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 - 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 - 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 - JOUR A1 - Yesilcicek, Yasemin A1 - Haas, S. A1 - Suárez Ocano, Patricia A1 - Zaiser, E. A1 - Hesse, René A1 - Többens, D. M. A1 - Glatzel, U. A1 - Manzoni, Anna Maria T1 - Controlling Lattice Misfit and Creep Rate Through the γ' Cube Shapes in the Al10Co25Cr8Fe15Ni36Ti6 Compositionally Complex Alloy with Hf and W Additions N2 - Trace elements play an important role in the fine-tuning of complex material properties. This study focuses on the correlation of microstructure, lattice misfit and creep properties. The compositionally complex alloy Al10Co25Cr8Fe15Ni36Ti6 (in at. %) was tuned with high melting trace elements Hf and W. The microstructure consists of a γ matrix, γ' precipitates and the Heusler phase and it is accompanied by good mechanical properties for high temperature applications. The addition of 0.5 at.% Hf to the Al10Co25Cr8Fe15Ni36Ti6 alloy resulted in more sharp-edged cubic γ′ precipitates and an increase in the Heusler phase amount. The addition of 1 at.% W led to more rounded γ′ precipitates and the dissolution of the Heusler phase. The shapes of the γ' precipitates of the alloys Al9.25Co25Cr8Fe15Ni36Ti6Hf0.25W0.5 and Al9.25Co25Cr8Fe15Ni36Ti6Hf0.5W0.25, that are the alloys of interest in this paper, create a transition from the well-rounded precipitates in the alloy with 1% W containing alloy to the sharp angular particles in the alloy with 0.5% Hf. While the lattice misfit has a direct correlation to the γ' precipitates shape, the creep rate is also related to the amount of the Heusler phase. The lattice misfit increases with decreasing corner radius of the γ' precipitates. So does the creep rate, but it also increases with the amount of Heusler phase. The microstructures were investigated by SEM and TEM, the lattice misfit was calculated from the lattice parameters obtained by synchrotron radiation measurements. KW - High entropy alloy KW - Lattice misfit KW - Creep KW - Transmission electron microscopy KW - X-ray diffraction PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565655 DO - https://doi.org/10.1007/s44210-022-00009-1 SP - 1 EP - 9 PB - Springer AN - OPUS4-56565 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Werner, Tiago A1 - Teske, Tanita A1 - Hilgenberg, Kai A1 - Mauro, Madia A1 - Nielsen, S. A1 - Gärtner, F. A1 - Klassen, T. T1 - Untersuchung des Potenzials von Kaltgasspritzen für die Reparatur zyklisch belasteter Bauteile T1 - Investigation on the capability of cold-spray for repair of cyclically loaded components N2 - Die Reparatur mittels Kaltgasspritzen ist eine vielversprechende Alternative zum teuren Austausch fehlerbehafteter Bauteile in der Luft- und Raumfahrt. Im Rahmen dieser Arbeit wurde das Potential des Verfahrens an der hochfesten Aluminiumlegierungen Al6061-T6 unter Anwendung von Stickstoff als kostengünstiges Prozessgas untersucht. Es wurden quasi-statische Zugversuche und einachsige Zeitfestigkeitsversuche mit besonderem Fokus auf das in-situ Kugelstrahlen zur Verbesserung der mechanischen Eigenschaften durchgeführt. Im Ergebnis wurde die Verbesserung der Adhäsion zwischen Substrat und aufgebautem Werkstoff als entscheidendes Kriterium für eine Anwendbarkeit ermittelt. Die Laserstrukturierung von Substratoberflächen ist hierfür vielversprechend und wurde im Rahmen der Arbeit mittels Adhäsionsversuchen untersucht. N2 - Repair by cold-spray is a promising alternative to the costly replacement of flawed components in aerospace applications. In the present work this process was investigated on the high-strength aluminum alloy Al6061-T6. For the cold-spray process, inexpensive Nitrogen was used as process-gas. Quasi-static tensile and highcycle- fatigue tests (HCF) were performed, focusing on in-situ shot peening to improve the mechanical properties of the repaired part. An improved adhesion between substrate and built-up material was identified as a key-factor for the applicability of the process. Under this respect laser-structuring of the substrate surface was applied and its effect on the mechanical performance of the restored samples were examined by adhesion tests. T2 - 9. Tagung des DVM-Arbeitskreises Additiv gefertigte Bauteile und Strukturen CY - Stuttgart, Germany DA - 06.11.2024 KW - Kaltgasspritzen KW - cold-spray KW - Reparatur KW - Repair KW - Ermüdungsfestigkeit KW - Fatigue KW - Luft- und Raumfahrt KW - Aerospace KW - Substratvorbehandlung KW - Substrate pre-treatment PY - 2024 DO - https://doi.org/10.48447/ADD-2024-BB VL - 409 SP - 67 EP - 79 AN - OPUS4-63182 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waske, Anja T1 - A unique authenticator for additively manufactured parts derived from their microstructure N2 - In the field of additive manufacturing, the ability to uniquely identify and authenticate parts is crucial for certification, logistics, and anti-counterfeiting efforts. This study introduces a novel methodology that leverages the intrinsic microstructural features of additively manufactured components for their identification, authentication, and traceability. Unlike traditional tagging methods, such as embedding QR codes on the surface [1] or within the volume of parts, this approach requires no alteration to the printing process, as it utilizes naturally occurring microstructural characteristics. The proposed workflow [2] involves the analysis of 3D micro-computed tomography data to identify specific voids that meet predefined identification criteria. This method is demonstrated on a batch of 20 parts manufactured with identical process parameters, proving capable of achieving unambiguous identification and authentication. By establishing a tamper-proof link between the physical part and its digital counterpart, this methodology effectively bridges the physical and digital realms. This not only enhances the traceability of additively manufactured parts but also provides a robust tool for integrating digital materials, parts databases, and product passports with their physical counterparts. T2 - Artificial Intelligence in MSE CY - Bochum, Germany DA - 18.11.2025 KW - Authentication KW - Additive Manufacturing KW - Non-destructive testing PY - 2025 AN - OPUS4-65204 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trappe, Volker T1 - Roving-Alterung und mechanische Eigenschaften N2 - Im statistischen Mittel steht eine Windkraftanlage (WKA) in Deutschland alle 6 Jahre wegen eines Schadens an den Rotorblättern und verursacht Kosten von 20k€-40k€ infolge Ertragsausfall und Reparaturkosten. Bei über 30.000 WKA in Deutschland verursacht dies jährlichen Kosten von 100-200 Mio. €. Zu 70% sind die Ursachen Fertigungsfehler. Diesem Themenkomplex widmet sich FB-5.3 in Kooperation mit FBs der Zerstörungsfreien Prüfung (Abt. 8) schon seit Jahren. Im aktuellen Projekt geht es um einen vorzeitigen Verschleiß der Rotorblätter infolge der Verwendung gealterter Glasfaser-Rovings. (GF). Die Entwicklung moderner Windkraftanlagen hatte in Europa seinen Ursprung in den 90er Jahren. OEMs und GF-Hersteller waren dicht beisammen. Die Globalisierung des Marktes führt heute zu einer weltweiten Verschiffung der GF in feucht-warmen Containern. Je nach Beschaffenheit (Chemie) der Schlichten (Oberflächenbehandlung) von GF können diese stark altern (Hydrolyse-Effekte) und die Festigkeit kann im Bauteil um bis zu 50% abgemindert sein. In einer Kooperation mit der Rotorblattallianz, einem Zusammenschluss der OEMs, Halbzeugherstellern und Forschungsinstituten, wurden schon vor 5 Jahren in einem Forschungsprojekt (FB-5.3; VH 5538) die chemischen Mechanismen der Alterung exemplarisch für eine Glasfaser-Roving-Type aufgeklärt. Im aktuellen Projekt (FB-5.3; VH 5304) wird ein beschleunigtes Alterungsverfahren (erhöhte Temperatur und Feuchte) am Roving im un-impregnierten Zustand entwickelt und die Festigkeit nachfolgend nach Einbettung in eine Epoxid-Harz-Matrix bestimmt. Je nach Alterungszustand zeigt sich eine Abnahme der Zwischenfaserbruchfestigkeit von bis zu 50%. Nicht alle Glasfaser-Roving-Typen zeigen diesen Effekt. Es ist gelungen für OEMs und Halbzeughersteller ein handhabbares Verfahren zur innerbetrieblichen Qualitätssicherung zu entwickeln, da die wenigsten Firmen über komplexe Analyseverfahren, wie an der BAM, verfügen. T2 - Composite United - AG Faserverbund in der Windenergie CY - Braunschweig, Germany DA - 09.05.2023 KW - Faserkunststoffverbunde KW - Windenergie KW - Alterung PY - 2023 AN - OPUS4-58409 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sänger, Johanna Christiane A1 - Pauw, Brian Richard A1 - Sturm, Heinz A1 - Günster, Jens T1 - First time additively manufactured advanced ceramics by using two-photon polymerization for powder processing N2 - Methods and materials are presented here, which enable the manufacturing of fine structures using a 3D-printing method known as two-photon polymerization (2PP). As traditional photolithography methods for structuring ceramic slurries do not function with 2PP, due to light scattering on ceramic particles, a novel water-based photoresist with high ceramic loading of extremely well dispersed ceramic nano particles was developed. This photoresist is basically a ceramic slurry containing a photocurable agent and a photoinitiator to be crosslinkable with the 780 nm wavelength femtosecond laser light source of the 2PP machine. It is demonstrated that it is possible to gain a highly transparent and low viscous slurry suitable for 2PP processing. This work shows the development of the slurry, first printing results and the post-printing processes required to form three dimensional ceramic microstructures consisting of alumina toughened zirconia (ATZ). KW - 3D-printing KW - Two-photon polymerization KW - 2PP KW - Ceramic nano particles KW - Slurry KW - Alumina toughened zirconia KW - ATZ KW - Additive manufacturing KW - SchwarzP cells KW - Nano-ceramic-additive-manufacturing photoresin KW - NanoCAM PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517441 DO - https://doi.org/10.1016/j.oceram.2020.100040 VL - 4 SP - 100040 PB - Elsevier Ltd. AN - OPUS4-51744 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ruehle, Bastian T1 - A Self-Driving Lab for Nano and Advanced Materials Synthesis in a Self-Driving Lab N2 - In this contribution, we present our Self-Driving Lab (SDL) for Nano and Advanced Materials, that integrates robotics for batched autonomous synthesis – from molecular precursors to fully purified nanomaterials – with automated characterization and data analysis, for a complete and reliable nanomaterial synthesis workflow. By fully automating the processing steps for seven different materials from five representative, completely different classes of nano- and advanced materials (metal, metal oxide, silica, metal organic framework, and core–shell particles) that follow different reaction mechanisms, we demonstrate the great versatility and flexibility of the platform. The system also exhibits high modularity and adaptability in terms of reaction scales and incorporates in-line characterization measurement of hydrodynamic diameter, zeta potential, and optical properties (absorbance, fluorescence). We discuss the excellent reproducibility of the various materials synthesized on the platform in terms of particle size and size distribution, and the adaptability and modularity that allows access to a diverse set of nanomaterial classes. We also present several key aspects of the central backend that orchestrates the (parallelized) syntheses workflows. One key feature is the resource management or “traffic control” for scheduling and executing parallel reactions in a multi-threaded environment. Another is the interface with data analysis algorithms from in-line, at-line, and off-line measurements. Here, we will give examples of how automatic image segmentation of electron microscopy images with the help of AI can be used for reducing the “data analysis bottleneck” from an off-line measurement. We will also discuss various machine learning (ML) algorithms that are currently implemented in the backend and can be used for ML-guided, closed-loop material optimization in our SDL. Lastly, we will show our recent efforts in making the workflow generation on SDLs more user-friendly by using large language models to generate executable workflows automatically from synthesis procedures given in natural language and user-friendly graphical user interfaces based on node editors that also allow for knowledge graph extraction from the workflows. In this context, we are currently also working on a common description or ontology for representing the process steps and parameters of the workflows, which will greatly facilitate the semantic description and interoperability of workflows between different SDL hardware and software platforms. T2 - Series on Digitalisation-Meet the Experts | Special Topic: Automation CY - Berlin, Germany DA - 27.02.2026 KW - Self-Driving Labs KW - Materials Acceleration Platforms KW - Advanced Materials KW - Nanomaterials KW - Automation KW - Digitalization PY - 2026 AN - OPUS4-65604 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Rosalie, Julian T1 - Small-angle scattering data analysis round robin - Anonymized results, figures and Jupyter notebook N2 - The intent of this round robin was to find out how comparable results from different researchers are, who analyse exactly the same processed, corrected dataset. This zip file contains the anonymized results and the jupyter notebook used to do the data processing, analysis and visualisation. Additionally, TEM images of the samples are included. KW - Round robin KW - Small-angle scattering KW - Data analysis PY - 2023 DO - https://doi.org/10.5281/zenodo.7509710 PB - Zenodo CY - Geneva AN - OPUS4-56803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Anker, A. S. A1 - Balazs, D. M. A1 - Beyer, F. L. A1 - Bienert, Ralf A1 - Bouwman, W. G. A1 - Breßler, Ingo A1 - Breternitz, J. A1 - Brok, E. S. A1 - Bryant, G. A1 - Clulow, A. J. A1 - Crater, E. R. A1 - De Geuser, F. A1 - Giudice, A. D. A1 - Deumer, J. A1 - Disch, S. A1 - Dutt, S. A1 - Frank, K. A1 - Fratini, E. A1 - Gilbert, E. P. A1 - Hahn, Marc Benjamin A1 - Hallett, J. A1 - Hohenschutz, Max A1 - Hollamby, M. J. A1 - Huband, S. A1 - Ilavsky, J. A1 - Jochum, J. K. A1 - Juelsholt, M. A1 - Mansel, B. W. A1 - Penttilä, P. A1 - Pittkowski, R. K. A1 - Portale, G. A1 - Pozzo, L. D. A1 - Ricardo de Abreu Furtado Garcia, P. A1 - Rochels, L. A1 - Rosalie, Julian A1 - Saloga, P. E. J. A1 - Seibt, S. A1 - Smith, A. J. A1 - Smith, G. N. A1 - Annadurai, V. A1 - Spiering, G. A. A1 - Stawski, Tomasz A1 - Taché, O. A1 - Thünemann, Andreas A1 - Toth, K. A1 - Whitten, A. E. A1 - Wuttke, J. T1 - The human factor - Results of a small-angle scattering data analysis round robin N2 - A Round Robin study has been carried out to estimate the impact of the human element in small-angle scattering data analysis. Four corrected datasets were provided to participants ready for analysis. All datasets were measured on samples containing spherical scatterers, with two datasets in dilute dispersions, and two from powders. Most of the 46 participants correctly identified the number of populations in the dilute dispersions, with half of the population mean entries within 1.5 % and half of the population width entries within 40 %, respectively. Due to the added complexity of the structure factor, much fewer people submitted answers on the powder datasets. For those that did, half of the entries for the means and widths were within 44 % and 86 % respectively. This Round Robin experiment highlights several causes for the discrepancies, for which solutions are proposed. KW - Round robin KW - Sall-angle scattering KW - Nanostructure quantification KW - Nanostructure KW - SAXS KW - MOUSE KW - X-ray scattering KW - Size distribution KW - Nanoparticles PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571342 DO - https://doi.org/10.48550/arXiv.2303.03772 SP - 1 EP - 23 PB - Cornell University CY - Ithaca, NY AN - OPUS4-57134 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mrkwitschka, Paul A1 - Abram, Sarah-Luise A1 - Thünemann, Andreas A1 - Rühle, Bastian A1 - Radnik, Jörg A1 - Bresch, Harald A1 - Resch-Genger, Ute A1 - Hodoroaba, Vasile-Dan T1 - The Role of Electron Microscopy in the Development of Monodisperse Cubic Iron Oxide Nanoparticles as Certified Reference Material for Size and Shape N2 - BAM is currently building up a platform of novel nanoRMs relying on iron oxide nanoparticles of different shape, size and surface chemistry. Iron oxide was chosen as a core material because of its relevance to the material and life sciences. As a first candidate of this series, we present cubic iron oxide nanoparticles with a nominal edge length of 8 nm. These particles were synthesized by thermal decomposition of iron oleate in high boiling organic solvents adapting well-known literature procedures. After dilution to a concentration suitable for electron microscopy (TEM and SEM) as well as for small-angle X-ray scattering (SAXS) measurements, the candidate nanoRM was bottled and assessed for homogeneity and stability by both methods following the guidelines of ISO 17034 and ISO Guide 35. The particle sizes obtained by both STEM-in-SEM and TEM are in excellent agreement with a minimum Feret of 8.3 nm ± 0.7 nm. The aspect ratio (AR) of the iron oxide cubes were extracted from the images as the ratio of minimum Feret to Feret resulting in an AR of 1.18 for TEM to 1.25 for SEM. Alternatively, a rectangular bounding box was fitted originating from the minimum Feret and the longest distance through the particle in perpendicular direction. This led to AR values of 1.05 for TEM and 1.12 for SEM, respectively. The results confirm the almost ideal cubic shape. KW - Reference nanoparticles KW - Iron oxide KW - Cubical shape KW - Electron microscopy KW - SAXS KW - Nano CRM KW - Size PY - 2022 DO - https://doi.org/10.1017/S1431927622003610 SN - 1435-8115 VL - 28 IS - Suppl. 1 SP - 802 EP - 805 PB - Cambridge University Press AN - OPUS4-55599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - The Role of Electron Microscopy in the Development of Monodisperse Cubic Iron Oxide Nanoparticles as CRM for Size and Shape N2 - Due to their unique physico-chemical properties, nanoparticles are well established in research and industrial applications. A reliable characterization of their size, shape, and size distribution is not only mandatory to fully understand and exploit their potential and develop reproducible syntheses, but also to manage environmental and health risks related to their exposure and for regulatory requirements. To validate and standardize methods for the accurate and reliable particle size determination nanoscale reference materials (nanoRMs) are necessary. However, there is only a very small number of nanoRMs for particle size offered by key distributors such as the National Institute of Standards and Technology (NIST) and the Joint Research Centre (JRC) and, moreover, few provide certified values. In addition, these materials are currently restricted to polymers, silica, titanium dioxide, gold and silver, which have a spherical shape except for titania nanorods. To expand this list with other relevant nanomaterials of different shapes and elemental composition, that can be used for more than one sizing technique, we are currently building up a platform of novel nanoRMs relying on iron oxide nanoparticles of different shape, size and surface chemistry. Iron oxide was chosen as a core material because of its relevance for the material and life sciences. T2 - Microscopy and Microanalysis 2022 CY - Online meeting DA - 31.07.2022 KW - Certified Referencematerial KW - Cubical Iron Oxide KW - Nanoparticles KW - Electron Microscopy KW - Small-Angle X-ray Scattering PY - 2022 AN - OPUS4-57035 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Comparative study of suitable preparation methods to evaluate irregular shaped, polydisperse nanoparticles by scanning electron microscopy (SEM). N2 - Reliable characterization of materials at the nanoscale regarding their physio-chemical properties is a challenging task, which is important when utilizing and designing nanoscale materials. Nanoscale materials pose a potential toxicological hazard to the environment and the human body. For this reason, the European Commission amended the REACH Regulation in 2018 to govern the classification of nanomaterials, relying on number-based distribution of the particle size. Suitable methods exist for the granulometric characterization of monodisperse and ideally shaped nanoparticles. However, the evaluation of commercially available nanoscale powders is problematic. These powders tend to agglomerate, show a wide particle size distribution and are of irregular particle shape. Zinc oxide, aluminum oxide and cerium oxide with particle sizes less than 100 nm were selected for the studies and different preparation methods were used comparatively. First, the nanoparticles were dispersed in different dispersants and prepared on TEM-supported copper grids. Furthermore, individual powders were deposited on carbon-based self-adhesive pads. In addition, the samples were embedded by hot mounting and then ground and polished. The prepared samples were investigated by scanning electron microscopy (including the transmission mode STEM-in-SEM) and Dynamic Light scattering. The software package ImageJ was used to segment the SEM images and obtain the particle sizes and shapes and finally the number-based particles size distribution with size expressed as various descriptors. T2 - Ceramics 2021 CY - Online meeting DA - 19.04.2021 KW - Nanoparticles KW - Preparation KW - Characterization PY - 2021 AN - OPUS4-53272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Fine iron oxide nanoparticles as a candidate reference material for reliable measurement of particle size N2 - Background, Motivation and Objective Nanomaterials are at the core of some of the 21st century’s most promising technologies. In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important. Furthermore, the European Commission has taken measures via the REACH Regulations to control the classification of nanomaterials. REACH Annexes which entered into force in January 2020 require manufacturers to register nanomaterials that are traded in larger quantities (at least 1 ton). Every powder or dispersion where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as a nanomaterial. This creates a need for both industrial manufacturers and research and analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is working on developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution, but also targeting other key parameters such as shape, structure (including porosity) and functional properties. Thus, candidate materials are considered to complement the already available spherical and monodisperse silica, Au and polystyrene reference nanoparticles, e.g. iron oxide and titanium oxide, with an average atomic number between those of silica and gold. Particularly for the imaging by electron microscopies, new nanoparticles of well-defined size in the range of 10 nm are decisive for the accurate particle segmentation by setting precise thresholds. Statement of Contribution/Methods Synthesis: Highly monodisperse iron oxide nanoparticles can be synthesized in large quantities by thermal decomposition of iron oleate or iron acetylacetonate precursors in high boiling solvents such as octadecene or dioctyl ether in the presence of oleic acid and oleylamine as capping agents. Scanning Electron Microscope: An SEM of type Supra 40 from Zeiss has been used including the dedicated measurement mode transmission in SEM (STEM-in-SEM) with a superior material contrast for the nanoparticle analysis. The software package ImageJ has been used for the analysis of the STEM-in-SEM images and to determine the particle size distribution. Dynamic Light scattering (DLS): Particles in suspension were measured in comparison by means of Zetasizer Nano (Malvern Panalytical; cumulants analysis) and NanoFlex (Microtrac; frequency power spectrum). Results/Discussion In this study iron oxide nanoparticles synthesized at BAM and pre-characterized by DLS, SEM (including the transmission mode STEM-in-SEM) are presented. The particles are spherical and highly monodisperse with sizes slightly larger than 10 nm. T2 - Nanosafe 2020 CY - Online meeting DA - 16.11.2020 KW - Reference nanomaterials KW - Imaging techniques KW - Size and size distribution KW - Reliable characterization KW - Iron oxide nanoparticles PY - 2020 AN - OPUS4-51767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -