TY - JOUR A1 - Unger, Wolfgang A1 - Stockmann, Jörg M. A1 - Senoner, Mathias A1 - Weimann, T. A1 - Bütefisch, S. A1 - Passiu, C. A1 - Spencer, N. D. A1 - Rossi, A. T1 - Introduction to lateral resolution and analysis area measurements in XPS N2 - Imaging and small-spot (small area) XPS have become increasingly important components of surface chemical analysis during the last three decades, and its use is growing. Some ambiguity in the use of terminology, understanding of concepts, and lack of appropriate reference materials leads to confusing and not always reproducible data. In this paper, it is shown that by using existing knowledge, appropriate test specimens, and standardized approaches, problems of comparability and such reproducibility issues recently observed for XPS data reported in the scientific literature can be overcome. The standardized methods of ISO 18516:2019, (i) the straight-edge, (ii) the narrow-line, and (iii) the grating method, can be used to characterize and compare the lateral resolution achieved by imaging XPS instruments and are described by reporting examples. The respective measurements are made using new test specimens. When running an XPS instrument in the small-spot (small area) mode for a quantitative analysis of a feature of interest, the question arises as to what contribution to the intensity originates from outside the analysis area. A valid measurement approach to control the intensity from outside the nominal analysis area is also described. As always, the relevant resolution depends on the specific question that needs to be addressed. The strengths and limitations of methods defining resolution are indicated. KW - Imaging XPS KW - Lateral resolution KW - Analysis area measurements KW - Small-spot XPS PY - 2020 DO - https://doi.org/10.1116/6.0000398 VL - 38 IS - 5 SP - 053206 AN - OPUS4-51394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Mast, J. A1 - Verleysen, E. A1 - Hodoroaba, Vasile-Dan A1 - Kaegi, R. ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Characterization of nanomaterials by transmission electron microscopy - Measurement procedures N2 - In this chapter, approaches are proposed for the descriptive and quantitative characterization of nano-objects with nanometer resolution. Measurements are based on the analysis of the characteristics of 2D projections of individual particles visualized on transmission electron micrographs. Incorporation of spectroscopic methods (EDS and EELS) for elemental analysis of nano-objects is recommended to identify subpopulations of nano-objects in mixtures based on their chemical composition. The focus lies on the determination of physicochemical properties which are essential in a legislatory and regulatory context to define the material as a nanomaterial (NM), and to assess its safety and toxicological potential, using widely accessible equipment. KW - Nanoparticles KW - Sample preparation KW - Image analysis KW - Transmission electron microscopy PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00004-3 SP - 29 EP - 48 PB - Elsevier CY - Amsterdam AN - OPUS4-50121 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Clifford, C. A1 - Stintz, M. A1 - Hodoroaba, Vasile-Dan A1 - Unger, Wolfgang A1 - Fujimoto, T. ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - International standards in nanotechnologies N2 - This chapter provides an overview of what standards are, why they are important, and how they are developed. There is a focus on the work of standards committees relevant to nanotechnology measurement and characterization with tables detailing the standards that are currently available for a large number of different techniques, materials, and applications at the nanoscale. KW - Standards KW - Nanotechnology KW - Reproducibility KW - ISO KW - CEN KW - VAMAS PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00026-2 SP - 511 EP - 525 PB - Elsevier CY - Amsterdam AN - OPUS4-50165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Shard, A. G. A1 - Hodoroaba, Vasile-Dan A1 - Unger, Wolfgang ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Introduction N2 - The purpose of this book is to provide a comprehensive collection of analytical methods that are commonly used to measure nanoparticles, providing information on one, or more, property of importance. The chapters provide up-to-date information and guidance on the use of these techniques, detailing the manner in which they may be reliably employed. Within this chapter, we detail the rationale and context of the whole book, which is driven by the observation of a low level of reproducibility in nanoparticle research. The aim of the book is to encourage awareness of both the strengths and weaknesses of the various methods used to measure nanoparticles and raise awareness of the range of methods that are available. The editors of the book have, for many years, been engaged in European projects and standardization activities concerned with nanoparticle analysis and have identified authors who are experts in the various methods included within the book. This has produced a book that can be used as a definitive guide to current best practice in nanoparticle measurement. KW - Nanoparticles KW - Size distribution KW - Shape KW - Chemistry KW - Coating KW - Concentration KW - Standards KW - Charge KW - Characterisation PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00001-8 SP - 1 EP - 6 PB - Elsevier CY - Amsterdam AN - OPUS4-50166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Titscher, Thomas A1 - Coehlo Lima, Isabela A1 - Unger, Jörg F. T1 - Model selection and model calibration for a digital twin N2 - The quality of a model - and thus its predictive capabilities - is influenced by numerous uncertainties. They include possibly unknown boundary and initial conditions, noise in the data used for its calibration and uncertainties in the model itself. Here, the latter part is not only restricted to uncertain model parameters, but also refers to the choice of the model itself. Inferring these uncertainties in an automatic way allows for an adaption of the model to new data sets and for a reliable, reproducible model assessment. Note that similar concepts apply at the structural level, where a continuously updated digital twin allows virtual measurements at inaccessible positions of the structure and a simulation based lifetime prediction. This work presents an inference workflow that describes the difference of measured data and simulated model responses with a generic interface that is independent from the specific model or even the geometry and can easily incorporate multiple data sources. A variational Bayesian inference algorithm is then used to a) calibrate a set of models to given data and to b) identify the best fitting one. The developed concepts are applied to a bridge Demonstrator equipped with displacement sensors, force sensors and a stereophotogrammetry system to perform a system identification of the material parameters as well as a real-time identification of a moving load. T2 - 6th GAMM AG Data Workshop CY - Berlin, Germany DA - 20.10.2020 KW - Digital twin KW - Demonstrator PY - 2020 AN - OPUS4-51532 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Jörg F. A1 - Titscher, Thomas A1 - Robens-Radermacher, Annika A1 - Muth, Thilo A1 - Coelho Lima, Isabela T1 - Stochastische Modellkalibrierung eines digitalen Zwillings N2 - Ein Digitaler Zwilling repräsentiert ein reales Objekt in der digitalen Welt. Die Digitalen Zwillinge sind aus Daten und Modellen/Algorithmen aufgebaut und kontinuierlich über Sensoren mit der realen Welt gekoppelt. Anwendung z.B. Modellbewertung, Monitoring, Schadensdetektion. T2 - DVM-Online-Workshop "Grundlagen und Beispiele zur Digitalisierung für die Materialforschung und -prüfung" CY - Online meeting DA - 20.10.2020 KW - Modellkalibrierung KW - Stochastischen Verfahren KW - Realtime model updating KW - Demonstrator PY - 2020 AN - OPUS4-52175 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stockmann, Jörg M. A1 - Radnik, Jörg A1 - Bütefisch, S. A1 - Busch, I. A1 - Weimann, T. A1 - Passiu, C. A1 - Rossi, A. A1 - Unger, Wolfgang T1 - New Test Specimen for the Determination of the Field of View of Small-Area XPS N2 - Small-area/spot photoelectron spectroscopy (SAXPS) is a powerful tool for the investigation of small surface features like microstructures of electronic devices, sensors or other functional surfaces. For evaluating the quality of such microstructures, it is crucial to know whether a small signal in a spectrum is an unwanted contamination of the field of view (FoV), defined by the instrument settings, or it originated from outside. The aperture has a major influence on the signal-contribution from the outside. For the evaluation of the FoV, we determined the Au4f intensities measured with the center of the FoV aligned with the center of the spot and normalized to the Au4f intensity determined on the Au-film. With this test specimen, it was possible to characterize the FoV: The signal-contribution from the outside is reduceable down to lower than 50 %, when the aperture is 30 % of the structure dimension for our Kratos AXIS Ultra DLD system. T2 - Kratos User's Meeting 2020 CY - Online meeting DA - 21.09.2020 KW - Small Area XPS KW - Reference Material KW - Imaging XPS KW - Field of View PY - 2020 AN - OPUS4-51413 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hodoroaba, Vasile-Dan ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Energy-dispersive X-ray spectroscopy (EDS) N2 - As one of the widely used analytical methods for the analysis of elemental composition of solid matter, energy dispersive X-ray spectroscopy (EDS) has recently gained significant importance regarding its application to the chemical analysis of nanoparticles, especially in conjunction with the use of a scanning electron microscope (SEM) and the use of the transmission operation mode of SEM (STEM-in-SEM). This development was mainly driven by the technological progress with highly sensitive EDS detectors, such that individual nanoparticles can be quickly inspected with EDS at a SEM. Qualitative information on elemental composition with about 10 nm spatial resolution can be achieved complementary to the high-resolution information of the sample surface morphology within the same scanned area as provided by the electron microscope. Representative examples with successful EDS analysis on nanoparticles are presented, but also limitations of the method are described. KW - EDS KW - EPMA KW - X-rays KW - SEM/EDS PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00021-3 SP - 397 EP - 417 PB - Elsevier CY - Amsterdam AN - OPUS4-49991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Vladár, A. E. A1 - Hodoroaba, Vasile-Dan ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Characterization of nanoparticles by scanning electron microscopy N2 - In this chapter sample preparation, image acquisition, and nanoparticle size and shape characterization methods using the scanning electron microscope (SEM) in reflective and transmitted working modes are described. These help in obtaining reliable, highly repeatable results. The best solutions vary case-by-case and depend on the raw (powdered or suspension) nanoparticle material, the required measurement uncertainty and on the performance of the SEM. KW - Nanoparticles KW - Sample preparation KW - Electron microscopy KW - SEM KW - Size measurement KW - Shape KW - Threshold PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00002-X SP - 7 EP - 27 PB - Elsevier CY - Amsterdam AN - OPUS4-50120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Unger, Wolfgang A1 - Wirth, Thomas A1 - Hodoroaba, Vasile-Dan ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Auger electron spectroscopy N2 - An introduction in the application of Auger Electron Spectroscopy to surface chemical analysis of nanoparticles is given. Auger Electron Spectroscopy is a mature method in the field of surface chemical analysis. The chapter addresses the physical basis of the method, the principal design of recent instruments together with modes of operation and options for the presentation of spectra, as well as different approaches for qualitative (including identification of chemical species) and quantitative surface analysis of elements. An application paragraph on surface chemical analysis of nanoparticles by AES or SAM introduces the different measurement approaches and sample preparation strategies applied by analysts. The analysis of nanoparticle ensembles, the so-called selected point analysis where a narrow primary electron beam is centered on an individual nanoparticle, and chemical mapping of individual nanoparticles (or a line scan across) are addressed. Existing literature is reviewed and informative case studies presented. Limitations and pitfalls in the application of AES in surface chemical analysis of nanoparticles are also addressed. KW - Auger Electron Spectroscopy KW - Surface chemical analysis KW - Imaging surface chemical analysis KW - Nanoparticles KW - Nanotechnology PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00020-1 SP - 373 EP - 395 PB - Elsevier CY - Amsterdam AN - OPUS4-50119 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg A1 - Kjaervik, Marit A1 - Unger, Wolfgang T1 - Surface chemical analysis surface chemical analysis of cells and biofilms N2 - The status of the planned technical report "Surface characterization of biomaterials" will be presented. T2 - ISO TC201 Meeting CY - Online meeting DA - 05.09.2020 KW - X-ray photoelectron spectroscopy KW - X-ray spectroscopy KW - Biomaterials KW - Standardization PY - 2020 AN - OPUS4-51197 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - An, Biwen Annie A1 - Deland, Eric A1 - Kleinbub, Sherin A1 - Koerdt, Andrea T1 - Standardization of MIC laboratory testing: with a special focus on corrosive methanogens N2 - Microbiologically influenced corrosion (MIC) is a highly unpredictable process involving a complex group of microorganisms, including sulfate-reducing bacteria and methanogens. Standard laboratory MIC testing using static serum bottle enrichments is an easy but limited method, offering poor resolution on the biomineralization process of corrosion products. An example of this is the presumed corrosion product siderite by corrosive methanogens (Mi-MIC). Previous publications reported siderite was the sole corrosion product of M. maripaludis using metal coupons incubated under stationary conditions. However, the formation of siderite is closely related to the surrounding environmental conditions, i.e. pH, CO2 concentration, flow and temperature. Thus, siderite as the sole corrosion product of Mi-MIC remain inconclusive and questionable. To study Mi-MIC effectively, a novel versatile multiport flow-column corrosion monitoring system (MFC) was developed. MFC allows sectional corrosion rate determination under flow conditions using different types of material, inoculum and packing material. MFC offers great flexibility, ease of operation and accurate corrosion measurements that can be combined with many other techniques. Using MFC, we studied multiple strains of methanogens and compared it with sulfate-reducing bacteria under neutral and low pH conditions. It was revealed by MFC that corrosive methanogens have equally high corrosion potential as sulfate-reducing bacteria. Additionally, siderite is not the dominant nor sole corrosion product of Mi-MIC. Thus, effective corrosion monitoring and establishing standard laboratory practices, i.e. incorporating MFC as part of regular testing process, will provide deeper understanding of MIC. This will allow further microbial electrophysiology understandings, contributing to effective mitigation strategy development. T2 - EUROPEAN MIC NETWORK WEBINAR CY - Online meeting DA - 19.05.2020 KW - MIC KW - Methanogen KW - FIB/SEM KW - Corrosion products KW - Microbiologically influenced corrosion KW - Flow Model KW - Modelling KW - Korrosion PY - 2020 AN - OPUS4-51554 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Feldkamp, Martin A1 - Quercetti, Thomas A1 - Wille, Frank T1 - Outcomes of three large scale fire reference tests conducted in BAM fire test facility N2 - Packages for the transport of high-level radioactive material are designed to withstand severe accidents. Hypothetical severe accident conditions are defined in the IAEA Regulations for the Safe Transport of Radioactive Materials. One of these accident conditions is the thermal test, mainly consisting of a 30 minute fully engulfing 800°C pool fire or an equally severe fire test. The heat fluxes into the package depend substantially on the fire characteristics and the Surface temperature of the package. Fire tests can be performed at BAM on a propane gas fire test facility. In order to investigate the heat fluxes over a wide range of surface temperatures in this test facility a fire reference package was designed for multiple use. The package represented the outer geometry of a specific transport cask for radioactive waste. The fire reference package is a closed steel sheet cylinder with a wall thickness of 10 mm, a length of 1500 mm and a diameter of 1050 mm. The package was instrumented with thermocouples and filled with heat resistant insulation material. Three open-air fire tests were performed in the BAM propane gas fire test facility. The flames exposure time period varied slightly for the fire tests. The wind direction as well as the wind Speed were measured and changed between and during the tests. Test stand parameters such as wind shield location and propane gas volume flow were chosen constant for the three tests. The locally measured fire reference package steel sheet temperatures were used for the calculation of heat fluxes as function of time and surface temperature. The measured temperatures allowed further calculations. In a first approach effective fire characteristics of the propane gas fire, including the flame temperature, the fire convection coefficient and a Radiation exchange coefficient mathematically describing the determined average heat flux over the surface temperature were calculated. T2 - Pressure Vessels & Piping Conference 2020 CY - Online meeting DA - 03.08.2020 KW - Fire KW - Testing KW - Large scale testing KW - Calorimeter KW - Heat flux PY - 2020 SP - 1 EP - 9 PB - ASME CY - New York AN - OPUS4-51192 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Komann, Steffen A1 - Ballheimer, Viktor A1 - Quercetti, Thomas A1 - Scheidemann, Robert A1 - Wille, Frank T1 - Mechanical and thermal assessment by BAM of a new package design for the transport of SNF from a german research reactor N2 - For disposal of the research reactor of the Technical University Munich FRM II a new transport and storage cask design was under approval assessment by the German authorities on the basis of International Atomic Energy Agency (IAEA) requirements. The cask body is made of ductile cast iron and closed by two bolted lid systems with metal seals. The material of the lids is stainless steel. On each end of the cask the wood-filled impact limiters are installed to reduce impact loads to the cask under drop test conditions. In the cavity of the cask a basket for five spent fuel elements is arranged. This design has been assessed by the Bundesanstalt für Materialforschung und -prüfung (BAM) in view to the mechanical and thermal safety analyses, the activity release approaches, and subjects of quality assurance and surveillance for manufacturing and operation of the package. For the mechanical safety analyses of the package a combination of experimental testing and analytical/numerical calculations were applied. In total, four drop tests were carried out at the BAM large drop test facility. Two tests were carried out as a full IAEA drop test sequence consisting of a 9m drop test onto an unyielding target and a 1m puncture bar drop test. The other two drop tests were performed as single 9m drop tests and completed by additional analyses for considering the effects of an IAEA drop test sequence. The main objectives of the drop tests were the investigation of the integrity of the package and its safety against release of radioactive material as well as the test of the fastening system of the impact limiters. Furthermore, the acceleration and strain signals measured during the tests were used for the verification of finite-element (FE) models applied in the safety analysis of the package design. T2 - Pressure Vessels & Piping Conference 2020 CY - Online meeting DA - 03.08.2020 KW - Mechanik KW - radioaktives Material KW - Transportbehälter KW - Antragsverfahren KW - Zulassungen KW - Typ-B Versandstück KW - Thermik PY - 2020 VL - 2020 SP - 1 EP - 7 PB - ASME CY - New York AN - OPUS4-51103 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -