schröder, Jakob T1 - Texture Dependent Micromechanical Anisotropy of Laser Powder Bed Fused Inconel 718 N2 - 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. T2 - International Conference on Additive Manufacturing ICAM 2022 CY - Orlando, FL, USA DA - 31.10.2022 KW - Laser powder bed fusion KW - Neutron diffraction KW - Electron backscatter diffraction KW - Mechanical behavior PY - 2022 AN - OPUS4-56376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schröder, Jakob T1 - Fundamentals of diffraction-based residual stress and texture analysis of PBF-LB Inconel 718 N2 - 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. T2 - MLZ User Meeting 2022 CY - Munich, Germany DA - 08.12.2022 KW - Diffraction KW - Residual Stress KW - Microstructure KW - Texture KW - Mechanical behavior PY - 2022 AN - OPUS4-56804 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Han, Ying T1 - Hochtemperaturermüdung der Aluminiumlegierung EN AW-2618A N2 - Abgasturbolader tragen wesentlich zur Effizienzsteigerung moderner Verbrennungsmotoren bei. Die im Abgasturbolader eingesetzten Radialverdichterräder werden überwiegend aus der warmfesten ausscheidungsgehärteten Aluminiumlegierung EN AW-2618A hergestellt. Die Anforderungen an die Radialverdichterräder steigen und die Betriebszeiten verlängern sich. Für eine optimale Auslegung des Bauteils ist unter anderem die Kenntnis des Ermüdungsverhaltens dieser Legierung erforderlich. Es ist bekannt, dass sich die Mikrostruktur dieser Legierung während des Betriebs vergröbert und dadurch die Festigkeit abnimmt. Das niederzyklische Ermüdungsverhalten für den Ausgangszustand des Werkstoffs und Prüftemperaturen bis 190 °C ist bereits gut untersucht. Für das hochzyklische Ermüdungsverhalten, insbesondere für Prüftemperaturen über 190 °C, liegen jedoch nur wenige Ergebnisse vor. Das Ziel dieser Arbeit ist es daher, die Datenbasis hinsichtlich der hochzyklischen Ermüdungslebensdauer bei erhöhten Prüftemperatur zu vervollständigen und das Werkstoffverhalten sowie die Schädigungsmechanismen zu charakterisieren. Zu diesem Zweck wurden axiale Ermüdungsversuche an glatten Proben durchgeführt. Neben dem T61-Ausgangszustand für eine Basischarakterisierung wurden zwei überalterte Zustände, jeweils bei 230 °C für 10 h und 1000 h ausgelagert und anschließend geprüft, um den Einfluss der Überalterung auf die Ermüdungslebensdauer zu erfassen. Die Auslagerungstemperatur von 230 °C der überalterten Zustände liegt deutlich über der Aushärtungstemperatur von 195 °C des T61-Zustands, was zu Veränderungen der optimal eingestellten Mikrostruktur führt, die sich wiederum in den mechanischen Eigenschaften widerspiegeln. Mit der Überalterungszeit von 10 h wurde ein Zustand untersucht, der einem Härteniveau entspricht, der bei Bauteilrückläufern nach Langzeitbetrieb beobachtet wurde und mit der Überalterungszeit von 1000 h wurden die Werkstoffgrenzen ermittelt. Zusätzlich wurde mittels Transmissionselektronenmikroskopie (TEM) die Vergröberung der festigkeitssteigernden S-Phase untersucht. Der Einfluss der Prüftemperatur auf die Ermüdungslebensdauer wurde durch Versuche bei 230 °C untersucht. Die Ermüdungsversuche wurde durch fraktographische Untersuchungen ergänzt und ausgewählte Ermüdungsversuche wurden mit zerstörungsfreien Prüfmethoden begleitet, um die Schädigung mit zunehmender Zyklenzahl dazustellen. Die Ergebnisse dieser Untersuchungen zeigen eine kürzere Ermüdungslebensdauer für die längere Überalterungszeit bei gleicher Spannungsamplitude. Die Transmissionselektronenmikroskopie zeigt, dass der mittlere Radius der S-Phase nach einer Überalterungszeit von 10 h um den Faktor 2,3 und nach 1000 h um den Faktor 2,7 im Vergleich zum Ausgangszustand zunimmt. Eine Erhöhung der Prüftemperatur auf 230 °C führt bei gleicher Spannungsamplitude zu einer Verkürzung der Ermüdungslebensdauer im Vergleich zu Raumtemperatur. Die fraktographischen Untersuchungen zeigen, dass unabhängig vom Werkstoffzustand und der Prüftemperatur die Rissinitiierung überwiegend an der Probenoberfläche oder in der Nähe der Primärphasen erfolgt. Das Risswachstum mit zunehmender Zyklenzahl kann mit der Replika-Methode erfolgreich abgebildet werden. Die Abbildung des Risses in der noch nicht gebrochenen Probe ist auch mit der Computertomographie möglich. KW - Aluminiumlegierung KW - EN AW-2618A KW - Ermüdung KW - HCF KW - Mikroskopie KW - Fraktographie PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615288 DO - https://doi.org/10.14279/depositonce-21381 SP - 1 EP - 109 PB - Depostit Once CY - Berlin AN - OPUS4-61528 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Rehmer, Birgit A1 - Bayram, Faruk A1 - Ávila Calderón, Luis A1 - Mohr, Gunther A1 - Skrotzki, Birgit T1 - BAM reference data: Temperature-dependent Young's and shear modulus data for additively and conventionally manufactured variants of Ti-6Al-4V N2 - 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. KW - Elastic modulus KW - Young's modulus KW - Shear modulus KW - Additive manufacturing KW - Ti-6Al-4V PY - 2023 DO - https://doi.org/10.5281/zenodo.7813732 PB - Zenodo CY - Geneva AN - OPUS4-57286 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Skrotzki, Birgit T1 - Improving the Reproducibility of Characterization and Quantification of Precipitates through Automated Image Processing and Digital Representation of Processing Steps N2 - The strength of age-hardenable aluminum alloys is based on the controlled formation of nm-sized precipitates, which represent obstacles to dislocation movement. Transmission electron microscopy (TEM) is generally used to identify precipitate types and orientations and to determine their size. This geometric quantification (e.g., length, diameter) is often performed by manual image analysis, which is very time consuming and sometimes poses reproducibility problems. The present work aims at the digital representation of this characterization method by proposing an automatable digital approach. Based on DF-TEM images of different precipitation states of alloy EN AW-2618A, a modularizable digital workflow is described for the quantitative analysis of precipitate dimensions. The integration of this workflow into a data pipeline concept is also presented. The semantic structuring of data allows data to be shared and reused for other applications and purposes, which enables interoperability. T2 - ICAA19 International Conference on Aluminum Alloys CY - Atlanta, GA, USA DA - 23.06.2024 KW - Digital representation KW - Automatable digital approach KW - Digital workflow KW - Quantitative image analysis KW - Data pipeline concept KW - Semantic structuring KW - Interoperability KW - FAIR data management PY - 2024 AN - OPUS4-60427 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Skrotzki, Birgit T1 - Ermüdungsrisswachstum von warmfestem austenitischem Gusseisen unter isothermen und anisothermen Belastungen N2 - Das Ermüdungsrisswachstumsverhalten des warmfesten Gusseisens EN-GJSA-XNiSiCr35-5-2 (auch unter der Bezeichnung Ni-Resist D-5S bekannt) wurde bei Raum- und hoher Temperatur untersucht. Es wurden kraftgeregelte Versuche bei konstanten Temperaturen (20 °C, 500 °C, 700 °C) ohne und mit Haltezeit und unterschiedlichen Lastverhältnissen durchgeführt. Zusätzlich wurde das Risswachstumsverhalten auch unter TMF-Belastung (Tmin = 400 °C, Tmax = 700 °C) unter IP- und OP-Bedingungen charakterisiert. Die Überwachung des Rissfortschritts erfolgte durch die Kombination von drei verschiedenen Techniken: Potenzialabfall, Thermografie und Compliance-Methode. Die Auswirkungen der verschiedenen Belastungsbedingungen auf das Ermüdungsrisswachstum werden vorgestellt und diskutiert. T2 - Bauteilverhalten bei thermomechanischer Ermüdung CY - Berlin, Germany DA - 25.03.2025 KW - Gusseisen KW - Thermomechanische Ermüdung KW - Rissfortschritt KW - Risswachstum KW - Ermüdungsriss KW - Thermographie PY - 2025 AN - OPUS4-63185 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis T1 - Microstructure Based Study on the Low Cycle Fatigue Behavior of Stainless Steel 316L manufactured by Laser Powder Bed Fusion N2 - Due to the advantages of Laser Powder Bed Fusion (PBF-LB), i.e., design freedom and the possibility to manufacture parts with filigree structures, and the considerable amount of knowledge available for 316L in its conventional variant, the mechanical behavior, and related microstructure-property relationships of PBF-LB/316L are increasingly subject of research. However, many aspects regarding the - application-relevant - mechanical behavior at high temperatures are not yet fully understood. Here, we present the results of an experimental study on the LCF behavior of PBF-LB/316L featuring a low defect population, which makes this study more microstructure-focused than most of the studies in the literature. The LCF tests were performed between room temperature (RT) and 600 °C. The mechanical response is characterized by strain-life curves, and hysteresis and cyclic deformation curves. The damage and deformation mechanisms are studied with X-ray computed tomography, and optical and electron microscopy. The PBF-LB/M/316L was heat treated at 450 °C for 4 h, and a hot‑rolled (HR) 316L variant with a fully recrystallized equiaxed microstructure was tested as a reference. Besides, selected investigations were performed after a subsequent heat treatment at 900 °C for 1 h. The PBF-LB/316L exhibits higher cyclic stresses than HR/316L for most of the fatigue life, especially at room temperature. At the smallest strain amplitudes, the fatigue lives of PBF-LB/M/316L are markedly shorter than in HR/316L. The main damage mechanisms are multiple cracking at slip bands (RT) and intergranular cracking (600 °C). Neither the melt pool boundaries nor the gas porosity have a significant influence on the LCF damage mechanism. The cyclic stress-strain deformation behavior of PBF-LB/M/316L features an initial hardening followed by a continuous softening. The additional heat treatment at 900 °C for 1 h led to decreased cyclic stresses, and a longer fatigue life. T2 - 4th Symposium on Materials and Additive Manufacturing CY - Berlin, Germany DA - 12.06.2024 KW - AGIL KW - 316L KW - Microstructure KW - Low Cycle Fatigue KW - Heat Treatment KW - Laser Poeder Bed Fusion PY - 2024 AN - OPUS4-60432 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Darvishi Kamachali, Reza A1 - Wang, Lei A1 - Lin, L. L. A1 - Manzoni, Anna Maria A1 - Skrotzki, Birgit A1 - Thompson, G. B. T1 - CALPHAD-informed density-based grain boundary thermodynamics N2 - The Gibbs free energy of a grain boundary is a complex thermodynamic function of temperature, pressure, and composition. These complexities add to the intrinsic crystallographic and chemical constraints imposed by the adjacent bulk phase. Recently we have proposed a density-based model for assessing grain boundary thermodynamics that enables a CALPHAD-informed description of the grain boundary. As such, the Gibbs free energy of the grain boundary is directly linked with available CALPHAD thermodynamic data. In this talk, new aspects of interfacial segregation and phase transformation are revealed by benchmarking the current model for various experimental cases, including several steels, high-entropy alloys and aluminum alloys. The effects of elastic interactions on the grain boundary segregation and the application of the model to a nanocrystalline Pt-Au alloy, with numerous grain boundaries of various characters, will be discussed. T2 - DPG (Deutsche Physiker Gesellschaft) CY - Online meeting DA - 27.09.2021 KW - Density-based model KW - Defects thermodynamics KW - Defects phase diagram KW - CALPHAD KW - Crystal Defects PY - 2021 AN - OPUS4-53556 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Rehmer, Birgit A1 - Bayram, Faruk A1 - Ávila Calderón, Luis A1 - Mohr, Gunther A1 - Skrotzki, Birgit T1 - BAM reference data: Temperature-dependent Young's and shear modulus data for additively and conventionally manufactured variants of Ni-based alloy Inconel IN718 N2 - 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. KW - Elastic modulus KW - Young's modulus KW - Shear modulus KW - Additive manufacturing KW - IN718 PY - 2023 DO - https://doi.org/10.5281/zenodo.7813824 PB - Zenodo CY - Geneva AN - OPUS4-57287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis T1 - Creep Behavior of Stainless Steel 316L Manufactured by Laser Powder Bed Fusion N2 - The broader industrial adoption of metal AM in safety-critical applications is limited, among others, by the still in-sufficient understanding of process–structure–property relationships and a lack of reliable mate-rial data. The content presented here approaches this limitation regarding the creep behavior of one of the most studied AM alloys: PBF-LB/M/316L stainless steel. A nearly as-built and a condition heat treated at 900 °C for 1 h, along with a conventionally manufactured variant are investigated. The creep behavior until reaching the minimum creep rate is mainly determined by the solidification cell structure. The damage is overall mainly intergranular, independent of the heat treated condition. The heat treatment at 900 °C for 1 h partially influenced the microstructure (mainly in terms of cell structure). The creep behavior until reaching the minimum creep rate remained nearly unchanged. The creep lifetime and ductility were enhanced. The crystallographic texture evolved after creep deformation. T2 - TMS 2025 Annual Meeting & Exhibition CY - Las Vegas, NV, USA DA - 23.03.2025 KW - AGIL KW - Creep KW - 316L KW - Microstructure PY - 2025 AN - OPUS4-63456 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Han, Ying T1 - The influence of overaging on high cycle fatigue of Al-alloy EN AW-2618A N2 - The aluminum alloy EN AW-2618A (2618A) is a precipitation hardened high strength alloy that is used at elevated temperatures in the transportation and aerospace industries. The main alloying elements are Cu and Mg which form a coarse intermetallic primary phase (Al9FeNi) of several µm in size. This phase is responsible for the long-term high temperature creep resistance. The basic strength is due to the precipitation of the so-called S-phase (Al2CuMg) of nm-size, which is known to coarsen during service at elevated temperatures. Previous projects have characterized the alloy in terms of strength, low cycle fatigue (LCF) and creep behavior, especially at high temperatures (up to 190 °C). Both the T61 and overaged states were used. In addition, the microstructural changes associated with overaging were extensively studied and quantified microscopically [1-2]. However, data on high cycle fatigue (HCF) is still very limited. Therefore, this study [3] investigates the influence of overaging on HCF of 2618A. For this purpose, axial HCF tests were performed at room temperature on two overaged states which are aged for 10 h and 1000 h at 230 °C. Electron microscopy was used to characterize the coarsening of the S-phase from the two overaged states. Fractographic studies were also performed to investigate the influence of the primary phase on the fatigue life. T2 - MSE 2024 CY - Darmstadt, Germany DA - 24.09.2024 KW - Fatigue KW - Aluminum alloy KW - EN AW-2618A PY - 2024 AN - OPUS4-61188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schilling, Markus T1 - FAIR tensile test data in PMD: From a standard-compliant application ontology to RDF data in a triple store N2 - Following the new paradigm of materials development, design and optimization, the digitalization of materials and processes is the main goal which imposes a huge challenge. In this respect, the quality assurance of processes and output data as well as the interoperability between applications following FAIR (findability, accessibility, interoperability, reusability) principles are to be ensured. This includes storage, processing and querying of data in a preferably standardized form, also addressing the incorporation of standardization bodies. To meet the challenge to contextualize material data in a way that is consistent with all stakeholders, all necessary information on the condition of the material including production and application-related changes have to be made available via a uniform, machine-readable description. For this purpose, ontologies are to be used since they allow for machine-understandable knowledge representations and semantic conceptualizations that are needed for data management and the digitalization in the field of materials science. With respect to this currently ever-growing topic of integration and reuse of data and knowledge from synthesis, production and characterization of materials, this presentation shows the efforts taken within the project Platform MaterialDigital (PMD, materialdigital.de) to store tensile test data in accordance with a standard-compliant ontological representation. The includes the path from developing an ontology in accordance with the respective standard, converting ordinary and arbitrarily selected data gained from standard tests into the interoperable RDF format, up to connecting the ontology and data, respectively. Finally, such data can be queried from a triple store. In the field of material science and engineering (MSE), most mechanical test methods are standardized which serves as a valid basis for ontology development. Therefore, the well-known tensile test of metals at room temperature (DIN EN ISO standard 6892-1:2019-11) was selected to be considered as one of the first use cases in PMD. This consideration within the PMD features both, the ontological representation of such a tensile test in accordance with the standard as well as exemplary data generation. The semantic connection of the ontology and data leads to interoperability and an enhanced ability of querying. T2 - MSE 2022 CY - Darmstadt, Germany DA - 27.09.2022 KW - S355 steel sheet KW - Mechanical testing KW - Tensile test KW - Digitization KW - Ontology KW - Data structure KW - Material digital PY - 2022 AN - OPUS4-55882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Hennecke, M. ED - Skrotzki, Birgit T1 - Hütte Band 1: Mathematisch-naturwissenschaftliche und allgemeine Grundlagen für Ingenieure N2 - 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 1 enthält die mathematisch-naturwissenschaftlichen und allgemeinen Grundlagen. KW - Mathematisch-naturwissenschaftliche Grundlagen KW - Allgemeine Grundlagen PY - 2022 SN - 978-3-662-64368-6 DO - https://doi.org/10.1007/978-3-662-64369-3 SN - 2522-8188 SP - 1 EP - 895 PB - Springer Vieweg CY - Berlin ET - 35 AN - OPUS4-56234 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schilling, Markus T1 - Transforming Materials Science with ontologies, ELN, and LIMS: Semantic Web Solutions for Digitalization and Data Excellence N2 - Following the new paradigm of materials development, design and optimization, digitalization is the main goal in materials sciences (MS) which imposes a huge challenge. In this respect, the quality assurance of processes and output data as well as the interoperability between applications following FAIR (findability, accessibility, interoperability, reusability) principles are to be ensured. For storage, processing, and querying of data in contextualized form, Semantic Web Technologies (SWT) are used since they allow for machine-understandable and human-readable knowledge representations needed for data management, retrieval, and (re)use. The project ‘platform MaterialDigital’ (PMD) is part of an initiative that aims to bring together and support interested parties from both industrial and academic sectors in a sustainable manner in solving digitalization tasks and implementing digital solutions. Therefore, the establishment of a virtual material data space and the systematization of the handling of hierarchical, process-dependent material data are focused. Core points to be dealt with are the development of agreements on data structures and interfaces implemented in distinct software tools and to offer users specific added values in their projects. Furthermore, the platform contributes to a standardized description of data processing methods in materials research. In this respect, selected MSE methods are ontologically represented which are supposed to serve as best practice examples with respect to knowledge representation and the creation of knowledge graphs used for material data. Accordingly, this presentation shows the efforts taken within the PMD project to store data in accordance with a testing standard compliant ontological representation of a tensile test of metals at room temperature (ISO 6892-1:2019-11). This includes the path from developing an ontology in accordance with the respective standard 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 enhanced reusability of data and knowledge from synthesis, production, and characterization of materials, the PMD core ontology (PMDco) was developed as mid-level ontology in the field of MSE. The semantic connection of the tensile test ontology (TTO) to the PMDco leads to enhanced expressivity and interoperability. Moreover, as a best practice example, generation and acquisition of test data semantically connected to the ontology (data mapping) was realized by applying an electronic laboratory notebook (ELN). Corresponding tensile tests were performed by materials science students at university. This enabled a fully digitally integrated experimental procedure that can be transferred to other test series and experiments. In addition to facilitating the acquisition, analysis, processing, and (re)usability of data, this also raises the awareness of students with respect to data structuring and semantic technologies in the sense of education and training. The entire data pipeline is further seamlessly integrable in a laboratory information management system (LIMS). More specifically, the integration of semantic conceptualization and knowledge graphs may become essential parts in LIMS as this would be very beneficial. Therefore, some first approaches of SWT integration in LIMS will also be presented briefly. T2 - TMS Specialty Congress 2024 CY - Cleveland, OH, USA DA - 16.06.2024 KW - Semantic Data KW - Plattform Material Digital KW - Tensile Test Ontology KW - Electronic Lab Notebook KW - Material Life Cycle PY - 2024 AN - OPUS4-60394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shakeel, Yusra A1 - Ávila Calderón, Luis T1 - Creating Exemplary RDM Reference Datasets: Technical Process Overview N2 - 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. T2 - All-Hands-on-Deck congress from the NFDI-MatWerk CY - Siegburg, Germany DA - 08.03.2023 KW - NFDI KW - Reference Dataset KW - FAIR KW - Research Data Management PY - 2022 AN - OPUS4-57149 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Beygi Nasrabadi, Hossein A1 - Skrotzki, Birgit T1 - Tensile stress relaxation test ontology (TSRTO) N2 - Tensile Stress Relaxation Test Ontology (TSRTO) has developed for representing the tensile stress relaxation testing process, testing equipment requirements, test pieces charactristics, and related testing parameters and their measurement procedure according to DIN EN ISO 10319-1 standard. Versions info: V1 developed using BFO+CCO top-level ontologies. V3 developed using PROV+PMDco top-level ontologies. Repositories: GitLab: https://gitlab.com/kupferdigital/process-graphs/relaxation-test GitHub: https://github.com/HosseinBeygiNasrabadi/Tensile-Stress-Relaxation-Test-Ontology-TSRTO MatPortal: https://matportal.org/ontologies/TSRTO IndustryPortal: https://industryportal.enit.fr/ontologies/TSRTO KW - Ontology KW - Tensile stress relaxation testing KW - FAIR data PY - 2024 UR - https://gitlab.com/kupferdigital/process-graphs/relaxation-test UR - https://github.com/HosseinBeygiNasrabadi/Tensile-Stress-Relaxation-Test-Ontology-TSRTO UR - https://matportal.org/ontologies/TSRTO UR - https://industryportal.enit.fr/ontologies/TSRTO PB - GitLab CY - San Francisco, CA, USA AN - OPUS4-60546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Skrotzki, Birgit T1 - Radii of S-phase Al2CuMg in Al-alloy EN AW 2618A after different aging times at 190°C N2 - The dataset contains data from quantitative microstructural analysis of transmission electron microscopy (TEM) studies of the S-phase (Al2CuMg) radii in Al-alloy EN AW 2618A. The investigated material and the applied methods were described in detail in two publications. KW - Aluminium alloy KW - EN AW 2618A a KW - S-phase KW - Al2CuMg KW - Aging KW - Creep KW - Radii distribution KW - TEM PY - 2022 UR - https://doi.org/10.5281/zenodo.6659461 UR - https://doi.org/10.5281/zenodo.7625259 DO - https://doi.org/10.5281/zenodo.6659460 PB - Zenodo CY - Geneva AN - OPUS4-55067 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis T1 - Research Data Management for Creep Reference Data of Ni Based Superalloys N2 - In times of digital data processing and sharing, a central challenge for the Materials Science and Engineering (MSE) community is the complete digital representation of materials, including their relevant processing and microstructure details and the resulting properties. This digital representation, supported by digital infrastructures, enables entirely new qualities of collaborative work and is central to how we will conduct MSE research and develop products in the future. The main challenges are the composition, shaping, and description of the data so that it can be easily interpreted, trusted, and re-used. This presentation introduces our current effort to develop a best practice framework for generating and distributing creep reference datasets for Ni-based superalloys, which builds on previous approaches. Researchers can use such datasets to compare their own experimental or simulation results, used, for instance, to perform simulation-based alloy design and optimization or in the verification of the own testing equipment. The concept includes building an easily accessible digital infrastructure to annotate and discover the datasets and the integration of an ontology that aligns with the necessary metadata schema. With the help of an ontology, the reference dataset for creep can be semantically described, thus enabling the digital representation and reusage of shared concepts from domain experts and the community. To achieve this, it is necessary to establish a defined vocabulary with corresponding relations and annotations. The interplay between a digital infrastructure, the agreement on the necessary metadata and related metadata schema, and an underlying ontology will ensure that data and results can be easily shared, taken up, and re-used, thus fulfilling the FAIR principles (Findable, Accessible, Interoperable, Reusable). Furthermore, we aim to develop a widely accepted definition of reference data and data quality levels and to reach a self-supported community process. We intend to motivate the discussion about reference material datasets, necessary metadata, and future collaborations within the creep community. T2 - 16th International Conference on Creep and Fracture of Engineering Materials and Structures CY - Bangalore, India DA - 28.07.2024 KW - Reference Data KW - Creep KW - Data schema KW - Research Data Management PY - 2024 AN - OPUS4-60837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gesell, Stephan T1 - A CTOD-based crack growth law for thermomechanical fatigue N2 - 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. T2 - European Conference on Fracture 2022 CY - Funchal, Portugal DA - 27.06.2022 KW - Fatigue crack growth KW - Finite elmenet simulation KW - TMF experiments PY - 2022 AN - OPUS4-56934 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mrkwitschka, Paul A1 - Abram, Sarah-Luise A1 - Thünemann, Andreas A1 - Rühle, Bastian A1 - Radnik, Jörg A1 - Bresch, Harald A1 - Resch-Genger, Ute A1 - Hodoroaba, Vasile-Dan T1 - The Role of Electron Microscopy in the Development of Monodisperse Cubic Iron Oxide Nanoparticles as Certified Reference Material for Size and Shape N2 - BAM is 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 to the material and life sciences. As a first candidate of this series, we present cubic iron oxide nanoparticles with a nominal edge length of 8 nm. These particles were synthesized by thermal decomposition of iron oleate in high boiling organic solvents adapting well-known literature procedures. After dilution to a concentration suitable for electron microscopy (TEM and SEM) as well as for small-angle X-ray scattering (SAXS) measurements, the candidate nanoRM was bottled and assessed for homogeneity and stability by both methods following the guidelines of ISO 17034 and ISO Guide 35. The particle sizes obtained by both STEM-in-SEM and TEM are in excellent agreement with a minimum Feret of 8.3 nm ± 0.7 nm. The aspect ratio (AR) of the iron oxide cubes were extracted from the images as the ratio of minimum Feret to Feret resulting in an AR of 1.18 for TEM to 1.25 for SEM. Alternatively, a rectangular bounding box was fitted originating from the minimum Feret and the longest distance through the particle in perpendicular direction. This led to AR values of 1.05 for TEM and 1.12 for SEM, respectively. The results confirm the almost ideal cubic shape. KW - Reference nanoparticles KW - Iron oxide KW - Cubical shape KW - Electron microscopy KW - SAXS KW - Nano CRM KW - Size PY - 2022 DO - https://doi.org/10.1017/S1431927622003610 SN - 1435-8115 VL - 28 IS - Suppl. 1 SP - 802 EP - 805 PB - Cambridge University Press AN - OPUS4-55599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - The Role of Electron Microscopy in the Development of Monodisperse Cubic Iron Oxide Nanoparticles as CRM for Size and Shape N2 - 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. T2 - Microscopy and Microanalysis 2022 CY - Online meeting DA - 31.07.2022 KW - Certified Referencematerial KW - Cubical Iron Oxide KW - Nanoparticles KW - Electron Microscopy KW - Small-Angle X-ray Scattering PY - 2022 AN - OPUS4-57035 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - López de Ipina, J.-M. A1 - Arevalillo, A. A1 - Martín, A. A1 - Caillard, B. A1 - Marcoulaki, E. A1 - Aguerre- Charol, O. A1 - van Duuren-Stuurman, B. A1 - Hodoroaba, Vasile-Dan A1 - Viitanen, A.-K. A1 - Witters, H. A1 - Vercauteren, S. A1 - Persson, K. A1 - Bard, D. A1 - Evans, G. A1 - Jensen, K.A. A1 - Himly, M. A1 - Scalbi, S. A1 - Papin, A. A1 - Le Bihan, O. A1 - Kanerva, T. A1 - Tirez, K. A1 - Frijns, E. A1 - Niga, P. A1 - Eleftheriadis, K. A1 - Travlos, A. A1 - Geppert, M. A1 - Himly, M. A1 - Radnik, Jörg A1 - Kuchenbecker, Petra A1 - Resch-Genger, Ute A1 - Fraboulet, I. A1 - Bressot, C. A1 - Rissler, J. A1 - Gaucher, R. A1 - Binotto, G. A1 - Krietsch, Arne A1 - Braun, A. A1 - Abenet, S. A1 - Catalan, J. A1 - Verstraelen, S. A1 - Manier, N. A1 - Manzo, S. A1 - Fransman, S. A1 - Queron, J. A1 - Charpentier, D. A1 - Taxell, D. A1 - Säämänen, A. A1 - Brignon, J.-M. A1 - Jovanovic, A. A1 - Bisson, M A1 - Neofytou, P. T1 - EC4Safenano - Catalogue of Services N2 - The publicly available document encapsulates the first version of the Catalogue of Services of the future EC4Safenano Centre (CoS 2019). The CoS 2019 is structured in 12 Service Categories and 27 Service Topics, for each of the 12 categories considered. This architecture configures a 12 x 27 matrix that allows ordering the potential EC4Safenano offer in 324 types of services/groups of services. Each type of service/group of services is described, in a simple and friendly way, by means of a specific service sheet: the EC4Safenano - Service Data Sheet (EC4-SDS). These EC4-SDSs allow structuring and summarizing the information of each service, providing the customer with a concise view of characteristics of the service and also the contact details with the service provider. The CoS 2019 deploys a map of services consisting of a set of 100 EC4-SDSs, covering 7 of the 12 Service Categories and 17 of the 27 Service Topics. The harmonization of services is visualized as a future necessary step in EC4Safenano, in order to strengthen the offer and provide added value to customers with a growing offer of harmonized services in future versions of the CoS. The information contained in this document is structured in 3 main sections, as follows: • Catalogue structure. This section describes in short the main characteristics of the CoS 2019. • Catalogue content. This section represents the core part of the document and encapsulates the set of 100 SDSs displaying the offer proposed by the CoS 2019. • Online Catalogue. This section describes the resources implemented by EC4Safenano to facilitate the on-line consultation of the CoS 2019 by customers and other interested parties. KW - Nano-safety KW - Analytical services KW - Nanomaterials KW - Catalogue of services KW - EC4SafeNano KW - European Centre PY - 2021 UR - https://ec4safenano.eu-vri.eu/Public/Guidance SP - 1 EP - 72 PB - EU-VRi – European Virtual Institute for Integrated Risk Management CY - Stuttgart, Germany AN - OPUS4-52943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis T1 - Kriech- und Bruchverhalten von additiv hergestelltem austenitischem Stahl 316L. Vergleich zum konventionellen Werkstoff. N2 - Eine kritische Aufgabe im Rahmen der Etablierung von Prozess-Struktur-Eigenschafts-Performance-Beziehungen bei der additiven Fertigung (AM) von Metallen ist die Ermittlung von zuverlässigen und gut dokumentierten Kennwerten zum Materialverhalten sowie das Schaffen von Wissen über die Struktur-Eigenschafts-Korrelation. Schließlich ist dies die Grundlage für die Entwicklung gezielterer Prozessoptimierungen und zuverlässigerer Lebensdauer-Vorhersagen. In diesem Zusammenhang zielt dieser Beitrag darauf ab, Daten und Erkenntnisse über das Kriechverhalten des austenitischen Edelstahls 316L zu liefern, der mittels Laser-Powder-Bed-Fusion (L-PBF) hergestellt wird. Um dieses Ziel zu erreichen, wurden Proben aus konventionellem warmgewalztem sowie AM-Material gemäß den bestehenden Normen für konventionelles Material geprüft und vor und nach dem Versagen mikrostrukturell charakterisiert. Die Probekörper wurden aus einzelnen Blöcken des AM-Materials gefertigt. Die Blöcke wurden mit einer Standard-Scan- und Aufbaustrategie hergestellt und anschließend wärmebehandelt. Das Kriechverhalten wird anhand der Kriechlebensdauer und ausgewählter Kriechkurven und Kennwerte beschrieben und vergleichend bewertet. Der Einfluss von Defekten und Mikrostruktur auf das Materialverhalten wird anhand von zerstörenden und zerstörungsfreien Auswertungen an ausgewählten Proben analysiert. Der AM-Werkstoff zeigt kürzere Kriechlebensdauern, erreicht das sekundäre Kriechstadium deutlich schneller und bei geringerer Dehnung und weist eine geringere Kriechduktilität im Vergleich zu seinem konventionellen Gegenstück auf. Das Kriechschädigungsverhalten des AM-Werkstoffs ist eher mikrostruktur- als defektgesteuert und ist durch die Bildung intergranularer Kriechrisse gekennzeichnet. Als kritische Merkmale werden die Versetzungsdichte sowie die Versprödung der Korngrenzen identifiziert. Die Mikro-Computertomographie (µCT) erweist sich als Alternative zur Metallographie, um die Kriechschädigung zu analysieren. T2 - Sitzung des DGM-Arbeitskreises Mechanisches Werkstoffverhalten bei hoher Temperatur CY - Online meeting DA - 07.10.2020 KW - 316L KW - Kriechen KW - Additive Fertigung KW - Mikrostruktur KW - Mikro-Computertomographie PY - 2020 AN - OPUS4-51824 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abel, Andreas A1 - Rosalie, Julian A1 - Reinsch, Stefan A1 - Zapala, Pawel A1 - Michels, Heiner A1 - Skrotzki, Birgit T1 - Influence of Mo and B additions in intermetallic near-Fe3Al alloys on microstructure and mechanical properties N2 - Iron aluminides, already reported in the late 19th century, did not cease to attract the interest of scientists and engineers ever since. Besides good oxidation resistance, low density and resource availability, potentials for hightemperature strengths that compete with high-alloy steels were unlocked by low alloy contents. Still, research on alloy design continues, as alloying usually comes at the price of brittleness in low-temperature regimes. A potential candidate is the quinary Fe–Al–Mo–Ti–B system which is strengthened by solid solution and eutectic borides. It was shown to have good strength and outstanding creep resistance under compressive loading up to elevated temperatures. Although the individual effect of alloy additions is well understood in iron aluminides, little is known about the combined effects of alloying concentrations on microstructure, phase stability and mechanical properties. Therefore a systematic study of two Ti-doped near-Fe3Al alloys with varying contents of Mo (2–4 at.%) and B (0.5–1 at.%) was conducted. In total eight different alloys were fabricated by investment casting into ceramic shell molds. Alloys were characterized and compared by grain size, phase transitions, microstructure evolution as well as elemental compositions and volume fractions of phases. For mechanical characterization, macrohardness and microhardness tests as well as tensile tests at ambient and high tempera tures were conducted. Independent of alloy additions, alloys with 24–25 at.% Al exhibit superior proof strength due to a higher matrix hardness. Decreasing B content generally decreases strength by lower secondary phase fractions which contribute via particle hardening. Reducing Mo content decreases both the solute concentration in the matrix and secondary phase fractions. Surprisingly, strength is similar or even superior to alloys with higher Mo content. Strength relations are discussed with a focus on solid-solution hardening theory and other competing strengthening mechanisms. KW - Materials Chemistry KW - Metals and Alloys KW - Mechanical Engineering KW - Mechanics of Materials KW - General Chemistry PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-585284 DO - https://doi.org/10.1016/j.intermet.2023.108074 VL - 163 SP - 1 EP - 11 PB - Elsevier Ltd. AN - OPUS4-58528 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Skrotzki, Birgit A1 - Czichos, Horst ED - Hennecke, Manfred ED - Skrotzki, Birgit T1 - Die Werkstoffklassen N2 - Es werden die vier Werkstoffklassen Metalle, Keramiken, Polymere und Verbundwerkstoffe sowie ihre Untergruppen vorgestellt. Die metallischen Werkstoffe umfassen die Eisen- wie die Nichteisenwerkstoffe und ihre Legierungen. Neben den Ingenieurkeramiken werden auch Glas und Glaskeramik, Naturstoffe und Erdstoffe sowie Baustoffe behandelt. KW - Metall KW - Keramik KW - Glas KW - Polymer KW - Verbundwerkstoff PY - 2020 SN - 978-3-662-57492-8 DO - https://doi.org/10.1007/978-3-662-57492-8_28-1 SP - 1 EP - 35 PB - Springer-Verlag GmbH Deutschland CY - Berlin, Heidelberg ET - 35. AN - OPUS4-50297 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bhadeliya, Ashok T1 - High temperature fatigue crack growth in nickel-based alloys joined by brazing and additive manufacturing N2 - 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. T2 - FEMS EUROMAT 2023 CY - Frankfurt a. M., Germany DA - 03.09.2023 KW - Fatigue crack growth KW - Joined nickel-based alloys PY - 2023 AN - OPUS4-58266 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana T1 - Separation of the impact of residual stress and microstructure on the fatigue performance of LPBF Ti-6Al-4V at elevated temperature (Keynote) N2 - Ti-6Al-4V alloy is intensively used in the aerospace industry because of its high specific strength. However, the application of Laser Powder Bed Fusion (LPBF) Ti-6Al-4V alloy for structurally critical load-bearing components is limited. One of the main limiting factors affecting the structural integrity, are manufacturing defects. Additionally, the high cooling rates associated with LPBF process result in the formation of large residual stress (RS) with complex fields. Such RS can cause cracking and geometrical distortions of the part even right after production. Also, the microstructure of LPBF Ti-6Al-4V in the as-built condition is significantly different from that of the conventionally produced alloy. All these factors affect the mechanical behavior of the material. Therefore, to improve the material performance it is important to evaluate the individual effect of RS, defects, and microstructure on fatigue life. To this aim Ti-6Al-4V LPBF material in as-built condition and subjected to different post-processing, including two heat treatments (for stress relief and microstructural modification) and Hot Isostatic Pressing (HIP, for densification), were investigated. Prior to fatigue tests at elevated temperature, the microstructure, the mesostructure, and subsurface RS on the fatigue samples were investigated. It was found that the fatigue performance of HIPped samples is similar to that of conventionally produced Ti-6Al-4V. The tensile RS found at the surface of as-built samples decreased the fatigue life compared to heat-treated samples. Additionally, the modification of the microstructure (by heat treatment) did not affect the fatigue performance in the regime of mostly elastic strain. This shows that in the absence of tensile RS the manufacturing defects solely control the failure of LPBF components and densification has the strongest effect on the improvement of the mechanical performance. T2 - EUROMAT 2021 CY - Online meeting DA - 12.09.2021 KW - Additive manufacturing KW - Ti-6Al-4V KW - Residual stress KW - Fatigue performance PY - 2021 AN - OPUS4-53278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Reaction sintering and sintering additives for cost-effective production of thermoelectric oxides N2 - Thermoelectric oxides attract much interest recently. Although their thermoelectric properties are inferior to non-oxides, they exhibit distinct advantages. Thermoelectric oxides are stable in air at higher temperatures, their raw materials are less toxic, and more abundant. To enhance attractivity of these materials for industrial applications, production costs need to be reduced. Conventionally, the legs of thermoelectric generators are sintered from green bodies of previously synthesized powder. Reaction-sintering is a fabrication method without a powder synthesis step, as the final phase is formed during the sintering from a raw material mixture. Moreover, the reduction of chemical potential during reaction-sintering is effective as an additional driving force for sintering. We show that reaction-sintering increases the densification of CaMnO3 (n-type, Sm doped). Consequently, the electrical conductivities improved by about 100 % leading to superior power factors (PF = 230 µW/mK² for CaMnO3). Another approach to reduce the production costs is to lower the sintering temperature by adding sinter additives. The addition of 4 wt% CuO to CaMnO3 lowers the sinter temperature from 1250 °C to 1050 °C. The achieved power factor PF = 264 µW/mK is more than two times higher as reported in literature for the same dopant. T2 - Virtual Conference on Thermoelectrics (VCT) CY - Online meeting DA - 21.07.2020 KW - Thermoelectrics KW - Reaction sintering KW - Sintering additives KW - Calcium manganate KW - Calcium cobaltite PY - 2020 AN - OPUS4-51070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul A1 - Mieller, Björn A1 - Rabe, Torsten A1 - Markötter, Henning ED - Petzow, G. ED - Mücklich, F. T1 - Machine learning assisted characterization of a Low Temperature Cofired Ceramic (LTCC) module measured by synchrotron computed tomography N2 - The 5G technology promises real time data transmission for industrial processes, autonomous driving, virtual and augmented reality, E-health applications and many more. The Low Temperature Co-fired Ceramics (LTCC) technology is well suited for the manufacturing of microelectronic components for such applications. Still, improvement of the technology such as further miniaturization is required. This study focuses on the characterization of inner metallization of LTCC multilayer modules, especially on the vertical interconnect access (VIA). Critical considerations for this characterization are delamination, pore clustering in and at the edge of the VIA, deformation, and stacking offset. A LTCC multilayer consisting of a glassy crystalline matrix with silver based VIAs was investigated by synchrotron x-ray tomography (CT). The aim of this study is to propose a multitude of structural characteristic values to maximize the information gained from the available dataset. Data analysis has been done with the open source software ImageJ as well as several additional plugins. The high-resolution CT data was evaluated through 2D slices for accessibility reasons. The segmentation of all 2000 slices to assess the different regions e.g. pores, silver and glass ceramic was done by a supervised machine learning algorithm. A quantitative evaluation of shape, deformation, and porosity of the VIA with respect to its dimensions is presented and the suitability of the characterization approach is assessed. T2 - 54. Metallographie Taagung CY - Online meeting DA - 16.09.2020 KW - Machine Learning KW - LTCC KW - Synchrotron Tomography PY - 2020 SN - 978-3-88355-422-8 VL - 54 SP - 136 EP - 141 PB - Deutsche Gesellschaft für Materialkunde e.V CY - Sankt Augustin AN - OPUS4-51298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas T1 - Evolution of CFRP stress cracks observed by in situ X-ray refractive imaging N2 - Modern air-liners and rotor blades of wind turbines are basically made of fiber reinforced plastics (FRP). Their failure heavily impairs the serviceability and the operational safety. Consequently, knowledge of the failure behavior under static and cyclic loads is of great interest to estimate the operational strength and to compare the performance of different materials. Ideally, the damage evolution under operational load is determined with in-situ non-destructive testing techniques. Here, we report on in-situ synchrotron X-ray imaging of tensile stress induced cracks in carbon fiber reinforced plastics (CFRP) due to inter fiber failure. An in-house designed compact-tensile testing machine with a load range up to 15 kN was integrated into the beam path. Since conventional radiographs do not reveal sufficient contrast to distinct cracks due to inter fiber failure and micro cracking from fiber bundles, the Diffraction Enhanced Imaging technique (DEI) is applied in order to separate primary and scattered (refracted) radiation by means of an analyzer crystal. In the laboratory, scanning X-ray refraction topography of CFRP has been applied long before but it comes along with several disadvantages: the long total measuring time hampers real time (in-situ) measurements and the required small beam size hinders end-to-end imaging. The introduced technique overcomes both drawbacks. Imaging and tensile test rig are run unsynchronized at the greatest possible frame rate (0.7 s-1 at 28.8 µm pixel size) and smallest possible strain rate (5.5∙10-4 s-1). For 0°/90° non-crimped fabrics (ncf) the first inter fiber cracks occurred at 380 MPa (strain 0.7 %). Prior to failure at about 760 MPa (strain 2.0 %) we observe the evolution of a nearly equidistant 1 mm grid of cracks running across the entire sample in the fully damaged state before total failure. T2 - 41st Risø International Symposium on Materials Science - Materials and Design for Next Generation Wind Turbine Blades CY - Online meeting DA - 07.09.2020 KW - X-ray refraction KW - Diffraction Enhanced Imaging KW - Carbon Fiber Reinforced Plastics KW - In situ tensile test KW - Crack evolution PY - 2020 AN - OPUS4-51223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana T1 - Influence of residual stress and microstructure on mechanical performance of LPBF TI-6AL-4V N2 - Ti-6Al-4V alloy is intensively used in the aerospace industry because of its high specific strength. However, the application of Laser Powder Bed Fusion (LPBF) Ti-6Al-4V alloy for structurally critical load-bearing components is limited. One of the main limiting factors affecting the structural integrity, are manufacturing defects. Additionally, the high cooling rates associated with LPBF process result in the formation of large residual stress (RS) with complex fields. Such RS can cause cracking and geometrical distortions of the part even right after production. Also, the microstructure of LPBF Ti-6Al-4V in the as-built condition is significantly different from that of the conventionally produced alloy. All these factors affect the mechanical behavior of the material. Therefore, to improve the material performance it is important to evaluate the individual effect of RS, defects, and microstructure on fatigue life. To this aim Ti-6Al-4V LPBF material in as-built condition and subjected to different post-processing, including two heat treatments (for stress relief and microstructural modification) and Hot Isostatic Pressing (HIP, for densification), were investigated. Prior to Low Cycle Fatigue (LCF) tests at operating temperature (300°C), the microstructure (phases, crystallographic texture, and grain morphology), the mesostructure (defect shape and distribution), and subsurface RS on the LCF samples were investigated. It was found that the fatigue performance of HIPped samples is similar to that of conventionally produced Ti-6Al-4V. The tensile RS found at the surface of as-built samples decreased the fatigue life compared to heat-treated samples. Additionally, the modification of the microstructure (by heat treatment) did not affect the fatigue performance in the regime of mostly elastic strain. This shows that in the absence of tensile RS the manufacturing defects solely control the failure of LPBF components and densification has the strongest effect on the improvement of the mechanical performance. T2 - ASTM ICAM 2020 CY - Online meeting DA - 16.11.2020 KW - Additive manufacturing KW - Ti-6Al-4V KW - Computed tomography KW - Residual stress PY - 2020 AN - OPUS4-51695 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas T1 - Evolution of CFRP stress cracks observed by in situ X-ray refractive imaging N2 - Modern air-liners and wind turbine rotor blades are made up primarily of fiber reinforced plastics. Failure of these materials heavily impairs the serviceability and the operational safety. Consequently, knowledge of the failure behavior under static and cyclic loads is of great interest to estimate the operational strength and to compare the performance of different materials. Ideally, the damage evolution under operational load is determined with in-situ non-destructive testing techniques. Here, we report in-situ synchrotron X-ray imaging of tensile stress induced cracks in carbon fiber reinforced plastics due to inter-fiber failure. An inhouse designed compact tensile testing machine with a load range up to 15 kN was integrated into the beamline. Since conventional radiographs do not reveal sufficient contrast to distinguish cracks due to inter-fiber failure and micro cracking from fiber bundles, the Diffraction Enhanced Imaging (DEI) technique is applied in order to separate primary and scattered (refracted) radiation by means of an analyzer crystal. This technique allows fast measurements over large fields-of-view and is ideal for in-situ investigations. T2 - 12th BESSY@HZB User Meeting 2020 CY - Online meeting DA - 10.12.2020 KW - Carbon Fiber Reinforced Plastics KW - Crack evolution KW - Diffraction Enhanced Imaging KW - In situ tensile test KW - X-ray refraction PY - 2020 AN - OPUS4-51802 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Improved thermoelectric properties of CaMnO3 and Ca3Co4O9 by increasing the driving force for sintering N2 - Thermoelectric materials can convert waste heat directly into electrical power by utilizing the Seebeck effect. Calcium cobaltite (Ca3Co4O9, p-type) and calcium manganate (CaMnO3, n-type) are two of the most promising oxide thermoelectric materials. The performance of these materials is evaluated by the power factor PF = S²∙σ and the figure of merit ZT = (PF ∙ T) / κ, demanding high Seebeck coefficient S, high electrical conductivity σ and low thermal conductivity κ. The latter two are increasing with increasing relative sinter density. According to theory, the relative density of ceramics can be improved by increasing the driving force for sintering. This study investigates different approaches to increase the driving force for sintering of Ca3Co4O9 and CaMnO3 to improve densities and thermoelectric properties. The following approaches were applied: minimizing the energy input during powder synthesis by calcination, fine milling of the powder, using reaction-sintering without a powder synthesis step, and adding a transient liquid phase by sinter additives. All different approaches led to an increased densification and thus higher electrical conductivity and higher PF. Thermal conductivity increased as well but not to the same extent. E.g. reaction-sintering increased the densification of Ca3Co4O9 (p-type) and CaMnO3 (n-type). Consequently, the electrical conductivities improved by about 100 % for both oxides leading to superior power factors (PF = 230 µW/mK² for CaMnO3). Although the thermal conductivity increased as well by 8 %, the figures of merit (ZT) were significantly higher compared to conventionally sintered bars. The addition of 4 wt% CuO as a sinter additive to CaMnO3 lowers the sinter temperature from above 1250 °C to below 1100 °C and increases the relative density. Due to the increased density, both electrical conductivity and PF increased by more than 200 % even though the sintering temperature was 150 K lower. T2 - Electroceramics XVII CY - Online meeting DA - 24.08.2020 KW - Thermoelectrics KW - Reaction sintering KW - Sintering additives PY - 2020 AN - OPUS4-51163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Practical breakdown voltage calculations using dielectric breakdown strength reference values N2 - Dielectric breakdown is a catastrophic failure of ceramic substrates and insulators. The use of dielectric breakdown strength (DBS) reference values for the dimensioning of such components is not straightforward, as the DBS depends on sample thickness and electrode area. This fact also hampers a valid comparison of data taken from different literature sources. Based on the empirically confirmed proportionality of DBS to the reciprocal square root of sample thickness and an approach to account for the influence of electrode area on the failure probability, a practical equation is derived to calculate the breakdown voltage for arbitrary sample thickness and electrode area from one set of DBS reference data. To validate the equation, the AC DBS of commercial alumina substrates with thicknesses ranging from 0.3 mm to 1.0 mm was performed using different printed electrodes with varying areas. The breakdown voltages comprise a range from 18 kV for thick samples to 8.5 kV for thin samples, resulting in DBS values from 17 kV/mm for 1.0 mm thick samples to 29 kV/mm for 0.3 mm thin samples, all made from the same material. The influence of electrode area is comparatively smaller. The results calculated with the proposed equation are in reasonable accordance with the measured data. Thus, the equation can be applied for a proper comparison of literature DBS data measured in different setups and for a reasonable estimation of breakdown voltages in DBS tests and applications based on reference data. T2 - Electroceramics Conference XVII CY - Online meeting DA - 24.08.2020 KW - Ceramics KW - Dielectric breakdown KW - Weibull distribution PY - 2020 AN - OPUS4-51151 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Machine learning assisted characterization of a Low Temperature Co-fired Ceramic (LTCC) module measured by synchrotron computed tomography. N2 - The 5G technology promises real time data transmission for industrial processes, autonomous driving, virtual and augmented reality, E-health applications and many more. The Low Temperature Co-fired Ceramics (LTCC) technology is well suited for the manufacturing of microelectronic components for such applications. Still, improvement of the technology such as further miniaturization is required. This study focuses on the characterization of inner metallization of LTCC multilayer modules, especially on the vertical interconnect access (VIA). Critical considerations for this characterization are delamination, pore clustering in and at the edge of the VIA, deformation, and stacking offset. A LTCC multilayer consisting of a glassy crystalline matrix with silver based VIAs was investigated by synchrotron x-ray tomography (CT). The aim of this study is to propose a multitude of structural characteristic values to maximize the information gained from the available dataset. Data analysis has been done with the open source software ImageJ as well as several additional plugins. The high-resolution CT data was evaluated through 2D slices for accessibility reasons. The segmentation of all 2000 slices to assess the different regions e.g. pores, silver and glass ceramic was done by a supervised machine learning algorithm. A quantitative evaluation of shape, deformation, and porosity of the VIA with respect to its dimensions is presented and the suitability of the characterization approach is assessed. T2 - 54. Metallographie Tagung CY - Online meeting DA - 16.09.2020 KW - Machine Learning KW - LTCC KW - Synchrotron Tomography PY - 2020 AN - OPUS4-51299 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas A1 - Trappe, Volker A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Rissentwicklung in CFK-Laminaten nachgewiesen durch in situ Röntgen-Refraktion N2 - 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. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Röntgen-Refraktion KW - Synchrotronstrahlung KW - CFK KW - Rissentwicklung PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576230 SN - 978-3-947971-29-9 VL - BB 180 SP - 1 EP - 8 AN - OPUS4-57623 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Mieller, Björn A1 - Maiwald, Michael A1 - Kipphardt, Heinrich A1 - Tuma, Dirk A1 - Prager, Jens A1 - Schukar, Marcus A1 - Strohhäcker, J. T1 - Sensoren und Analytik für Sicherheit und Prozesskontrolle in Wasserstofftechnologien N2 - Die Nutzung von Sensortechnologien, insbesondere im Bereich der Gasdetektion mit einem Schwerpunkt auf Wasserstoff, spielt eine entscheidende Rolle in verschiedenen Anwendungsbereichen der Wasserstofftechnologie. Sicherheitsüberwachung, Leckdetektion und Prozesskontrolle gehören zu den prominenten Anwendungsgebieten dieser Sensortechnologien. Ein zentrales Ziel ist die Erkennung von freigesetztem Wasserstoff sowie die genaue Bestimmung des Wasserstoff-Luftverhältnisses mithilfe von Gassensoren. Dies ist von entscheidender Bedeutung, um potenzielle Gefahren frühzeitig zu erkennen und angemessene Maßnahmen zu ergreifen. Ein weiterer Schwerpunkt dieses Beitrags liegt auf der Analytik und der Verwendung zertifizierter Referenzmaterialien in Verbindung mit Metrologie für die Wasserstoffspeicherung. Dies gewährleistet eine präzise und zuverlässige Charakterisierung von Wasserstoff und unterstützt die Entwicklung sicherer Speichertechnologien. Im Rahmen des Euramet-Vorhabens Metrology for Advanced Hydrogen Storage Solutions (MefHySto) wird eine Kurzvorstellung präsentiert. Der Vortrag stellt zwei zerstörungsfreie Prüfverfahren zum strukturellen Zustandsüberwachung (Structural Health Monitoring, SHM) für Wasserstofftechnologien vor. Insbesondere die Fehlstellenerkennung mittels geführter Ultraschallwellen spielt eine bedeutende Rolle bei der Lebensdauerüberwachung von Wasserstoffspeichern. Ein weiterer Aspekt ist die Anwendung faseroptischer Sensorik zur Schadensfrüherkennung von Wasserstoffspeichern. Diese zerstörungsfreien Prüfverfahren ermöglichen eine präzise und frühzeitige Identifizierung von Schäden, was die Sicherheit und Effizienz von Wasserstoffspeichersystemen entscheidend verbessert. T2 - DVGW Kongress H2 Sicherheit CY - Online meeting DA - 15.11.2023 KW - H2Safety@BAM KW - Gassensorik KW - Metrologie KW - zertifizierte Referenzmaterialien KW - Zerstörungsfreie Prüfung KW - Ultraschall KW - Faseroptik PY - 2023 AN - OPUS4-59230 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eddah, Mustapha T1 - Synchrotron Multi-energy HDR tomography for LTCC systems N2 - 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. T2 - Bessy II User Meeting CY - Berlin, Germany DA - 22.06.2023 KW - LTCC KW - Synchrotron tomography KW - Data fusion KW - In-situ tomography PY - 2023 AN - OPUS4-57795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Texturing of calcium cobaltite for thermoelectric applications by pressure assisted sintering N2 - Thermoelectric materials can convert waste heat directly into electrical power by using the Seebeck effect. Calcium cobaltite (CCO) is considered as a promising thermoelectric p-type oxide for energy harvesting applications at temperatures above 500 °C. The properties and morphology of single-crystal CCO are strongly anisotropic because of its crystal structure of alternating layers of CoO2 and Ca2CoO3. By aligning the plate-like grains, the anisotropic properties of the grains can be assigned to the poly-crystalline parts. In this study, the combination of tape casting and pressure-assisted sintering is used to texture and densify large scale components (50 cm²). Thereby, the influence of powder preparation and applied pressure during sintering on texturing and thermoelectric properties is investigated. The analysis of XRD pole figures revealed that tape casting already leads to highly textured CCO. By pressure variation during sintering, the microstructure of CCO can be tailored either toward maximum power factor as required for energy harvesting or toward maximum figure of merit as required for energy recovery. Low pressure lead to a porous microstructure and maximum figure of merit and higher pressure to full densification and maximum power factor. The electrical and thermal conductivity of CCO seem depending on both texture and sinter density. T2 - KERAMIK 2021 / CERAMICS 2021 CY - Online meeting DA - 19.04.2021 KW - Thermoelectrics KW - Hot pressing KW - Pole figures PY - 2021 AN - OPUS4-52490 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Thermoelectric multilayer generators: development from oxide powder to demonstrator N2 - Thermoelectric generators can be used for energy harvesting by directly transforming a temperature gradient into a voltage. Multilayer generators based on ceramic multilayer technology are an interesting alternative to conventional π-type generators. They exhibit several advantages like high filling factor, possibility of texturing, co-firing of all materials in one single-step, and reduction of production costs due to the high possible degree of automation. But, co-firing of promising oxide thermoelectric materials, Ca3Co4O9 (p-type) and CaMnO3 (n-type), is very challenging due to the large difference in sintering temperature (300 K). In this work we show the material development of Ca3Co4O9, CaMnO3, and insulation for multilayer generators co-fired under uniaxial pressure at 900 °C. The materials are tailored regarding their sintering behavior, electrical performance and coefficients of thermal expansion. Tape-casting and pressure assisted sintering are applied to fabricate textured Ca3Co4O9. Compared to conventional sintering, pressure assisted sintering increases the strength by the factor 10 and the power factor by the factor of 20. The combination of sintering additives and uniaxial pressure is used to decrease the sintering temperature of CaMnO3 to 900 °C while maintaining acceptable thermoelectric properties. Different generator designs (unileg and pn-type) were fabricated and analyzed regarding microstructure and thermoelectric performance. A lower level of complexity is beneficial for co-firing and performance. The unileg demonstrators reach 80% of the simulated output power and the power output is highly reproducible between the different demonstrators (99%). T2 - Ceramics in Europe 2022 CY - Krakow, Poland DA - 10.07.2022 KW - Thermoelectrics KW - Multilayer technology KW - Co-firing KW - Texture PY - 2022 AN - OPUS4-55357 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Miliūtė, Aistė ED - Bustamante, Joana ED - Karafiludis, Stephanos ED - Zöllner, Moritz ED - Eddah, Mustapha ED - Emmerling, Franziska ED - Mieller, Björn ED - George, Janine ED - Stawski, Tomasz T1 - Synthesis and phase purity of the negative thermal expansion material ZrV2O7 N2 - Synthesis of pure, homogeneous, and reproducible materials is key for the comprehensive understanding, design, and tailoring of material properties. In this study, we focus on the synthesis of ZrV2O7, a material known for its negative thermal expansion properties. We investigate the influence of solid-state and wet chemistry synthesis methods on the purity and homogeneity of ZrV2O7 samples. Our findings indicate that different synthesis methods significantly impact the material's characteristics. The solid-state reaction provided high-purity material through extended milling time and repeated calcination cycles, while the sol-gel reaction enabled a “near-atomic” level of mixing and, therefore, homogenous phase-pure ZrV2O7. We confirmed purity via X-ray diffraction and Raman spectroscopy, highlighting differences between phase-pure and multiphase ceramics. These analytical techniques allowed us to distinguish subtle differences in the structure of the material. Based on ab initio simulated phonon data, we were able to interpret the Raman spectra and visualise Raman active atom vibrations. We show that phase purity enables the unbiased characterisation of material properties such as negative thermal expansion. KW - NTE KW - Sol-gel KW - Solid-state KW - Ab-initio KW - XRD KW - Raman PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613643 DO - https://doi.org/10.26434/chemrxiv-2024-d4sj9 SN - 2573-2293 VL - 2024 SP - 1 EP - 60 PB - American Chemical Society CY - Washington, D.C. AN - OPUS4-61364 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie T1 - Thin-film capability of commercial LTCC N2 - 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. T2 - XVIII EcerS Conference & Exhibition CY - Lyon, France DA - 02.07.2023 KW - Glass-ceramics KW - Etching KW - Resistance PY - 2023 AN - OPUS4-58019 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė T1 - Structural evolution of ZrV2O7: supercell persistence revealing local and global structure duality N2 - In the AM2O7 family of negative thermal expansion materials (NTE), evidence of supercell at room temperature was reported following the Völlenke et al. discovery of missed superlattice due to the apparent linearity of the M-O-M bond in GeP2O7. Korthuis et al. and Khosrovani et al. demonstrated it to be true for cubic ZrV2O7 as well. It was concluded that at room temperature, the structure consists of 27 'subcells' with bent M2O7 groups that appear to form a linear configuration due to refinement of averaged position. However, around 100 °C, the transition to the “parent” cell was reported, where the cell volume increases, and the M-O-M angles are constrained by the Pa-3 space group symmetry to be 180°. We followed structural changes in the ZrV2O7 at high temperatures to demonstrate partial disorder within the crystal, local and global structural duality and supercell persistence at high temperatures. Total scattering measurements and Pair Distribution Function (PDF) analysis revealed that the experimental pattern cannot be fitted with the “parent structure” model, and only the 3×3×3 supercell model can correspond to local and global structures throughout the full 25-700 °C temperature range. We also show how short and long-range order within the crystal changes when approaching the phase transition, which might indicate the existence of coherent structural domains that evolve between order and disorder with increasing temperature. We further hypothesize how this can be related to the negative thermal expansion mechanism and the interpretation of structure solutions presenting data from high-temperature X-ray absorption fine structure (XAFS) and Transmission Electron Microscopy (TEM) measurements. T2 - 5th International Symposium on Negative Thermal Expansion and Related Materials (ISNTE-5) CY - Porto, Portugal DA - 29.07.2025 KW - NTE KW - Ab initio KW - PDF KW - CSM PY - 2025 AN - OPUS4-63874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė T1 - Theoretical and experimental development of negative thermal expansion material ZrV2O7 N2 - Zirconium vanadate (ZrV2O7) is a well-known negative thermal expansion (NTE) material which stands out for its remarkable isotropic unit cell contraction over a broad temperature range (130°C < T < 800°C). This enables the fabrication of composites where the overall expansion coefficient can be tailored to a specific negative, positive, or neutral value. Consequently, such composite materials are attractive for many device applications because they can compensate for damage caused by thermal expansion. They are relevant to optical systems, electronic and biomedical applications. In this study, we implement ab-initio-based vibrational computations with partially treated anharmonicity (quasi-harmonic approximation (QHA), temperature-dependent effective harmonic potentials (TDEP)[5]) 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. In analytical techniques that can provide structural information such as pair distribution function analysis (PDF), X-ray diffraction (XRD), and Extended X-ray Absorption Fine Structure (EXAFS), molecules and atoms are fit geometrically without consideration of atom interactions. Therefore, in combination with these methods, we also consider potential energy surfaces and conclude what structures are likely to form energetically in the full NTE temperature range, in addition to fitting experimental data geometrically. We also optimise experimentally fitted structures to their lowest energy configurations and re-generate comparative data to observe what differences would be visible experimentally. T2 - XLVIII International Congress of Theoretical Chemists of Latin Expression CY - Cartagena de Indias, Colombia DA - 13.07.2025 KW - NTE KW - Ab initio KW - QHA KW - TDEP KW - anharmonicity PY - 2025 AN - OPUS4-63873 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miliūtė, Aistė T1 - How experimental and computational methods allow us to design negative thermal expansion materials N2 - Combined experimental and computational methods allow comprehensive understanding, design, and tailoring of material properties. We focus on a well-known negative thermal expansion (NTE) material, zirconium vanadate (ZrV2O7), and address synthesis, characterisation and validation of results with computational simulations. Experimental and computational X-ray diffraction and Raman spectroscopy data highlighted differences between phase-pure and multiphase ceramics. These techniques allowed us to distinguish subtle differences in the structure of the material. Based on ab initio simulated phonon data, unaffected by impurities or instrumental errors, we could interpret the Raman spectra and visualise Raman active atom vibrations. These computational models allowed better insight and further experimental improvement while high-quality experimental data granted the validation and improvement of computational simulation strategy. T2 - Application of Neutrons and Synchrotron Radiation in Engineering Materials Science CY - Hamburg, Germany DA - 23.03.2025 KW - NTE KW - Sol-gel KW - Ab initio KW - Raman KW - XRD PY - 2025 AN - OPUS4-62832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -