TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - DELTA - Investigation of corrosion and microbially influenced corrosion processes by means of X-Ray absorption spectroscopy N2 - Alloys relevant for corrosion research are inherently complex in chemical composition and microstructure. Their local surface chemistry differs significantly from the bulk composition and their surfaces are subjected to ever changing environmental conditions. Thus, a thorough understanding of the mechanisms leading to material degradation and failure requires a detailed characterisation of the initial and final states as well as an adequate monitoring of the relevant properties as a function of time. Moreover, corrosion products tend to oxidize in contact with the atmosphere. Microbially influenced corrosion (MIC) poses a particular challenge regarding the experimental methods that can be used for the investigations. The use of highly sensitive methods of ultra-high vacuum surface analysis requires the removal of the biofilm, which leads to significant changes in the interfacial chemistry. In recent projects we applied X-ray absorption near edge spectroscopy (XANES) to investigate mechanisms of aqueous corrosion, high temperature corrosion and MIC processes of stainless steel and multi-principal element alloys (MPEAs). By combining in situ XANES studies on model thin films with ex situ XANES analysis of technical samples we aimed to obtain a holistic understanding of degradation processes. In this presentation we will summarize our results on the application of XANES to corrosion and MIC research with two case studies. In the first case study, in situ and ex situ XANES were used for the investigation of aqueous and high-temperature corrosion processes of alloys from FeNiCr-Mn MPEA family to clarify the role of Mn in determining the corrosion resistance and passive film formation. Our results indicate that Mn plays a major role in suppressing Fe oxidation. In the second example we have shown by means of in situ and ex situ XANES analysis that cultivation of metal reducing bacteria (MRB) in abundance of Fe(III) ions leads to a significant increase in electrochemical activity and thus, to an accelerated corrosion of the metallic substrate. This implies that bacterial colonies released from active corrosion sites might show a preconditioning effect and pose a higher corrosion risk. T2 - eMRS 2024 Spring Meeting CY - Strasbourg, France DA - 27.05.2024 KW - Corrosion KW - XANES KW - MIC KW - Multi-principal element alloys PY - 2024 AN - OPUS4-62636 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - Material Acceleration Platforms of BAM (MAPs@BAM) N2 - Material Acceleration Platforms (MAPs) represent a transformative approach to the development of resilient and sustainable technology value chains. These platforms can identify candidate chemistries and structures via simulations, and database searches and leverage machine learning-based rapid screening to accelerate the discovery and deployment of novel materials, thereby addressing critical challenges in modern technology sectors. Incorporating high-fidelity advanced characterization in the early phases of material development is crucial for early de-risking. Advanced characterization techniques, such as X-ray diffraction, advanced electrochemical and spectroscopic techniques provide comprehensive insights into the structural, chemical, and physical properties of materials. Long-term testing further contributes to the de-risking process by evaluating the durability and stability of materials under various environmental and operational conditions. This presentation will briefly summarize how we address these issues at MAPs@BAM and provide deep-dives on best practices. As the demand for advanced materials continues to grow, MAPs will play an increasingly vital role in driving technological advancements and addressing global challenges. T2 - FutureLabsLive Basel CY - Basel, Switzerland DA - 25.06.2024 KW - MAPs@BAM PY - 2024 AN - OPUS4-62643 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - Material Acceleration Platforms of BAM (MAPs@BAM) N2 - Material Acceleration Platforms (MAPs) represent a transformative approach to the development of resilient and sustainable technology value chains. These platforms can identify candidate chemistries and structures via simulations, and database searches and leverage machine learning-based rapid screening to accelerate the discovery and deployment of novel materials, thereby addressing critical challenges in modern technology sectors. Incorporating high-fidelity advanced characterization in the early phases of material development is crucial for early de-risking. Advanced characterization techniques, such as X-ray diffraction, advanced electrochemical and spectroscopic techniques provide comprehensive insights into the structural, chemical, and physical properties of materials. Long-term testing further contributes to the de-risking process by evaluating the durability and stability of materials under various environmental and operational conditions. This presentation will briefly summarize how we address these issues at MAPs@BAM and provide deep-dives on best practices. As the demand for advanced materials continues to grow, MAPs will play an increasingly vital role in driving technological advancements and addressing global challenges. T2 - EERA-JPNM Days Workshop (EERA-Joint Programme on Nuclear Materials) CY - Online meeting DA - 29.05.2024 KW - MAPs@BAM PY - 2024 AN - OPUS4-62642 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - The interplay of anodic passivation and oxygen evolution on multi-principal element alloys (MPEAs) N2 - Multi-principal element alloys (MPEAs) are of great academic and industrial interest as emerging materials for engineering applications as well as potential electrode materials in energy conversion and storage. Several MPEAs have been studied for their general corrosion behavior, but studies on their dissolution in the high anodic “transpassive” potentials relevant for oxygen evolution reaction (OER) and local corrosion behavior remained scarce. In this project we have investigated CrMnFeCoNi, FeCrNi and CrCoNi MPEAs in terms of their transpassive behavior in NaCl electrolytes and artificial seawater [1, 2]. We introduced a characterization procedure to distinguish the individual contributions of oxygen evolution reaction (OER) and alloy dissolution [2]. This scheme utilizes scanning electrochemical microscopy (SECM) for detecting the onset of OER and employs quantitative chemical analysis methods, namely inductively coupled mass spectrometry (ICP-MS) and ultraviolet-visible light (UV-Vis) spectroscopy, to elucidate the processes of metal dissolution. In-situ atomic force microscopy (AFM) and scanning Kelvin probe force microscopy (SKPFM) were used to analyze the corrosion morphology and surface potentials before, during, and after passivity breakdown. Our results clearly demonstrate the superior corrosion behavior of CrCoNi and FeCrNi MPEA in comparison to the CrFeMnCoNi HEA, as well as AISI 304 stainless steel. We have observed that significant OER occurs in parallel with metal dissolution on the CrCoNi and FeCrNi MPEA surfaces during anodic polarization at potentials relevant to water electrolysis. Most importantly, our findings underscore the necessity of analyzing metal ions dissolved into the electrolyte to accurately assess the Faradaic efficiencies of non-noble metal OER electrocatalysts. The presentation will summarize our characterization procedure and give an overview on the key properties of the studied MPEAs.  [1] A. Wetzel, M. von der Au, P.M. Dietrich, J. Radnik, O. Ozcan, J. Witt, The comparison of the corrosion behavior of the CrCoNi medium entropy alloy and CrMnFeCoNi high entropy alloy, Appl. Surf. Sci., 601 (2022) 154171. [2] A. Wetzel, D. Morell, M. von der Au, G. Wittstock, O. Ozcan, J. Witt, Transpassive Metal Dissolution vs. Oxygen Evolution Reaction: Implication for Alloy Stability and Electrocatalysis, Angew. Chem. Int. Ed. Engl., n/a (2024) e202317058. T2 - ECASIA 2024 CY - Gothenburg, Sweden DA - 09.06.2024 KW - CCMat KW - Corrosion KW - Electrocatalysis KW - Oxygen evolution reaction PY - 2024 AN - OPUS4-62637 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - State-of-the-art in map development: Best practices for application in nuclear materials N2 - Material Acceleration Platforms (MAPs) represent a transformative approach to the development of resilient and sustainable technology value chains. These platforms can identify candidate chemistries and structures via simulations, and database searches and leverage machine learning-based rapid screening to accelerate the discovery and deployment of novel materials, thereby addressing critical challenges in modern technology sectors. Incorporating high-fidelity advanced characterization in the early phases of material development is crucial for early de-risking. Advanced characterization techniques, such as X-ray diffraction, advanced electrochemical and spectroscopic techniques provide comprehensive insights into the structural, chemical, and physical properties of materials. Long-term testing further contributes to the de-risking process by evaluating the durability and stability of materials under various environmental and operational conditions. This presentation will briefly summarize how we address these issues at MAPs@BAM and provide deep-dives on best practices. As the demand for advanced materials continues to grow, MAPs will play an increasingly vital role in driving technological advancements and addressing global challenges. T2 - CONNECT-NM European Partnership Kick-off Meeting CY - Madrid, Spain DA - 02.10.2024 KW - MAPs@BAM KW - Corrosion PY - 2024 AN - OPUS4-62646 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - Material Acceleration Platforms of BAM (MAPs@BAM) N2 - Material Acceleration Platforms (MAPs) represent a transformative approach to the development of resilient and sustainable technology value chains. These platforms can identify candidate chemistries and structures via simulations, and database searches and leverage machine learning-based rapid screening to accelerate the discovery and deployment of novel materials, thereby addressing critical challenges in modern technology sectors. Incorporating high-fidelity advanced characterization in the early phases of material development is crucial for early de-risking. Advanced characterization techniques, such as X-ray diffraction, advanced electrochemical and spectroscopic techniques provide comprehensive insights into the structural, chemical, and physical properties of materials. Long-term testing further contributes to the de-risking process by evaluating the durability and stability of materials under various environmental and operational conditions. This presentation will briefly summarize how we address these issues at MAPs@BAM and provide deep-dives on best practices. As the demand for advanced materials continues to grow, MAPs will play an increasingly vital role in driving technological advancements and addressing global challenges. T2 - International Cooperation on Innovative Materials for Energy Workshop CY - Brussels, Belgium DA - 19.04.2024 KW - MAPs@BAM PY - 2024 AN - OPUS4-62641 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - Autonomous exploration of new alloy chemistries using a Material Acceleration Platform (MAP) N2 - The discovery and commercialization of new corrosion resistant alloys by conventional approaches and manual experimentation is a slow and expensive process. In the last few years, efforts have been dedicated internationally to design self-driving-laboratories, also called Material Acceleration Platforms (MAPs). MAPs integrate material synthesis, characterization and testing modules into circular workflows through automation and use artificial intelligence (AI) for efficient and autonomous experiment design, property prediction and data analysis. We have established a MAP for corrosion research by automating diverse liquid operations, electrochemical testing and data evaluation, where the test results are interpreted via a machine learning (ML)-based backend. The workflows of the electrochemistry module are configured for electrodeposition of different alloys and subsequently performing electrochemical corrosion testing. The platform uses the results of the electrochemical tests to determine the next set of deposition parameters in a continuous and autonomous loop until the user-defined objectives are met. In this project we used the MAP to design new multi-principal element alloys (MPEAs) as corrosion resistant electrode materials for H2O and CO2 electrolysis. One campaign contains a maximum of 144 runs. From each successful campaign top five leads and another five randomly selected materials proceed to upscaling either by electrodeposition at larger scale or as bulk ingots cast by means of arc-melting. With these samples, a detailed chemical and electrochemical characterization using surface analysis techniques was performed to validate the success of the MAP-based optimization. The presentation will give an overview of the design and build phases of our MAP, its modules and workflows. Moreover, we will summarize our results from the FeNiCrCuCoMo MPEA system. T2 - EUROCORR 2024 CY - Paris, France DA - 01.09.2024 KW - MAPs@BAM KW - Corrosion KW - Electrodeposition KW - Material Acceleration Platform KW - Electrochemistry PY - 2024 AN - OPUS4-62635 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - Exploration of Fe-Ni-Cr-X systems using diffusion couples for new alloy chemistries with improved mechanical and corrosion properties N2 - Multi-principal element alloys (MPEAs) are disrupting methodologies in conventional alloy design, characterized by a singular dominant element dictating composition. The traditional optimization of the functional properties of alloys primarily relies on microalloying techniques. The advent of MPEAs has significantly broadened the chemical landscape available for exploration, approaching near-infinite possibilities. Consequently, innovative methodologies are imperative for discovering new alloys that exhibit properties customized for specific applications, simultaneously mitigating dependence on critical minerals. One promising approach for rapid screening of possible alloy chemistries and exploring the hitherto untouched regions of ternary, quaternary or higher order phase diagrams is the use of diffusion couples and multiples. The present study focusses on the exploration of quaternary multi-principle-element alloys (MPEAs) using diffusion multiples. We established diffusion systems by combining an equimolar ternary alloy (FeNiCr) with single diffusing elements Mn, Mo and Ta. Using ThermoCalc® and DICTRA® simulations, we determined suitable parameters (temperature and diffusion time) that would lead to the formation of single-phase alloys and diffusion lengths (>50 μm) that suit the application of high-resolution characterization methods. Microstructural and compositional characterization was performed via scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX), electron probe microanalyzer (EPMA) and correlated to local mechanical properties evaluated by means of nanoindentation. Selected compositions from the diffusion couples were recast and homogenized to obtain bulk samples for the assessment of high-temperature and aqueous corrosion properties. Our results indicate that the ThermoCalc simulations have a good predictive power for crystallographic phases for Mn and Mo containing MPEAs derived from the diffusion couples. Moreover, our data on FeCrNi-Ta system provides valuable experimental input for respective databases necessary for simulation of phase diagrams. The presentation will summarize our methodology using diffusion couples as an efficient tool for exploring compositional spaces of MPEAs in the search for novel alloy chemistries and the results of our correlative study on the mechanical and corrosion properties of the selected quaternary systems. T2 - EUROCORR 2024 CY - Paris, France DA - 01.09.2024 KW - CCMat KW - Corrosion KW - Diffusion couples KW - Multi-principal element alloys PY - 2024 AN - OPUS4-62634 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - High-throughput, automated and autonomous approaches for the design of corrosion resistant materials N2 - The integration of high-throughput electrochemistry, experimental automation and AI-driven processes is enabling the rapid discovery and optimization of advanced materials. This presentation will summarize our research in this field. T2 - GfKORR Grundlagen und Simulation Arbeitsgruppentreffen CY - Online meeting DA - 04.07.2024 KW - MAPs@BAM KW - CCMat KW - Corrosion KW - Electrochemistry PY - 2024 AN - OPUS4-62644 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 - GEN A1 - Ávila Calderón, Luis A1 - Schriever, Sina T1 - BAM Reference Data: Creep of Single-Crystal Ni-Based Superalloy CMSX-6 N2 - This publication provides comprehensive metadata and test results of constant force creep tests according to DIN EN ISO 204:2019-4 on the single crystal Ni-based superalloy CMSX-6 at T = 980 °C and initial stresses between 140 MPa and 230 MPa. The tests were carried out in an accredited test laboratory using calibrated measuring equipment. The data were audited and are BAM reference data. KW - NFDI-MatWerk KW - Digitalisierung KW - CMSX-6 KW - Creep KW - Reference Data KW - Referenzdaten KW - Ni-Based Superalloy PY - 2024 DO - https://doi.org/10.5281/zenodo.13937986 PB - Zenodo CY - Geneva AN - OPUS4-61649 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 - Metal additive manufacturing (Metal AM) continues to gain momentum. Many companies explore the manufacturing of innovative products, including components for safety critical applications. Despite the intensive research of recent years, a fundamental understanding of the process‑structure‑property relationships remains challenging due to, i.a., the inherently complex and highly hierarchical microstructures arising from the wide range of build process parameter variability. This contribution presents the resu lts 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 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 a llowed 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 hwas also tested as a reference. The produced PBF LB/M/316L possesses shorter primary and secondary creep stages and times to rupture and smaller creep stress exponents than the hot‑rolled variant. Overall, the creep damage is more extensive in the PBF LB/M/316L and is characterized as predominantly intergranular. It is considered that the damage behavior is mainly impacted by the formation of precipitates at the grain boundaries combined with their unfavorable orientation. The dislocation substructure and local elemental segregation appear to have a decisive impact on the overall creep behavior. T2 - 16th International Conference on Creep and Fracture of Engineering Materials and Structures CY - Bangalore, India DA - 28.07.2024 KW - AGIL KW - 316L KW - Additive Manufacturing KW - Creep KW - Microstructure evolution PY - 2024 AN - OPUS4-60839 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 - 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 - 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 - 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 - Ávila Calderón, Luis T1 - Framework for Curation and Distribution of Reference Datasets on the Example of Creep Data of Ni- Based Superalloys N2 - This presentation introduces our current effort to develop a best practice framework for generating and distributing MSE reference datasets using creep data of Ni-based superalloys as an example, building on previous approaches. Such reference datasets can be used in the verification of testing equipment or to compare experimental or simulation results among different laboratories or collaborative centers. Our framework concept, for reference data, includes the generation of the data along with an agreement on the necessary metadata, considering the intended usage, and the integration into an easily accessible digital infrastructure to annotate and discover/distribute the datasets using a metadata schema accordingly aligned to a domain ontology. T2 - International Materials Science and Engineering Congress - MSE 2024 CY - Darmstadt, Germany DA - 24.09.2024 KW - Referenzdaten KW - Digitalisierung KW - Data schema KW - NFDI-MatWerk KW - Datenschema KW - FAIR PY - 2024 AN - OPUS4-61175 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis T1 - Low-cycle-fatigue behavior of stainless steel 316L manufactured by laser powder bed fusion N2 - This contribution presents the results of an experimental study on the LCF behavior of an austenitic 316L stainless steel produced by laser powder bed fusion featuring a low defect population, which allows for an improved understanding of the role of other typical aspects of a PBF‑LB microstructure. The LCF tests were performed between room temperature and 600 °C. A hot‑rolled 316L variant was tested as a reference. The mechanical response is characterized by strain-life curves, a Coffin‑Manson‑Basquin fitting, and cyclic deformation curves. The damage and deformation mechanisms are studied with X-ray computed tomography, optical and electron microscopy. The PBF‑LB/M/316L exhibits lower fatigue lives at lower strain amplitudes. The crack propagation is mainly transgranular. The solidification cellular structure seems to be the most relevant underlying microstructural feature determining the cyclic deformation behavior. T2 - TMS 2024 Annual Meeting & Exhibition CY - Orlando, Florida, US DA - 03.03.2024 KW - AGIL KW - Additive Fertigung KW - Mikrostruktur KW - LCF KW - 316L PY - 2024 AN - OPUS4-59782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zuffa, Caterina A1 - Cappuccino, Chiara A1 - Casali, Lucia A1 - Emmerling, Franziska A1 - Maini, Lucia T1 - Liquid reagents are not enough for liquid assisted grinding in the synthesis of [(AgBr)(n-pica)]n N2 - This study investigates the mechanochemical reactions between AgBr 3-picolylamine and 4-picolylamine. The use of different stoichiometry ratios of the reagents allows [(AgBr)(n-pica)]n and [(AgBr)2(n-pica)]n to be obtained, and we report the new structures of [(AgBr)2(3-pica)]n and [(AgBr)2(4-pica)]n which are characterized by the presence of the following: (a) infinite inorganic chains, (b) silver atom coordinated only by bromide atoms and (c) argentophilic interactions. Furthermore, we studied the interconversion of [(AgBr)(n-pica)]n/[(AgBr)2(n-pica)]n by mechanochemical and thermal properties. The in situ experiments suggest that [(AgBr)(3-pica)]n is kinetically favoured while [(AgBr)2(3-pica)]n is converted into [(AgBr)(3-pica)]n only with a high excess of the ligand. Finally, the liquid nature of the ligands is not sufficient to assist the grinding process, and the complete reaction is observed with the addition of a small quantity of acetonitrile. KW - Mechanochemistry KW - Complex PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594755 DO - https://doi.org/10.1039/d3cp04791a SN - 1463-9076 SP - 1 EP - 10 PB - Royal Society of Chemistry (RSC) AN - OPUS4-59475 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zorn, R. A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed Aejaz A1 - Malpass-Evans, R. A1 - McKeown, N. A1 - Jalarvo, N. A1 - Tyagi, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Microscopic molecular mobility of high-performance polymers of intrinsic microporosity revealed by neutron scattering – bend fluctuations and signature of methyl group rotation N2 - Polymers of intrinsic microporosity exhibit a combination of high gas permeability and reasonable permselectivity, which makes them attractive candidates for gas separation membrane materials. The diffusional selective gas transport properties are connected to the molecular mobility of these polymers in the condensed state. Incoherent quasielastic neutron scattering was carried out on two polymers of intrinsic microporosity, PIM-EA-TB(CH3) and its demethylated counterpart PIM-EA-TB(H2), which have high Brunauer–Emmett–Teller surface area values of 1030 m2 g-1 and 836 m2 g-1, respectively. As these two polymers only differ in the presence of two methyl groups at the ethanoanthracene unit, the effect of methyl group rotation can be investigated solely. To cover a broad dynamic range, neutron time-of-flight was combined with neutron backscattering. The demethylated PIM-EA-TB(H2) exhibits a relaxation process with a weak intensity at short times. As the backbone is rigid and stiff this process was assigned to bendand-flex fluctuations. This process was also observed for the PIM-EA-TB(CH3). A further relaxation process is found for PIM-EA-TB(CH3), which is the methyl group rotation. It was analyzed by a jump-diffusion in a three-fold potential considering also the fact that only a fraction of the present hydrogens in PIM-EATB(CH3) participate in the methyl group rotation. This analysis can quantitatively describe the q dependence of the elastic incoherent structure factor. Furthermore, a relaxation time for the methyl group rotation can be extracted. A high activation energy of 35 kJ mol-1 was deduced. This high activation energy evidences a strong hindrance of the methyl group rotation in the bridged PIM-EA-TB(CH3) structure. KW - Polymers of Intrinsic Microporosity KW - Neutron Scattering PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-604114 DO - https://doi.org/10.1039/d4sm00520a SP - 1 EP - 11 PB - RSC AN - OPUS4-60411 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -