TY - CONF A1 - Schröder, Jakob T1 - The heat treatment of L-PBF Inconel 718: A manyfold problem N2 - The interest to additively manufacture Nickel-based superalloys has substantially grown within the past decade both academically and industrially. More specifically, additive manufacturing processes such as laser powder bed fusion (LPBF) offer the ability to produce dense parts within a single manufacturing step. In fact, the exceptional freedom in design associated with the layer-based nature of the processes is of particular interest for the complex shapes typically required in turbine applications. In certain cases, the overall part performance can be achieved by tailoring the microstructure and the crystallographic texture to the specific application. However, these advantages must be paid at a price: the large local temperature gradients associated with the rapid melting and solidification produce parts that inherently contain large residual stress in the as-manufactured state. In addition, the presence of pores in the final part may further affect the in-service part failure. As among Nickel-based alloys Inconel 718 exhibits excellent weldability, this alloy has been widely studied in open research in the domain of LPBF. However, significant microsegregation of the heavier alloying elements such as Niobium and Molybdenum accompanied by dislocation entanglements may preclude the application of conventional heat treatment schedules. Therefore, different post processing heat treatments are required for laser powder bed fused Inconel 718 as compared to conventional variants of the same alloy. In this study, we investigated two different heat treatment routes for LPBF Inconel 718. In a first routine, the samples were stress relieved and subsequently subjected to hot isostatic pressing (HIP) followed by a solution heat treatment and a two-step age (referred to as FHT). In a second routine, the samples were subjected to a single-step direct age post stress relieving heat treatment (referred to DA). We investigated the consequences of such heat treatment schedules on the microstructure, texture, and mechanical behavior. We show that by applying a DA heat treatment the typical columnar microstructure possessing a crystallographic texture is retained, while an equiaxed untextured microstructure prevails in case of an FHT heat treatment. We further evaluate how these heat treatments affect the mechanical behaviour on the macroscopic and microscopic scale. T2 - 4th European Symposium on Superalloys and their Applications EuroSuperalloys 2022 CY - Bamberg, Germany DA - 18.09.2022 KW - Electron Backscatter Diffraction KW - Additive Manufacturing KW - Laser Powder Bed Fusion KW - Mechanical Behavior KW - Heat Treatment KW - X-Ray Diffraction PY - 2022 AN - OPUS4-55811 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sonnenburg, Elke T1 - Präparation, Kontrastierung und Darstellung des Gefüges von additiv gefertigtem austenitischem Stahl 316L N2 - Der weit verbreitete austenitische Stahl 316L soll auch mittels additiver Fertigung verarbeitet werden (316L-AM). Zur Entwicklung optimaler Aufbauverfahren ist ein detailliertes Verständnis des Gefüges notwendig. Das additiv aufgebaute Gefüge zeigt eine Mikrostruktur, die geprägt ist von sehr hohen Abkühlraten und gerichtetem Kornwachstum. Mittels klassischer Metallographie können die Charakteristika des Gefüges wie Körner, Subkörner und Schmelzlinien sichtbar gemacht werden. Mittels EBSD werden Kristallorientierungen ermittelt und bildhaft aufbereitet. Die Feinstruktur der Körner wird im REM in der Übersicht aufgelöst. Erst im TEM kann bei hoher Vergrößerung die Natur der Zellstruktur quantitativ ermittelt werden. T2 - Metallographie 2020 CY - Online meeting DA - 16.09.2020 KW - Präparation KW - Kontrastierung KW - Additiv gefertigter Stahl PY - 2020 AN - OPUS4-51244 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wojciak, K. A1 - Tokarski, T. A1 - Cios, G. A1 - Nolze, Gert T1 - Precision and accuracy during standard-less mapping of local lattice distortions using ebsd and calm technique N2 - Electron Back Scatter Diffraction (EBSD) is a very versatile analytical technique allowing for the characterization of material structure. Historically, diffraction images (Kikuchi patterns) registered during EBSD analysis were solved using Hough/Radon transformation. The last decade brought several novel techniques of experimental pattern analysis, focusing entirely on image analysis routines such as pattern matching, or various variants of High-Resolution EBSD. However, all the above-mentioned techniques require prior knowledge of the material structure to perform orientation analysis. The recently presented algorithm employed in Crystallographic Analysis of Lattice Metric (CALM) software, effectively removes this limitation enabling a standard-less analytical approach in EBSD systems. At its core, the CALM technique couples accurate detection of the Kikuchi bands position, with a rigid construction of reciprocal lattice resulting from translational crystal symmetry. A unique characteristic of the methodology also gives an opportunity for application in the analysis of continuous lattice changes, for example tetragonality mapping. During mapping, however, the geometry of the gnomonic projection (represented by the projection center) is continuously altered decreasing overall algorithm efficiency. The work presents an analysis of the projection center in terms of precision and accuracy. T2 - Oxford User Meeting 2024 CY - Krakow, Poland DA - 14.05.2024 KW - EBSD KW - Kikuchi KW - Lattice parameters KW - Ratio refinement PY - 2024 AN - OPUS4-60087 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wehmann, N. T1 - Non classical nucleation in calcium sulfates Insights from the hyper arid Atacama Desert N2 - Gypsum (CaSO4∙2H2O) and anhydrite (CaSO4) are among the dominant evaporite minerals in the Atacama Desert [1]. They are distributed ubiquitously, and play a key role in local landscape evolution. The formation mechanism of especially anhydrite has been a matter of scientific debate for more than a century [2]. To date, there exists no model that can reliably predict anhydrite formation at earth’s surface conditions. While thermodynamics favor its formation [3], it is hardly achieved on laboratory time scales at conditions fitting the Atacama Desert. Long induction times for nucleation have recently been modeled by Ossorio et al. [4]. However, anhydrite can be readily found in the Atacama Desert. Recently, the mineral was synthesized in flow-through reactors as a byproduct of K-jarosite dissolution at high water activity (aw=0.98) and room temperature [5], even-though the thermodynamic stability field begins only under a value of ~0.8. Additionally, recent studies investigated the nano-structure of various calcium-sulfates, which advocate for highly non-classical crystallization behavior [6]. The specific roles of particulates, ionic or organic reagents working as catalysts for the non-classical crystallization pathway remain to be determined. Here, we present recent results from flow-through experiments as well as analyses of anhydrite samples from the Atacama Desert. Flow-through experiments were performed to systematically explore the domains of flow rate, composition, ionic-strengths and starting materials. Neither primary, nor secondary anhydrite was produced in any of these experiments. Analyses on Atacama samples reveal the existence of at least three distinct anhydrite facies, with differing mineralogy and micro- to nano-structures. The facies are (1) aeolian deposits with sub-µm grain sizes, (2) (sub-)surface nodules that formed from aeolian deposits and (3) selenites with secondary anhydrite rims. Possible mechanisms of their formation will be discussed. T2 - Goldschmidt2023 CY - Lyon, France DA - 13.07.2023 KW - Gypsum KW - Anhydrite KW - Atacama Desert KW - Local landscape evolution PY - 2023 AN - OPUS4-58988 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bettge, Dirk T1 - Merkmale von alltäglichen Brüchen und wie wir daraus lernen können N2 - Schadensfälle aus dem Alltag erscheinen oft simpel, sind im Detail aber meist komplexer als erwartet und eröffnen die Möglichkeit, Merkmale zu studieren, Aufnahmetechniken und Bildbearbeitung zu optimieren und die Erfahrungen am Ende ohne Restriktionen weiter zu vermitteln. Beispielsweise verändern sich die mikroskopischen Merkmale von Schwingrissen über ihren Verlauf oft deutlich. Dies hängt von der Art des Werkstoffs und von den Beanspruchungsbedingungen ab. Die Bruchmerkmale werden schließlich systematisch dargestellt und ein Datensatz für die Fraktographische online-Datenbank der DVM/DGM AG Fraktographie erstellt, die fachöffentlich einsehbar ist. T2 - Metallographietagung 2024 CY - Berlin, Germany DA - 18.09.2024 KW - Fraktographie KW - Schadensanalyse PY - 2024 AN - OPUS4-61239 LA - deu 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 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. 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 - Adlershofer Forschungsforum 2022 CY - Berlin, Germany DA - 11.11.2022 KW - Lithium Ion Batteries KW - GD-OES KW - FIB KW - SEM KW - EDX PY - 2022 AN - OPUS4-56246 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 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 - Lehmusto, Juho T1 - Initial oxidation of the refractory high-entropy superalloy AlMo0.5NbTa0.5TiZr N2 - In contrast to traditional alloys, which are typically based on a single dominant element, high-entropy alloys (HEAs) consist of five or more principal elements in roughly equal proportions. These complex alloys often exhibit superior characteristics compared to conventional alloys, including enhanced strength and hardness, exceptional wear resistance, high structural stability, and strong resistance to oxidation. Despite these promising characteristics, the vast compositional space of HEAs means that only a limited number have been thoroughly investigated for their mechanical and chemical behavior. One notable example is the refractory high-entropy superalloy AlMo0.5NbTa0.5TiZr, which represents a newly emerging class of materials. This alloy features a nanoscale microstructure composed of B2 and bcc phases, resulting in compressive strength at elevated temperatures that surpasses that of conventional Ni-based superalloys. Such performance offers potential benefits for improving turbine efficiency in aerospace and energy generation applications. However, the alloy’s microstructure is known to be sensitive to annealing. Specifically, its mechanical properties deteriorate when intragranular hexagonal Al-Zr-based intermetallic compounds form, likely due to issues with phase stability. On the other hand, the inclusion of Al has been shown to enhance oxidation resistance. Nevertheless, HEAs are also known to develop pronounced internal aging zones caused by diffusion during oxidation processes. These findings indicate a need for further investigation into the thermodynamic stability of this alloy. In addition, its oxidation behavior—both at the surface and within the material—remains incompletely understood. This ongoing research explores the oxidation behavior of the AlMo0.5NbTa0.5TiZr alloy at temperatures ranging from 800 °C to 1000 °C. The influence of water vapor on the oxidation process is also examined. Ultimately, the goal is to integrate insights into the alloy’s structural, mechanical, and chemical characteristics at high temperatures. T2 - Gordon Research Conference - High Temperature Corrosion CY - New London, United States DA - 16.07.2023 KW - High-Entropy superalloy KW - Phase stability KW - Microstructural evolution KW - Oxidation behavior KW - High-Temperature Performance PY - 2023 AN - OPUS4-63851 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo T1 - In situ electron-beam 'melting' (sublimation) of gold microparticles in the SEM N2 - Gold micro particles have been modified in the past using the high power density of a localized electron beam of acceleration voltages above 100 kV as an energy source to transform matter at the sub-micron scale in a transmission electron microscope uses. Here, the e-beam-induced transformation of precursor microparticles employing a low-energy e-beam with an acceleration voltage of 30 kV in a scanning electron microscope is implemented. Under these conditions, the technique can be classified between e-beam lithography, where the e-beam is used to mill holes in or grow some different material onto a substrate, and e-beam welding, where matter can be welded together when overcoming the melting phase. Modifying gold microparticles on an amorphous SiOx substrate reveals the dominant role of inelastic electron-matter interaction and subsequent localized heating for the observed melting and vaporization of the precursor microparticles under the electron beam. Monte-Carlo scattering simulations and thermodynamic modeling further support the findings. T2 - IKZ International Fellowship Award & Summer School 2025 from May 5 to 7, 2025 CY - Berlin, Germany DA - 05.05.2025 KW - Gold Nanoparticle KW - Scanning Electron Microscopy KW - In situ irradiation KW - Thermodynamic modelling KW - Heat Transfer PY - 2025 AN - OPUS4-63256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bayerlein, Bernd T1 - Focused ion beam techniques beyond the ordinary - Methodological developments within ADVENT N2 - This poster presents the focused ion beam preparation methodologies developed within the framework of the EU funded EURAMET project ADVENT (Advanced Energy-Saving Technology). It summarises the key breakthroughs achieved for various in situ investigation techniques, e.g. in situ experiments at the Synchrotron facility BESSY II (IR-SNOM and XRS), TEM and SMM instrumentation. The created experimental devices from diverse thin-film semiconductor materials paved the way to dynamic structural studies bearing the potential to determine nanoscale correlations between strain and electric fields and, moreover, for the fundamental development of new in situ capabilities. N2 - Dieses Poster zeigt die FIB Präparationstechniquen, die im Rahmen des EU-finanzierten EURAMET-Projekts ADVENT (Advanced Energy Saving Technology) entwickelt wurden. Es fasst die wichtigsten Errungenschaften zusammen, die für verschiedene in situ Untersuchungstechniken erzielt wurden, z.B. situ-Experimente in dem Synchrotronring BESSY II (IR-SNOM und XRS), in situ TEM Experimente und für die SMM Technik. Die experimentellen Probenstrukturen, die aus verschiedenen Dünnschicht-Halbleitermaterialien erzeugt wurden, ebneten den Weg für dynamische Strukturstudien, die das Potenzial haben, nanoskalige Korrelationen zwischen Dehnung und elektrischen Feldern zu bestimmen und darüber hinaus neue in situ Messmethoden zu entwickeln. T2 - Final Meeting CY - Online Meeting DA - 30.06.2020 KW - FIB KW - Sample preparation KW - In situ KW - TEM KW - AFM PY - 2020 AN - OPUS4-51606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -