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 - MAPz@BAM Material Acceleration Plattform Zentrum @ BAM N2 - Die Material Acceleration Platform der BAM (MAPz@BAM) bündelt unsere Automatisierungs-Expertise auf dem Gebiet der Materialwissenschaft und -prüfung. Wir entwickeln modulare Experimentmodule, automatische Prüf- und Auswerteverfahren und setzen künstliche Intelligenz für eine effiziente und autonome Versuchsplanung, - vorhersage und Datenanalyse ein. T2 - Kick off Meeting / EnerMAC ZIM Network CY - Berlin, Germany DA - 07.12.2023 KW - Material Acceleration Platforms (MAPs) KW - Self-driving-labs (SDLs) KW - MAPz@BAM PY - 2023 AN - OPUS4-59411 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - MAPz@BAM Material Acceleration Plattform Zentrum @ BAM N2 - Die Material Acceleration Platform der BAM (MAPz@BAM) bündelt unsere Automatisierungs-Expertise auf dem Gebiet der Materialwissenschaft und -prüfung. Wir entwickeln modulare Experimentmodule, automatische Prüf- und Auswerteverfahren und setzen künstliche Intelligenz für eine effiziente und autonome Versuchsplanung, - vorhersage und Datenanalyse ein. T2 - TechConnect Adlershof: Grand Solutions CY - Berlin, Germany DA - 06.11.2023 KW - Material Acceleration Platforms (MAPs) KW - Self-driving-labs (SDLs) KW - MAPz@BAM PY - 2023 AN - OPUS4-59412 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 - Material acceleration platforms (MAPs) - Global activities and developments at BAM N2 - Die Material Acceleration Platform der BAM (MAPz@BAM) bündelt unsere Automatisierungs-Expertise auf dem Gebiet der Materialwissenschaft und -prüfung. Wir entwickeln modulare Experimentmodule, automatische Prüf- und Auswerteverfahren und setzen künstliche Intelligenz für eine effiziente und autonome Versuchsplanung, - vorhersage und Datenanalyse ein. T2 - WPFM Expert Group on Structural Materials (EGSM) CY - Online meeting DA - 23.05.2023 KW - Material Acceleration Platforms (MAPs) KW - MAPz@BAM KW - Self-driving-labs PY - 2023 AN - OPUS4-59409 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 - JOUR A1 - Ávila Calderón, Luis A1 - Shakeel, Y. A1 - Gedsun, A. A1 - Forti, M. A1 - Hunke, S. A1 - Han, Ying A1 - Hammerschmidt, T. A1 - Aversa, R. A1 - Olbricht, Jürgen A1 - Chmielowski, M. A1 - Stotzka, R. A1 - Bitzek, E. A1 - Hickel, Tilmann A1 - Skrotzki, Birgit T1 - Management of reference data in materials science and engineering exemplified for creep data of a single-crystalline Ni-based superalloy N2 - The identification of process-structure-property relationships of materials inevitably requires the combination of research data from different measurements. Therefore, the concepts related to FAIR (findable, accessible, interoperable, reusable) data handling, increasingly reported in literature, are particularly important in the materials science and engineering domain. However, they have not yet been integrated into a single, overarching methodological framework, particularly for reference data. Here, we introduce such a framework. Our concept covers data generation, documentation, handling, storage, sharing, data search and discovery, retrieval, and usage. Furthermore, we prototypically implement it using a real dataset with creep data of a single-crystal CMSX-6 Ni-based superalloy. The presented implementation is traceable and permanently accessible through open repositories. The individual elements considered in the framework ensure the functionality and usability of the data and, thus, the adherence to the FAIR principles. In conjunction with this, we present a definition for reference data of materials. Our definition underlines particularly the importance of a comprehensive documentation, e.g., on material provenance, data processing procedures, and the software and hardware used, including software-specific input parameters, as these details enable data users or independent parties to assess the quality of the datasets and to reuse and reproduce the results. Reference data that is managed according to the proposed framework can be used to advance knowledge in the materials science and engineering domain, e.g., by identifying new process-structure-property relations. KW - Referenzdaten KW - NFDI-MatWerk KW - Data schema KW - Research Data Management KW - Reference Data PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625047 DO - https://doi.org/10.1016/j.actamat.2025.120735 VL - 286 SP - 1 EP - 15 PB - Elsevier Inc. AN - OPUS4-62504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis A1 - Hammerschmidt, T. A1 - Stotzka, R. T1 - Demonstration of the Infrastructure Use Case 02: Framework for curation and distribution of reference datasets N2 - In our current view, reference datasets in the MSE domain represent specific material properties, e.g., structural, mechanical, … characteristics. A reference dataset must fulfill high-quality standards, not only in precision of measurement but also in a comprehensive documentation of material, processing, and testing history (metadata). This Infrastructure Use Case (IUC) aims to develop a framework for generating reference material datasets using creep data of a single crystal Ni-based superalloy as a best practice example. In a community-driven process, we aim to encourage the discussion and establish a framework for the creation and distribution of reference material datasets. In this poster presentation, we highlight our current vision and activities and intend to stimulate the discussion about the topic reference datasets and future collaborations and work. T2 - NFDI-MatWerk Conference CY - Siegburg, Germany DA - 27.06.2023 KW - Referenzdaten KW - Reference data KW - Creep KW - Metadata schema KW - Syngle Crystal alloy PY - 2023 AN - OPUS4-57924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis A1 - Hammerschmidt, T. A1 - Gedsun, A. A1 - Forti, M. A1 - Olbricht, Jürgen A1 - Stotzka, R. A1 - Skrotzki, Birgit T1 - IUC02 Framework for Curation and Distribution of Reference Datasets using Creep Data of Ni-Base Superalloys as an Example N2 - In our current view, reference datasets in the MSE domain represent specific material properties, e.g., structural, mechanical, … characteristics. A reference dataset must fulfill high-quality standards, not only in precision of measurement but also in a comprehensive documentation of material, processing, and testing history (metadata). This Infrastructure Use Case (IUC) aims to develop a framework for generating reference material datasets using creep data of a single crystal Ni-based superalloy as a best practice example. In a community-driven process, we aim to encourage the discussion and establish a framework for the creation and distribution of reference material datasets. In this poster presentation, we highlight our current vision and activities and intend to stimulate the discussion about the topic reference datasets and future collaborations and work. T2 - NFDI-MatWerk Conference CY - Siegburg, Germany DA - 27.06.2023 KW - Referenzdaten KW - Reference data KW - Syngle Crystal alloy KW - Creep KW - Metadata schema PY - 2023 AN - OPUS4-57923 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 - Management of Reference Data of Creep of Ni-Based Superalloys Exemplified for CMSX-6 N2 - The identification of process-structure-property relationships of materials inevitably requires the combination of research data from different measurements. Therefore, the concepts related to FAIR (findable, accessible, interoperable, reusable) data handling, increasingly reported in literature, are particularly important in the materials science and engineering domain. However, they have not yet been integrated into a single, overarching methodological framework, particularly for reference data. Here, we introduce such a framework, which covers data generation, documentation, handling, storage, sharing, data search and discovery, retrieval, and usage. Furthermore, we prototypically implement it using a real dataset with creep data of a single-crystal CMSX-6 Ni-based superalloy. The implementation is traceable and permanently accessible through open repositories. The individual elements considered in the framework ensure the functionality and usability of the data and, thus, the adherence to the FAIR principles. In conjunction with this, we present a definition for reference data of materials. Our definition underlines particularly the importance of a comprehensive documentation, e.g., on material provenance, data processing procedures, and the software and hardware used, including software-specific input parameters, as these details enable data users or independent parties to assess the quality of the datasets and to reuse and reproduce the results. Reference data that is managed according to the proposed framework can be used to advance knowledge in the materials science and engineering domain, e.g., by identifying new process-structure-property relations. T2 - The 20th International Conference on Strength of Materials CY - Kyoto, Japan DA - 02.06.2025 KW - NFDI-MatWerk KW - Referenzdaten KW - Data schema KW - Creep PY - 2025 AN - OPUS4-63428 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis T1 - Management of Reference Data of Creep of Ni-Based Superalloys Exemplified for CMSX-6 N2 - The identification of process-structure-property relationships of materials inevitably requires the combination of research data from different measurements. Therefore, the concepts related to FAIR (findable, accessible, interoperable, reusable) data handling, increasingly reported in literature, are particularly important in the materials science and engineering domain. However, they have not yet been integrated into a single, overarching methodological framework, particularly for reference data. Here, we introduce such a framework, which covers data generation, documentation, handling, storage, sharing, data search and discovery, retrieval, and usage. Furthermore, we prototypically implement it using a real dataset with creep data of a single-crystal CMSX-6 Ni-based superalloy. The implementation is traceable and permanently accessible through open repositories. The individual elements considered in the framework ensure the functionality and usability of the data and, thus, the adherence to the FAIR principles. In conjunction with this, we present a definition for reference data of materials. Our definition underlines particularly the importance of a comprehensive documentation, e.g., on material provenance, data processing procedures, and the software and hardware used, including software-specific input parameters, as these details enable data users or independent parties to assess the quality of the datasets and to reuse and reproduce the results. Reference data that is managed according to the proposed framework can be used to advance knowledge in the materials science and engineering domain, e.g., by identifying new process-structure-property relations. T2 - TMS 2025 Annual Meeting & Exhibition CY - Las Vegas, NV, USA DA - 22.03.2025 KW - Referenzdaten KW - Creep KW - Data schema KW - NFDI-MatWerk PY - 2025 AN - OPUS4-62849 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis T1 - IUC02: Framework for Curation & Distribution of Reference Datasets (On the example of Creep Data of Ni Based superalloys) N2 - A research data management framework to conceptualize & implement a digital infrastructure for the Generation, Distribution, and Utilization of reference datasets of materials is presented. The documentation of the test data is often incomplete. This concerns, e.g., material’s manufacturing process or chemical composition, or test equipment’s description and its calibration status. Our concept addresses this issue by proposing the implementation of a requirements profile. A crucial part of the concept is to reach a community-agreement on the definition of reference data and on the underlying data schema and vocabulary. In this presentation a general workflow overview and the relevance of selected individual subworkflows is presented. T2 - MSE Research Data Forum 2025 CY - Siegburg, Germany DA - 08.07.2025 KW - NFDI MatWerk KW - Referenzdaten KW - Kriechen PY - 2025 AN - OPUS4-64881 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis T1 - Management of Reference Data of Creep of Ni Based Superalloys Exemplified for CMSX 6 N2 - Research data management (RDM) framework to conceptualize & implement a digital infrastructure for the Generation, Distribution, and Utilization of reference datasets of materials. Documentation of the test data is often incomplete. This concerns, e.g., material’s manufacturing process or chemical composition, or test equipment’s description and its calibration status. Our concept addresses this issue by proposing the implementation of a requirements profile. A crucial part of the concept is to reach a community-agreement on the definition of reference data and on the underlying data schema and vocabulary. T2 - 2. SupERBO Symposium on Superalloys CY - Bochum, Germany DA - 27.02.2025 KW - NFDI MatWerk KW - Referenzdaten KW - Kriechen PY - 2025 AN - OPUS4-64859 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis T1 - Management of Reference Data in Materials Science and Engineering Exemplified for Creep Data of a Single-Crystalline Ni-Based Superalloy N2 - Here we present our research data management (RDM) framework to conceptualize & implement a digital infrastructure for the Generation, Distribution, and Utilization of reference datasets of materials. The documentation of the test data is often incomplete. This concerns, e.g., material’s manufacturing process or chemical composition, or test equipment’s description and its calibration status. Our concept addresses this issue by proposing the implementation of a requirements profile. A crucial aspect of our concept is to reach a community-agreement on the definition of reference data and on the underlying data schema and vocabulary. T2 - MaRDA2025 Virtual Annual Meeting CY - Online meeting DA - 18.02.2025 KW - NFDI MatWerk KW - Referenzdaten KW - Kriechen KW - Datenschema PY - 2025 AN - OPUS4-64858 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zänker, Steffen A1 - Scholz, Gudrun A1 - Krahl, Thoralf A1 - Prinz, Carsten A1 - Emmerling, Franziska A1 - Kemnitz, E. T1 - Luminescent properties of Eu3+/Tb3+ doped fluorine containing coordination polymers N2 - Lanthanides doped coordination polymers (CPs) with different binding motifs were synthesized to investigate the influence of the different fluorine positions in the structure on the decay time τ of the excited states. Fluorine can be integrated into the network mechanochemically via a fluorinated organic linker, here barium tetrafluoroterephthalate Ba(p-BDC-F4)2 or directly via a metal-fluorine bond (barium terephthalate fluoride BaF(p-BDC)0.5). The CP with a metal-fluorine bond shows the highest lifetime of the excited states of lanthanides (Eu3+, Tb3+ or Eu3+& Tb3+). The excitation of the lanthanides can be performed directly via the excitation wavelength typical for lanthanides and via the excitation wavelength of the linker. This enabled the simultaneous excitation of Eu3+ and Tb3+ in one CP. In the emission spectra (λem = 393 nm) of the mixed doped CPs (Eu3+ and Tb3+) the bands of both lanthanides can be observed. The integration into the crystal lattice and the homogeneous distribution of the lanthanides in the CPs is shown by X-ray diffraction, TEM, STEM-EDS measurements and the long decay times. KW - Alkaline earth metal coordination polymers KW - Fluorine coordination polymers KW - Lanthanides doped coordination polymers KW - Luminescence PY - 2021 DO - https://doi.org/10.1016/j.solidstatesciences.2021.106614 VL - 117 SP - 106614 PB - Elsevier Masson SAS AN - OPUS4-52559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zänker, Steffen A1 - Scholz, G. A1 - Xu, W. A1 - Kemnitz, E. A1 - Emmerling, Franziska T1 - Structure and properties of fluorinated and non-fluorinated Ba-coordination polymers - the position of fluorine makes the difference N2 - As the most electronegative element, fluorine has a strong influence on material properties such as absorption behaviour or chemical and thermal stability. Fluorine can be easily integrated into coordination polymers (CPs) via a fluorinated acetate, here trifluoroacetate in Ba(CF3COO)2, or directly via a metal fluorine bond (BaF(CH3COO)). In the present study both possibilities of fluorine integration were tested and their effect on structure and properties of barium coordination polymers was investigated in comparison with the non-fluorinated barium acetate (Ba(CH3COO)2). In addition to the study of their thermal behaviour and their decomposition temperature, the CPs structures were tested for their application as possible anode materials in lithium ion batteries and for their sorption of water and ammonia. The properties of the CPs can be traced back to the individual structural motifs and could thus trigger new design ideas for CPs in LIBs and/or catalysis. KW - Alkaline earth metal coordination polymers KW - Lithium-ion battery KW - Water stability KW - Fluorine coordination PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-524041 DO - https://doi.org/10.1002/zaac.202000360 SN - 0044-2313 VL - 647 IS - 9 SP - 1014 EP - 1024 PB - Wiley-VCH GmbH AN - OPUS4-52404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zänker, Steffen A1 - Scholz, G. A1 - Marquardt, Julien A1 - Emmerling, Franziska T1 - Structural changes in Ba-compounds of different hardness induced by high-energy ball milling – evidenced by 137Ba NMR and X-ray powder diffraction N2 - Changes in the global bulk and local structures, of three different barium compounds (BaZrO3, BaF2, and BaFCl),were induced by mechanical milling and followed using X-ray powder diffraction (PXRD), subsequent microstructure analysis, and 137Ba solid state NMR spectroscopy. Harder materials like BaZrO3 experience significantly higher structural changes upon milling than softer materials like BaF2. Moreover, soft materials with layered structures, like BaFCl, show a pronounced structural change during the milling process. By combining PXRD and solid state NMR, detailed information on the changes to the global and local structures were obtained, which are of interest for mechanochemical synthesis, mechanically treated catalysts or ionic conductors. KW - Mechanochemistry KW - X-ray diffraction KW - Solid state NMR PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547397 DO - https://doi.org/10.1002/zaac.202200026 SN - 0044-2313 VL - 648 IS - 10 SP - 1 EP - 8 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zänker, Steffen A1 - Scholz, G. A1 - Heise, M. A1 - Kemnitz, E. A1 - Emmerling, Franziska T1 - New 2D layered structures with direct fluorine-metal bonds: MF(CH3COO) (M: Sr, Ba, Pb) N2 - New coordination polymers with 2D network structures with fluorine directly coordinated to the metal ion were prepared both via mechanochemical synthesis and fluorolytic sol–gel synthesis. Depending on the synthesis route, the samples show different particle sizes, according to SEM imaging. The crystal structures of barium acetate fluoride, strontium acetate fluoride, and lead acetate fluoride (BaFIJCH3COO), SrFIJCH3COO) and PbFIJCH3COO)) were solved from X-ray powder diffraction data. The structure solution is backed by the results from 19F MAS NMR, FT IR data, and thermal analysis. The calculated chemical shifts of the 19F MAS NMR spectra coincide well with the measured ones. It turns out that the grinding conditions have a remarkable influence on the mechanochemical synthesis and its products. Our systematic study also indicates a strong influence of the atomic radii of Ca, Sr, Ba, and Pb on the success of the syntheses. KW - Mechanochemistry KW - Coordination polymers PY - 2020 DO - https://doi.org/10.1039/d0ce00287a VL - 22 IS - 16 SP - 2772 EP - 2780 PB - Royal Society of Chemistry AN - OPUS4-50789 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zvereva, V.V. A1 - Asanov, I.P. A1 - Yusenko, Kirill A1 - Zadesenec, A.V. A1 - Plyusnin, P.E. A1 - Gerasimov, E.Yu. A1 - Maksimovskiy, E.A. A1 - Korenev, S.V. A1 - Asanova, T.I. T1 - Local atomic and electronic structure of Pt‑Os nanoplates and nanofbers derived from the single‑source precursor (NH4)2[Pt0.5Os0.5Cl6] N2 - Abstract Nowadays, Pt-Os binary systems are mainly considered as catalysts and electrocatalysts, but the role of Os in these processes is still poorly understood. The electronic structure of Pt-Os nanosystems remains a few studied as well. Using bimetallic (NH4)2[Pt0.5Os0.5Cl6] as a single-source precursor for preparing Pt-Os nanoalloy through the thermal decomposition in hydrogen and inert atmospheres, the relation of morphology, atomic ordering, and electronic structure of Pt-Os nanoalloy was examined by in situ Quick XAFS, XPS, PXRD, SEM, and HRTEM techniques. Being the only variable parameter, the decomposition atmosphere was found to govern the morphology of the Pt-Os nanoalloy and change the atomic ordering (alloying extent), which involves a change in the electronic structure. In a hydrogen atmosphere, the nanofibers (NFs) (ø ~ 5–6 nm) with the atomic ordering Oscore&Pt-richshell were observed to form; in a nitrogen atmosphere, thin nanoplates (NPLs) (~ 12 nm) with the atomic architecture Os-richcore&Ptrichshell were found out. The depletion in the Os 5d5/2 and Pt 5d5/2,3/2 states was revealed for Pt-Os nanoalloys. This unusual result disagrees with the known d-band theory and indicates that there is a gain of non-d conduction electron counts at one or both sites. Mixed conductivity may exist in such Pt-Os nanoalloy that may be responsible for a manifestation of new physical properties of this binary system . KW - Bimetallic alloy KW - Nanoalloy KW - Synchrotron radiation KW - XAFS KW - Electronic structure KW - Alloy morphology PY - 2021 DO - https://doi.org/10.1007/s11051-021-05378-z SN - 1388-0764 VL - 24 IS - 1 SP - 1 EP - 23 PB - Springer AN - OPUS4-55347 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zutta Villate, J. M. A1 - Viviana Rojas, J. A1 - Hahn, Marc Benjamin A1 - Anselmo Puerta, J. T1 - Synthesis of 198Au nanoparticles sub 10 nm due optimization on local dose by Monte Carlo simulations for cancer treatment N2 - To enhance the biological effects of radiation damage in cancerous cells, we present an alternative approach to the use of gold nanoparticles (AuNP), focusing on the synthesis and characterization of highly monodisperse, spherical radioactive gold nanoparticles 198AuNP. The size of the AuNP size was optimized with the help of Geant4/TOPAS particle scattering simulations, and energy deposition per nm3 per decay for varying radii (2–10 nm) was evaluated. This work is the foundation for ongoing experimental work to evaluate cell death induced by 198AuNP which aims for the use of radioactive gold nanoparticles in cancer treatment. KW - AuNP KW - Beta decay KW - Beta particle KW - Brachytherapy KW - Cancer treatment KW - Nanoparticles KW - Nanoparticle KW - DNA KW - DNA damage KW - Dosimetry KW - Energy deposit KW - Gamma ray KW - Geant4 KW - Geant4-DNA KW - Gold Nanoparticles KW - LEE KW - Low energy electrons KW - MCS KW - Microdosimetry KW - Monte-Carlo simulation KW - NP KW - Synthesis KW - TEM KW - OH radicals KW - Particle scattering KW - Radiation damage KW - Radiationtherapy KW - Radioactive decay KW - Radiolysis KW - Simulation KW - TOPAS KW - TOPAS-nbio PY - 2022 DO - https://doi.org/10.1007/s10967-022-08355-5 SN - 1588-2780 SP - 1 EP - 9 PB - Springer Nature AN - OPUS4-55132 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 - CONF A1 - Zubia Aranburu, Judith A1 - Cappella, Brunero A1 - Zabala Eguren, A. A1 - Buruaga Lamarain, L. A1 - Aginagalde Lopez, A. A1 - Bonse, Jörn A1 - Schwibbert, Karin T1 - Quantification of the adhesion force of E. coli on Ti via single-cell force spectroscopy N2 - Antibiotic resistance is a growing global problem which poses a massive threat to human health. Although human activity contributes to the acceleration of the process, bacteria have a self-driven stabilisation mechanism to protect themselves from such and other external threats: biofilm formation. Nonetheless, it is the adhesion of a single bacterial cell to a surface that triggers the formation of such network of biomolecules and microorganisms, as well as its hazardous consequences. The main objective of this work was to quantify the adhesion force of a single E. coli cell on a Ti substrate via the AFM-related single-cell force spectroscopy, with both the cell and the substrate material being of high clinical relevance. A set of 25 x 25 force displacement curves was acquired with a maximum force of 3.2 nN without dwell time, yielding a topography map and an adhesion force map that showed to be correlated. A mean adhesion force of 0.85 ± 0.175 nN was measured and the presence of cell appendages on the bacterial cell wall was verified through individual force-displacement curves. Bacterial viability was assessed after the measurements via live/dead staining. T2 - XL Congreso Anual de la Sociedad Española de Ingeniería Biomédica CASEIB 2022 CY - Valladolid, Spain DA - 23.11.2022 KW - Bacteria KW - Atomic force microscopy KW - Force distance curve PY - 2022 SN - 978-84-09-45972-8 SP - 217 EP - 220 AN - OPUS4-57039 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zou, T. A1 - Nonappa, N. A1 - Khavani, M. A1 - Vuorte, M. A1 - Penttilä, P. A1 - Zitting, A. A1 - Valle-Delgado, J. J. A1 - Elert, Anna Maria A1 - Silbernagl, Dorothee A1 - Balakshin, M. A1 - Sammalkorpi, M. A1 - Österberg, M. T1 - Experimental and Simulation Study of the Solvent Effects on the Intrinsic Properties of Spherical Lignin Nanoparticles N2 - Spherical lignin nanoparticles (LNPs) fabricated via nanoprecipitation of dissolved lignin are among the most attractive biomass-derived nanomaterials. Despite various studies exploring the methods to improve the uniformity of LNPs or seeking more application opportunities for LNPs, little attention has been given to the fundamental aspects of the solvent effects on the intrinsic properties of LNPs. In this study, we employed a variety of experimental techniques and molecular dynamics (MD) simulations to investigate the solvent effects on the intrinsic properties of LNPs. The LNPs were prepared from softwood Kraft lignin (SKL) using the binary solvents of aqueous acetone or aqueous tetrahydrofuran (THF) via nanoprecipitation. The internal morphology, porosity, and mechanical properties of the LNPs were analyzed with electron tomography (ET), small-angle X-ray scattering (SAXS), atomic force microscopy (AFM), and intermodulation AFM (ImAFM). We found that aqueous acetone resulted in smaller LNPs with higher uniformity compared to aqueous THF, mainly ascribing to stronger solvent−lignin interactions as suggested by MD simulation results and confirmed with aqueous 1,4-dioxane (DXN) and aqueous dimethyl sulfoxide (DMSO). More importantly, we report that both LNPs were compact particles with relatively homogeneous density distribution and very low porosity in the internal structure. The stiffness of the particles was independent of the size, and the Young’s modulus was in the range of 0.3−4 GPa. Overall, the fundamental understandings of LNPs gained in this study are essential for the design of LNPs with optimal performance in applications. KW - Lignin KW - Electron tomography KW - Intermodulation AFM KW - Modulus KW - SAXS PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546948 DO - https://doi.org/10.1021/acs.jpcb.1c05319 SN - 1520-5207 VL - 125 IS - 44 SP - 12315 EP - 12328 PB - ACS AN - OPUS4-54694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zosef, M. A1 - Fahmy, Alaa A1 - El Hotaby, W. A1 - Hassan, A. A1 - Khalil, A. A1 - Anis, B. T1 - High performance graphene-based PVF foam for lead removal from water N2 - The synthesis and optimization of superior and eco-friendly sorbents for Pb(II) pose a great challenge in the field of water treatment. The sorbent was developed by introducing graphene oxide (GO) into the matrix of polyvinyl formaldehyde (PVF) foam. The immobilization of GO in PVF results in significant increase in the maximum adsorption capacity (Qt) of GO powder for Pb(II), from ≈800 to ≈1730 mg g−1 in the case of GO/PVF foam. As compared with GO powder in Pb(II) aqueous solutions, PVF matrix keeps GO sheets stable without any agglomeration. The large surface area of GO sheet allows the abundant oxygenated functional groups on its surface to participate effectively in the Pb(II) adsorption process, leading to the huge increase of the Qt. Adsorption isotherms and kinetic studies indicated that the sorption process of Pb(II) on GO/PVF was done on heterogenous surface by ion-exchange reaction. The GO/PVF foam showed an excellent reusability for more than 10 cycles with almost the same efficiency and without any significant change in its physical properties. KW - Water treatment KW - Graphene oxide KW - Lead ions KW - Polyvinyl formaldehyde foam KW - Superior sorbent PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-523013 DO - https://doi.org/10.1016/j.jmrt.2020.08.011 VL - 9 IS - 5 SP - 11861 EP - 11875 PB - Elsevier B.V. AN - OPUS4-52301 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 - Wolf, M. A1 - Alentiev, D. A1 - Bermeshev, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Low frequency vibrational density of state of highly permeable super glassy polynorbornenes – The Boson peak N2 - Inelastic incoherent neutron time-of flight scattering was employed to measure the low frequency density of states for a series of addition polynorbornenes with bulky side groups. The rigid main chain in combination with the bulky side groups give rise to a microporosity of these polymers in the solid state. The microporosity characterized by the BET surfaces area varies systematically in the considered series. Such materials have some possible application as active separation layer in gas separation membranes. All investigated materials show excess contributions to the Debye type density of states characteristic for glasses known as Boson peak. The maximum position of the Boson peak shifts to lower frequency values with increasing microporosity. Data for PIM-1 and Matrimid included for comparison are in good agreement to this dependency. This result supports the sound wave interpretation of the Boson peak. KW - Polynorbornes KW - Neutron Scattering PY - 2020 DO - https://doi.org/10.1039/d0cp03360j SN - 1463-9076 VL - 22 IS - 33 SP - 18381 EP - 18387 PB - Royal Chemical Society AN - OPUS4-51165 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 - Tyagi, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Low frequency vibrations and diffusion in disordered polymers bearing an intrinsic microporosity as revealed by neutron scattering N2 - The microscopic diffusion and the low frequency density of states (VDOS) of PIM-EATB(CH3) are investigated by inelastic and quasi-elastic neutron scattering where also the demethylated counterpart of PIM-EA-TB(H2) is considered. These intrinsic microporous polymers are characterized by large BET surface area values of several hundred m2/g and pore sizes between 0.5 and 2 nm. Detailed comparison is made to the archetype of polymers of intrinsic microporosity, PIM-1, and polynorbornenes also bearing a microporosity. Due to the wavelength of neutrons, the diffusion and vibrations can be addressed on microscopic length and time scales. From the inelastic neutron scattering experiments the low frequency density of states (VDOS) is estimated which shows excess contributions to the Debye-type VDOS known as Boson peak. It was found that the maximum frequency of the Boson peak decreases with increasing microporosity characterized by the BET surface area. However, besides the BET surface area, additional factors such as the backbone stiffness govern the maximum frequency of the Boson peak. Further the mean squared displacement related to microscopic motions was estimated from elastic fixed window scans. At temperatures above 175 K, the mean squared displacement PIM-EA-TB(CH3) is higher than that for the demethylated counterpart PIM-EA-TB(H2). The additional contribution found for PIM-EATB(CH3) is ascribed to the rotation of the methyl group in this polymer because the only difference between the two structures is that PIM-EA-TB(CH3) has methyl groups where PIM-EA-TB(H2) has none. A detailed comparison of the molecular dynamics is also made to that of PIM-1 and the microporous polynorbornene PTCNSi1. The manuscript focuses on the importance of vibrations and the localized molecular mobility characterized by the microscopic diffusion on the gas Transport in polymeric separation membranes. In the frame of the random gate model localized fluctuations can open or close bottlenecks between pores to enable the diffusion of gas molecules. KW - Polymer of intrisic microporosity KW - Neutron scattering KW - Boson peak KW - Methyl group rotation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538490 DO - https://doi.org/10.3390/cryst11121482 VL - 11 IS - 12 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-53849 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 - TY - JOUR A1 - Zorn, R. A1 - Lohstroh, W. A1 - Zamponi, M. A1 - Harrison, W. A1 - Budd, P. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Molecular mobility of a polymer of intrinsic microporosity revealed by quasielastic neutron scattering N2 - Quasielastic neutron scattering by employing a combination of time-of-flight and backscattering techniques is carried out to explore the molecular mobility of a polymer of intrinsic microporosity (PIM-1) at microscopic time scales in comparison with a high-performance polyimide. Molecular fluctuations can change the structure of the temporary network of micropores and open or close pathways for gas molecules. Therefore, the investigation might help to understand the selectivity of PIMs in gas separation processes. The performed neutron scattering experiments provide evidence for a low-temperature relaxation process, which was assigned to methyl group rotation. This methyl group rotation was analyzed in terms of jump diffusion in a three-fold potential. The analysis results in a fraction of methyl groups which are immobilized. For PIM-1 it was found that the fraction of immobilized methyl groups decreases with increasing temperature up to 350 K. At higher temperatures the number of immobilized methyl group increases gain due to an underlying relaxation process. This motional process on a somewhat larger length scale might lead to a reversible structural rearrangement which partially hinders the strongly localized methyl group rotation. In addition, it was found that the activation energy for the methyl group rotation for PIM-1 and the polyimide is significantly higher than for conventional polymers. KW - Polymer of intrinsic microporosity KW - Quasielastic neutron scattering PY - 2020 DO - https://doi.org/10.1021/acs.macromol.0c00963 SN - 0024-9297 SN - 1520-5835 VL - 53 IS - 15 SP - 6731 EP - 6739 PB - American Chemical Society CY - Washington, DC AN - OPUS4-51147 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zocca, Andrea A1 - Müller, Bernd R. A1 - Laquai, René A1 - Kupsch, Andreas A1 - Wieder, Frank A1 - Benemann, Sigrid A1 - Wilbig, Janka A1 - Günster, Jens A1 - Bruno, Giovanni T1 - Microstructural characterization of AP40 apatite-wollastonite glass-ceramic N2 - The microstructure of an apatite-wollastonite (code name AP40) glass-ceramic is analyzed in this study by combining 2D microscopy, phase analysis, X-ray absorption and synchrotron X-ray refraction computed tomography (XCT and SXRCT, respectively). It is shown that this combination provides a useful toolbox to characterize the global microstructure in a wide scale range, from sub-micrometer to millimeter. The material displays a complex microstructure comprising a glassy matrix with embedded fluorapatite and wollastonite small crystals. In this matrix, large (up to 200 μm) spike-shaped structures are distributed. Such microstructural features are oriented around a central sphere, thereby forming a structure resembling a sea urchin. A unique feature of SXRCT, in contrast to XCT, is that internal interfaces are visualized; this allows one to show the 3D distribution of these urchins with exceptionally good contrast. Furthermore, it is revealed that the spike-shaped structures are not single crystals, but rather composed of sub-micrometric crystals, which are identified as fluorapatite and diopside phases by SEM-EDX analysis. KW - Glass-ceramic KW - X-ray refraction KW - Computed tomography KW - Microstructure PY - 2023 DO - https://doi.org/10.1016/j.ceramint.2022.12.130 SN - 0272-8842 VL - 49 IS - 8 SP - 12672 EP - 12679 PB - Elsevier Science CY - Amsterdam AN - OPUS4-57452 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Zimmermann, Yoel A1 - Bazgir, Adib A1 - Al-Feghali, Alexander A1 - Ansari, Mehrad A1 - Bocarsly, Joshua A1 - Brinson, L. Catherine A1 - Chiang, Yuan A1 - Circi, Defne A1 - Chiu, Min-Hsueh A1 - Daelman, Nathan A1 - Evans, Matthew L. A1 - Gangan, Abhijeet S. A1 - George, Janine A1 - Harb, Hassan A1 - Khalighinejad, Ghazal A1 - Khan, Sartaaj Takrim A1 - Klawohn, Sascha A1 - Lederbauer, Magdalena A1 - Mahjoubi, Soroush A1 - Mohr, Bernadette A1 - Moosavi, Seyed Mohamad A1 - Naik, Aakash A1 - Ozhan, Aleyna Beste A1 - Plessers, Dieter A1 - Roy, Aritra A1 - Schöppach, Fabian A1 - Schwaller, Philippe A1 - Terboven, Carla A1 - Ueltzen, Katharina A1 - Wu, Yue A1 - Zhu, Shang A1 - Janssen, Jan A1 - Li, Calvin A1 - Foster, Ian A1 - Blaiszik, Ben T1 - 34 Examples of LLM Applications in Materials Science and Chemistry: Towards Automation, Assistants, Agents, and Accelerated Scientific Discovery N2 - Large Language Models (LLMs) are reshaping many aspects of materials science and chemistry research, enabling advances in molecular property prediction, materials design, scientific automation, knowledge extraction, and more. Recent developments demonstrate that the latest class of models are able to integrate structured and unstructured data, assist in hypothesis generation, and streamline research workflows. To explore the frontier of LLM capabilities across the research lifecycle, we review applications of LLMs through 34 total projects developed during the second annual Large Language Model Hackathon for Applications in Materials Science and Chemistry, a global hybrid event. These projects spanned seven key research areas: (1) molecular and material property prediction, (2) molecular and material design, (3) automation and novel interfaces, (4) scientific communication and education, (5) research data management and automation, (6) hypothesis generation and evaluation, and (7) knowledge extraction and reasoning from the scientific literature. Collectively, these applications illustrate how LLMs serve as versatile predictive models, platforms for rapid prototyping of domain-specific tools, and much more. In particular, improvements in both open source and proprietary LLM performance through the addition of reasoning, additional training data, and new techniques have expanded effectiveness, particularly in low-data environments and interdisciplinary research. As LLMs continue to improve, their integration into scientific workflows presents both new opportunities and new challenges, requiring ongoing exploration, continued refinement, and further research to address reliability, interpretability, and reproducibility. KW - Automation KW - LLM KW - Machine Learning KW - Agent KW - Bonding Analysis KW - Materials Searches KW - Finetuning PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-631720 DO - https://doi.org/10.48550/arXiv.2505.03049 SP - 1 EP - 33 AN - OPUS4-63172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zimmermann, Yoel A1 - Bazgir, Adib A1 - Al-Feghali, Alexander A1 - Ansari, Mehrad A1 - Bocarsly, Joshua A1 - Brinson, L Catherine A1 - Chiang, Yuan A1 - Circi, Defne A1 - Chiu, Min-Hsueh A1 - Daelman, Nathan A1 - Evans, Matthew A1 - Gangan, Abhijeet S A1 - George, Janine A1 - Harb, Hassan A1 - Khalighinejad, Ghazal A1 - Takrim Khan, Sartaaj A1 - Klawohn, Sascha A1 - Lederbauer, Magdalena A1 - Mahjoubi, Soroush A1 - Mohr, Bernadette A1 - Mohamad Moosavi, Seyed A1 - Naik, Aakash Ashok A1 - Ozhan, Aleyna Beste A1 - Plessers, Dieter A1 - Roy, Aritra A1 - Schoeppach, Fabian A1 - Schwaller, Philippe A1 - Terboven, Carla A1 - Ueltzen, Katharina A1 - Wu, Yue A1 - Zhu, Shang A1 - Janssen, Jan A1 - Li, Calvin A1 - Foster, Ian A1 - Blaiszik, Ben T1 - 32 examples of LLM applications in materials science and chemistry: towards automation, assistants, agents, and accelerated scientific discovery N2 - Large Language Models (LLMs) are reshaping many aspects of materials science and chemistry research, enabling advances in molecular property prediction, materials design, scientific automation, knowledge extraction, and more. Recent developments demonstrate that the latest class of models are able to integrate structured and unstructured data, assist in hypothesis generation, and streamline research workflows. To explore the frontier of LLM capabilities across the research lifecycle, we review applications of LLMs through 34 total projects developed during the second annual Large Language Model Hackathon for Applications in Materials Science and Chemistry, a global hybrid event. These projects spanned seven key research areas: (1) molecular and material property prediction, (2) molecular and material design, (3) automation and novel interfaces, (4) scientific communication and education, (5) research data management and automation, (6) hypothesis generation and evaluation, and (7) knowledge extraction and reasoning from the scientific literature. Collectively, these applications illustrate how LLMs serve as versatile predictive models, platforms for rapid prototyping of domain-specific tools, and much more. In particular, improvements in both open source and proprietary LLM performance through the addition of reasoning, additional training data, and new techniques have expanded effectiveness, particularly in low-data environments and interdisciplinary research. As LLMs continue to improve, their integration into scientific workflows presents both new opportunities and new challenges, requiring ongoing exploration, continued refinement, and further research to address reliability, interpretability, and reproducibility. KW - Large Language Models KW - Machine Learning KW - Materials Design KW - Bonding Analysis KW - Phonons KW - Thermal properties PY - 2025 DO - https://doi.org/10.1088/2632-2153/ae011a SN - 2632-2153 VL - 6 IS - 3 SP - 1 EP - 34 PB - IOP Publishing AN - OPUS4-64019 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhuang, Yiling A1 - Haderlein, Stefan B. A1 - Lutze, Holger V. A1 - Sun, Chen A1 - Fink, Friedrich A1 - Paul, Andrea A1 - Spahr, Stephanie T1 - Persulfate activation by biochar for trace organic contaminant removal from urban stormwater N2 - Persistent and mobile trace organic contaminants (TrOCs) in urban stormwater are difficult to remove through sedimentation- or sorption-based treatment and pose a risk to aquatic ecosystems and drinking water supplies. We demonstrate that the chemical oxidant peroxydisulfate (PDS) can be activated by shrimp shell biochar at pH 7 to form reactive species that selectively react with widespread stormwater contaminants. Of 11 TrOCs tested, oxidative transformation was observed for 1,3-diphenylguanidine, 2-hydroxybenzothiazole, 1H-benzotriazole, 5-methyl-benzotriazole, and diuron during water treatment with biochar and PDS. Laboratory batch experiments conducted with street runoff and a synthetic water showed that the water matrix, containing up to 7.5 mg L-1 dissolved organic carbon and 100 mM chloride, had a minor effect on the formation of reactive species and contaminant transformation. Using a set of scavengers and probe compounds, we provide evidence for singlet oxygen (1O2) as the predominant reactive species in the biochar/PDS system, which is in agreement with the selectivity of the process to oxidize electron-rich organic contaminants. The results of our study inform new strategies for stormwater treatment using heterogeneous oxidation processes for the abatement of persistent and mobile organic contaminants. KW - Stormwater treatment KW - Oxidation processes KW - Pyrogenic carbon PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637952 DO - https://doi.org/10.1016/j.watres.2025.123921 SN - 0043-1354 VL - 284 SP - 1 EP - 8 PB - Elsevier Ltd. AN - OPUS4-63795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhu, L. A1 - Srinivasan, P. A1 - Gong, Y. A1 - Hickel, Tilmann A1 - Grabowski, B. A1 - Körmann, Fritz A1 - Neugebauer, J. T1 - Melting properties of the refractory metals V and W and the binary VW alloy fully from first principles N2 - We investigate the melting properties of the bcc refractory metals V and W, and the disordered equiatomic VW alloy from first principles. We show that thermal vibrations have a large impact on the electronic density of states (DOS) and thus considerably affect the electronic contribution to the free energy. For W, the impact of vibrations on the electronic free energy of solid and liquid is different. This difference substantially impacts the computed melting point and also triggers a large electronic heat capacity difference between solid and liquid. For V, although vibrations likewise affect the electronic free energy, the effect on the melting properties cancels out to a large degree. For the binary VW alloy we observe a similar impact as for W, but slightly weaker. The underlying physics is explained in terms of the electronic DOS of the solid and liquid phases. Based on our accurate first-principles results, we reveal critical limitations of the Sommerfeld approximation in predicting the electronic heat KW - Crystal melting KW - Thermodynamics KW - Metals KW - Ab initio molecular dynamics KW - Density functional theory PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618100 DO - https://doi.org/10.1103/PhysRevB.109.094110 SN - 2469-9950 VL - 109 IS - 9 SP - 1 EP - 18 PB - American Physical Society (APS) AN - OPUS4-61810 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhou, X. A1 - Mathews, P. A1 - Berkels, B. A1 - Delis, W. A1 - Saood, S. A1 - Alhassan, A. A1 - Keuter, P. A1 - Schneider, J. A1 - Korte-Kerzel, S. A1 - Sandlöbes, S. A1 - Raabe, D. A1 - Neugebauer, j. A1 - Dehm, G. A1 - Hickel, Tilmann A1 - Scheu, C. A1 - Zhang, S. T1 - Materials Design by Constructing Phase Diagrams for Defects N2 - Phase transformations and crystallographic defects are two essential tools todrive innovations in materials. Bulk materials design via tuning chemicalcompositions is systematized using phase diagrams. It is shown here that thesame thermodynamic concept can be applied to manipulate the chemistry atdefects. Grain boundaries in Mg–Ga system are chosen as a model system,because Ga segregates to the boundaries, while simultaneously improving thestrength and ductility of Mg alloys. To reveal the role of grain boundaries,correlated atomic-scale characterization and simulation to scope and buildphase diagrams for defects are presented. The discovery is enabled bytriggering phase transformations of individual grain boundaries through localalloying, and sequentially imaging the structural and chemical changes usingatomic-resolution scanning transmission electron microscopy. Ab initiosimulations determined the thermodynamic stability of grain boundaryphases, and found out that increasing Ga content enhances grain boundarycohesion, relating to improved ductility. The methodology to trigger, trace,and simulate defect transformation at atomic resolution enables a systematicdevelopment of defect phase diagrams, providing a valuable tool to utilizechemical complexity and phase transformations at defects. KW - Automatic pattern recognition KW - Defect phase diagram KW - Density functional theory KW - Grain boundary complexion KW - Transmission electron microscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618063 DO - https://doi.org/10.1002/adma.202402191 SN - 1521-4095 SP - 1 EP - 9 PB - Wiley AN - OPUS4-61806 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhao, H. A1 - Chakraborty, Poulami A1 - Ponge, D. A1 - Hickel, Tilmann A1 - Sun, B. A1 - Wu, C.-H. A1 - Gault, B. A1 - Raabe, D. T1 - Hydrogen trapping and embrittlement in high-strength Al alloys N2 - Ever more stringent regulations on greenhouse gas emissions from transportation motivate efforts to revisit materials used for vehicles. High-strength aluminium alloys often used in aircrafts could help reduce the weight of automobiles, but are susceptible to environmental degradation. Hydrogen ‘embrittlement’ is often indicated as the main culprit; however, the exact mechanisms underpinning failure are not precisely known: atomic-scale analysis of H inside an alloy remains a challenge, and this prevents deploying alloy design strategies to enhance the durability of the materials. Here we performed near-atomic-scale analysis of H trapped in second-phase particles and at grain boundaries in a high-strength 7xxx Al alloy. We used these observations to guide atomistic ab initio calculations, which show that the co-segregation of alloying elements and H favours grain boundary decohesion, and the strong partitioning of H into the second-phase particles removes solute H from the matrix, hence preventing H embrittlement. Our insights further advance the mechanistic understanding of H-assisted embrittlement in Al alloys, emphasizing the role of H traps in minimizing cracking and guiding new alloy design. KW - Atomistic models KW - Hydrogen KW - Metals and alloys KW - Mechanical properties PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543631 DO - https://doi.org/10.1038/s41586-021-04343-z SN - 1476-4687 VL - 602 IS - 7897 SP - 437 EP - 441 PB - Nature Publ. Group CY - London AN - OPUS4-54363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, X. A1 - Zhang, J. A1 - Wang, H. A1 - Rogal, J: A1 - Li, H.-Y. A1 - Wei, S.-H. A1 - Hickel, Tilmann T1 - Defect-characterized phase transition kinetics N2 - Phase transitions are a common phenomenon in condensed matter and act as a critical degree of freedom that can be employed to tailor the mechanical or electronic properties of materials. Understanding the fundamental mechanisms of the thermodynamics and kinetics of phase transitions is, thus, at the core of modern materials design. Conventionally, studies of phase transitions have, to a large extent, focused on pristine bulk phases. However, realistic materials exist in a complex form; their microstructures consist of different point and extended defects. The presence of defects impacts the thermodynamics and kinetics of phase transitions, but has been commonly ignored or treated separately. In recent years, with the significant advances in theoretical and experimental techniques, there has been an increasing research interest in modeling and characterizing how defects impact or even dictate phase transitions. The present review systematically discusses the recent progress in understanding the kinetics of defect-characterized phase transitions, derives the key mechanisms underlying these phase transitions, and envisions the remaining challenges and fruitful research directions. We hope that these discussions and insights will help to inspire future research and development in the field. KW - Kinetics KW - Atomistic models KW - Phase transitions KW - Defects PY - 2022 DO - https://doi.org/10.1063/5.0117234 SN - 1931-9401 VL - 9 IS - 4 SP - 1 EP - 42 PB - AIP CY - New York, NY AN - OPUS4-56507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Runze A1 - Sur, Debashish A1 - Li, Kangming A1 - Witt, Julia A1 - Black, Robert A1 - Whittingham, Alexander A1 - Scully, John R. A1 - Hattrick-Simpers, Jason T1 - Bayesian assessment of commonly used equivalent circuit models for corrosion analysis in electrochemical impedance spectroscopy N2 - Electrochemical Impedance Spectroscopy (EIS) is a crucial technique for assessing corrosion of metallic materials. The analysis of EIS hinges on the selection of an appropriate equivalent circuit model (ECM) that accurately characterizes the system under study. In this work, we systematically examined the applicability of three commonly used ECMs across several typical material degradation scenarios. By applying Bayesian Inference to simulated corrosion EIS data, we assessed the suitability of these ECMs under different corrosion conditions and identified regions where the EIS data lacks sufficient information to statistically substantiate the ECM structure. Additionally, we posit that the traditional approach to EIS analysis, which often requires measurements to very low frequencies, might not be always necessary to correctly model the appropriate ECM. Our study assesses the impact of omitting data from low to medium-frequency ranges on inference results and reveals that a significant portion of low-frequency measurements can be excluded without substantially compromising the accuracy of extracting system parameters. Further, we propose simple checks to the posterior distributions of the ECM components and posterior predictions, which can be used to quantitatively evaluate the suitability of a particular ECM and the minimum frequency required to be measured. This framework points to a pathway for expediting EIS acquisition by intelligently reducing low-frequency data collection and permitting on-the-fly EIS measurements. KW - Electrochemical Impedance Spectroscopy (EIS) KW - MAPz@BAM KW - Bayesian Inference KW - Corrosion PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623392 DO - https://doi.org/10.1038/s41529-024-00537-8 VL - 8 SP - 120 PB - Springer Materials AN - OPUS4-62339 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Qiang A1 - Heuchel, Matthias A1 - Thünemann, Andreas A1 - Machatscheck, Rainhard T1 - The role of diffusion in the hydrolytic degradation of poly(lactic-co-glycolic acid): A molecular perspective N2 - This research emphasizes the importance of internal surface erosion as a key factor in the hydrolytic degradation of PLGA (poly(D,L-lactic-co-glycolic acid)) providing an alternative view of the established surface and bulk erosion degradation modes. Using molecular dynamics (MD) simulations, this study reveals the role of water and oligomer diffusion during the degradation of PLGA and highlights the importance of water channels formed as the overall water content increases. We found that these continuous water channels play a crucial role in accelerating the transport of water and the release of degradation products from the polymer matrix, as the diffusion coefficients of water and small oligomers exhibit significant differences spanning 2 to 3 orders of magnitude between the water and polymer phases. Water follows a different diffusion mechanism than polymer fragments. The diffusion rate of the fragments up to a size of octamers was found to be size-dependent and reasonably well approximated by a 1/N behavior, in line with the Rouse model. KW - Small-angle X-ray scattering KW - SAXS KW - Nanostructure KW - PLGA PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621250 DO - https://doi.org/10.1016/j.polymdegradstab.2024.111119 VL - 232 SP - 1 EP - 12 PB - Elsevier Ltd. AN - OPUS4-62125 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Kun A1 - Carrod, Andrew J. A1 - Del Giorgio, Elena A1 - Hughes, Joseph A1 - Rurack, Knut A1 - Bennet, Francesca A1 - Hodoroaba, Vasile-Dan A1 - Harrad, Stuart A1 - Pikramenou, Zoe T1 - Luminescence Lifetime-Based Sensing Platform Based on Cyclometalated Iridium(III) Complexes for the Detection of Perfluorooctanoic Acid in Aqueous Samples N2 - Luminescence lifetimes are an attractive analytical method for detection due to its high sensitivity and stability. Iridium probes exhibit luminescence with long excited-state lifetimes, which are sensitive to the local environment. Perfluorooctanoic acid (PFOA) is listed as a chemical of high concern regarding its toxicity and is classified as a “forever chemical”. In addition to strict limits on the presence of PFOA in drinking water, environmental contamination from industrial effluent or chemical spills requires rapid, simple, accurate, and cost-effective analysis in order to aid containment. Herein, we report the fabrication and function of a novel and facile luminescence sensor for PFOA based on iridium modified on gold surfaces. These surfaces were modified with lipophilic iridium complexes bearing alkyl chains, namely, IrC6 and IrC12, and Zonyl-FSA surfactant. Upon addition of PFOA, the modified surfaces IrC6-FSA@Au and IrC12-FSA @Au show the largest change in the red luminescence signal with changes in the luminescence lifetime that allow monitoring of PFOA concentrations in aqueous solutions. The platform was tested for the measurement of PFOA in aqueous samples spiked with known concentrations of PFOA and demonstrated the capacity to determine PFOA at concentrations >100 μg/L (240 nM). KW - Perfluorooctanoic Acid (PFOA) KW - Cyclometalated iridium (III) complexes KW - Luminescent lifetime KW - Optically active surfaces KW - ToF-SIMS PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594535 UR - https://pubs.acs.org/doi/10.1021/acs.analchem.3c04289 DO - https://doi.org/10.1021/acs.analchem.3c04289 VL - 96 IS - 4 SP - 1565 EP - 1575 PB - American Chemical Society (ACS) AN - OPUS4-59453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zarinwall, A. A1 - Waniek, Tassilo A1 - Saadat, R. A1 - Braun, U. A1 - Sturm, Heinz A1 - Garnweitner, G. T1 - Comprehensive Characterization of APTES Surface Modifications of Hydrous Boehmite Nanoparticles N2 - Hydrous boehmite (γ-AlOOH) nanoparticles (BNP) show great potential as nanoscale filler for the fabrication of fiber reinforced nanocomposite materials. Notably, the particle−matrix interaction has been demonstrated to be decisive for improving the matrix-dominant mechanical properties in the past years. Tailoring the surface properties of the nanofiller enables to selectively design the interaction and thus to exploit the benefits of the nanocomposite in an optimal way. Here, an extensive study is presented on the binding of (3-aminopropyl)triethoxysilane (APTES), a common silane surface modifier, on BNP in correlation to different process parameters (concentration, time, temperature, and pH). Furthermore, a comprehensive characterization of the modified BNP was performed by using elemental analysis (EA), thermogravimetric analysis (TGA) coupled with mass spectrometry (TGA-MS), and Kaiser’s test (KT). The results show an increasing monolayer formation up to a complete surface coverage with rising APTES concentration, time, and temperature, resulting in a maximal grafting density of 1.3 molecules/nm². Unspecific multilayer formation was solely observed under acidic conditions. Comparison of TGA-MS results with data recorded from EA, TGA, and KT verified that TGA-MS is a convenient and highly suitable method to elucidate the ligand binding in detail. KW - Boehmite KW - Nanoparticle KW - Surface KW - APTES KW - Functionalization KW - BET KW - TGA KW - Grafting KW - Nanocomposite KW - Silane PY - 2020 DO - https://doi.org/10.1021/acs.langmuir.0c02682 VL - 37 IS - 1 SP - 171 EP - 179 PB - ACS Publications AN - OPUS4-51954 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Zarinwall, A. A1 - Waniek, Tassilo A1 - Finke, B. A1 - Sadaat, R. A1 - Sturm, Heinz A1 - Garnweitner, G. ED - Sinapius, M. ED - Ziegmann, G. T1 - Particle Surface Modification N2 - Whilst a decisive role of the particle-matrix interphase on the mechanical properties of nanoparticle-filled polymers has been demonstrated in the last years, the arbitrary design of this interphase remains a very challenging goal. In principle, this could be realized via an appropriate surfacemodification of the nanofiller prior to its incorporation in the polymer. For most systems, such as for boehmite nanofillers, however, the interaction of organic modifiers with the particle surface has not been studied in detail, and only single studies are known rather than systematic investiga- tions on the effects of different chemical functions anchored on the particle surface. In this chapter, we present an extensive study on the binding of APTES, a common silane surface modifier, with boehmite, and show that thermogravimetric analysis (TGA) coupled with mass spectrometry (MS) is a convenient and highly suitable method to elucidate the ligand binding in detail. Furthermore, a two-step coupling strategy is presented, demonstrating that based on APTES anchored to the parti- cle surface, the condensation of various carboxylic acids can be utilized to enable highly diverse chemical properties of the nanofillers, which leads to very different particle-matrix interactions in the nanocomposites. KW - APTES KW - Boehmite KW - Nanoparticle KW - TGA-MS PY - 2021 SN - 978-3-030-68522-5 SN - 978-3-030-68523-2 DO - https://doi.org/10.1007/978-3-030-68523-2 SN - 2194-8240 SN - 2194-8259 SP - 119 EP - 142 PB - Springer Nature Switzerland AG CY - Cham AN - OPUS4-53727 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yusenko, Kirill A1 - Zvereva, V. A1 - Martynova, S. A1 - Asanov, I. A1 - La Fontaine, C. A1 - Roudenko, O. A1 - Gubanov, A. A1 - Plyusnin, P. A1 - Korenev, S. A1 - Asanova, T. T1 - Insight of the thermal decomposition of ammonium hexahalogenoiridates(IV) and hexachloroiridate(III) N2 - Thermal decomposition of (NH4)3[IrCl6]·H2O, (NH4)2[IrCl6] and (NH4)2[IrBr6] in reductive and inert atmospheres has been investigated in situ using quick-EXAFS and temperature-resolved powder X-ray diffraction. For the first time, (NH4)2[Ir(NH3)Cl5] and (NH4)2[Ir(NH3)Br5] have been proven as intermediates of thermal decomposition of (NH4)3[IrCl6]·H2O, (NH4)2[IrCl6] and (NH4)2[IrBr6]. Thermal degradation of (NH4)2[IrCl6] and (NH4)2[IrBr6] is a more complex process as suggested previously and includes simultaneous formation of (NH4)2[Ir(NH3)Cl5] and (NH4)2[Ir(NH3)Br5] intermediates mixed with metallic iridium. In the inert atmosphere, complexes (NH4)[Ir(NH3)2Cl4] and (NH4)[Ir(NH3)2Br4] as well as [Ir(NH3)3Br3] were proposed as possible intermediates before formation of metallic iridium particles KW - Thermal decomposition KW - Iridium compounds KW - EXAFS KW - In situ PXRD PY - 2020 DO - https://doi.org/10.1039/D0CP02743J VL - 22 IS - 40 SP - 22923 EP - 22934 AN - OPUS4-51224 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yusenko, Kirill A1 - Sukhikh, A. A1 - Kraus, Werner A1 - Gromilov, S. T1 - Synthesis and Crystal Chemistry of Octahedral Rhodium(III) Chloroamines N2 - Rhodium(III) octahedral complexes with amine and chloride ligands are the most common starting compounds for preparing catalytically active rhodium(I) and rhodium(III) species. Despite intensive study during the last 100 years, synthesis and crystal structures of rhodium(III) complexes were described only briefly. Some [RhClx(NH3)6-x] compounds are still unknown. In this study, available information about synthetic protocols and the crystal structures of possible [RhClx(NH3)6−x] octahedral species are summarized and critically analyzed. Unknown crystal structuresof(NH4)2[Rh(NH3)Cl5],trans–[Rh(NH3)4Cl2]Cl·H2O,andcis–[Rh(NH3)4Cl2]Clarereported based on high quality single crystal X-ray diffraction data. The crystal structure of [Rh(NH3)5Cl]Cl2 was redetermined. All available crystal structures with octahedral complexes [RhClx(NH3)6-x] were analyzed in terms of their packings and pseudo-translational sublattices. Pseudo-translation lattices suggest face-centered cubic and hexagonal closed-packed sub-cells, where Rh atoms occupy nearly ideal lattices. KW - Pseudo-translationalsublattices KW - Rhodiumcomplexes KW - Ligandsubstitution KW - Crystalstructure PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508194 DO - https://doi.org/10.3390/molecules25040768 VL - 25 IS - 4 SP - 768 PB - MDPI CY - Basel AN - OPUS4-50819 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -