TY - CONF A1 - Bhattacharya, Biswajit A1 - Michalchuk, Adam A1 - Emmerling, Franziska T1 - Revealing Mechanical Plastic Bending in Coordination Polymer Crystals N2 - Crystalline molecular materials with mechanical flexibility are promising for technological development. This is particularly true for the development of advanced materials with optoelectronic and biomedical applications. While a growing number of mechanically flexible crystalline molecular materials are being reported,1 they remain scarce. At present, most discoveries are serendipitous, as limited design strategies are currently known. Amongst these strategies Desiraju et. al. suggested that elastic materials must contain herringbone structures.2 For plastic crystals, the so-called ‘shape-synthon’ strategy has been developed, in which weak non-covalent interactions are introduced into structures to facilitate mobility of molecules.3 This includes formation of slip planes. Generally, these models have performed very well at predicting and rationalizing the mechanical properties of new materials. Recently, however, a family of one-dimensional covalent networks (coordination polymers; CPs) has been described, which show mechanical elasticity. With drastically different structural chemistry, these systems do not seem to adhere to the currently established rules. Herein, we present the first such system: a plastically bendable crystal of a 1D CP, [Zn(-Cl)2(3,5-Cl2Py)2]n (where 3,5-Cl2Py = 3,5-dichloro pyridine). This CP crystallizes in a tetragonal, and can therefore be bent over two major faces to acute angles without fracturing. We conducted bending and indentation experiments to quantify the mechanical properties of the CP crystal. This was complimented by Vibrational (Raman and Terahertz) spectroscopy and theoretical calculations for deeper understanding of molecular level structural deformation. T2 - 32nd European Crystallographic Meeting (ECM32) CY - University of Vienna, Vienna, Austria DA - 18.08.2019 KW - Mechanical Flexiblity KW - Crystal engineering KW - Coordination Polymers PY - 2019 AN - OPUS4-49875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas A1 - Yildirim, Arda T1 - Combining Broadband Dielectric Spectroscopy with advanced calorimetry to reveal the multiple glass transitions in discotic liquid crystals N2 - Broadband dielectric spectroscopy and advanced calorimetry were combined to investigate the molecular dynamics of discotic liquid crystals T2 - Flash DSC Conference CY - Zurich, Switzerland DA - 24.11.2019 KW - Discotic Liquid Crystals PY - 2019 AN - OPUS4-49879 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana A1 - Epping, Ruben T1 - View into the Depths of Copolymer Microstructure N2 - For different kinds of polymers it will be shown how it could be realized to obtain information on small, sometimes isomeric topological heterogeneities by coupling UPLC / ESI-TOF-MS and LC /MALDI-TOF-MS. T2 - DSM, Fall Meeting CY - Breda, The Netherlands DA - 07.11.2019 KW - Microstructure KW - LC-MS KW - Copolymer PY - 2019 AN - OPUS4-49587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühle, Bastian A1 - Bresch, Harald A1 - Resch-Genger, Ute A1 - Hodoroaba, Vasile-Dan A1 - Radnick, Jörg T1 - Perspektive der BAM auf neuartige Materialien N2 - Neuartige Materialien, die bekannte (Werk-)Stoffe mit neuen Funktionalitäten ausstatten, spielen eine zunehmend wichtige Rolle im Bereich der Materialforschung und -prüfung. Das Spektrum neuartiger Materialien reicht von der gezielten Oberflächenfunktionalisierung und -strukturierung makroskopischer Materialien, dünnen Beschichtungen bis hin zu mikro- und nanoskaligen Kompositmaterialien und funktionalen Materialien an der Schnittstelle zur Biologie, Biotechnologie, nachhaltige Energiespeicherung und Sensorik. Dabei bieten neuartige Materialien die Chance, Werkstoffe und Produkte mit erweiterter oder verbesserter Funktionalität zu erhalten und Sicherheit bereits im Designprozess zu berücksichtigen. Durch dieses breite Anwendungsspektrum und die Herausforderungen, die solche Materialien für die Sicherheit in Chemie und Technik mit sich bringen, sind diese in allen Themenfeldern der BAM repräsentiert (Material, Analytical Sciences, Energie, Infrastruktur und Umwelt). Die Aufgaben der BAM erstrecken sich dabei von der Herstellung von Referenzmaterialien für Industrie, Forschung und Regulation, über die Erstellung von standardisierten Referenzverfahren für nachhaltige Messungen im Umwelt- und Lebenswissenschaftsbereich bis hin zur Bereitstellung von belastbaren und zitierbaren Referenzdaten. Durch die genaue Charakterisierung neuartiger Materialien können potentiell problematische Substanzen identifiziert und deren Risiken besser abgeschätzt werden. In diesem Beitrag werden einige aktuelle Beispiele aus diesen Bereichen vorgestellt. T2 - NanoDialog der Bundesregierung - Chancen und Risiken von Neuartigen Materialien CY - Berlin, Germany DA - 22.05.2019 KW - Advanced Materials KW - Nanomaterialien KW - Neuartige Materialien PY - 2019 AN - OPUS4-49594 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem A1 - Witt, Julia A1 - Schenderlein, Matthias A1 - Hampel, Marco A1 - Almalla, Ahed T1 - Untersuchung lokaler Korrosionsprozesse mittels kombinierter elektrochemischer und mikroskopischer Methoden N2 - Forschungsarbeiten des Fachbereichs auf dem Gebiet "Methoden für die Analyse der lokalen Korrosionsprozesse". T2 - ProcessNet-Arbeitsausschuss Elektrochemische Prozesse (AA ECP) CY - DECHEMA, Frankfurt am Main, Germany DA - 21.01.2019 KW - Scanning electrochemical microscope (SECM) KW - Atomic Force Microscopy (AFM) KW - Multielectrode based sensors PY - 2019 AN - OPUS4-49751 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem A1 - Wurzler, Nina A1 - Witt, Julia A1 - Dimper, Matthias A1 - Wagner, R. A1 - Lützenkirchen-Hecht, D. T1 - Changes in passive film chemistry of stainless steels in the presence of iron reducing bacteria N2 - Summary of the results obtained at DELTA-Beamline 8 in 2018. T2 - DELTA User Treffen CY - Dortmund, Germany DA - 28.11.2018 KW - MIC KW - Corrosion KW - XANES PY - 2018 AN - OPUS4-50312 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem A1 - Wurzler, Nina A1 - Hampel, Marco A1 - Witt, Julia A1 - Schenderlein, Matthias T1 - Combined electrochemical techniques for the investigation of corrosion processes N2 - Short presentation of BAM, a summary of the methods available in FB 6.2 and recent results on MIC and high resolution corrosion studies T2 - Institute Seminar: Jerzy Haber Institute of Catalysis and Surface Chemistry CY - Cracow, Poland DA - 07.11.2018 KW - MIC KW - Corrosion KW - Atomic Force Microscopy (AFM) KW - Combined corrosive and mechanical load PY - 2018 AN - OPUS4-50313 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Marcoulaki, E. A1 - van Duuren, B A1 - Kunz, Valentin A1 - Unger, Wolfgang A1 - Shandilya, N. T1 - Testing and benchmarking nanosafety services N2 - One of the objectives of the EU Project EC4SafeNano (European Centre for Risk Management and Safe Innovation in Nanomaterials & Nanotechnologies) was to test and benchmark the services in order to check their relevance to address identified stakeholder needs, but also to evaluate the governance of the structure delivering the proposed services. The aim is to demonstrate the technical relevance of the services and the overall open structure organisation, including governance rules and operating procedures, by answering relevant identified questions (case studies) selected by a panel of stakeholders. Therefore, a significant part of the project will be devoted to this demonstration of the operational and functional basis of the organized network. T2 - Review Meeting EC4SafeNano CY - Brussels, Belgium DA - 16.01.2020 KW - Nanosafety KW - EC4SafeNano KW - Nanosafety services KW - EU KW - Case studies PY - 2020 AN - OPUS4-50273 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Schmitt, M. T1 - EMPIR nPSize - Improved Traceability Chain of Nanoparticle Size Measurement; What nPSize can offer to CEN/TC 352? N2 - The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities (e.g. reference materials, measurement procedures, inter-laboratory comparisons) as pertinent contributions to normative projects within CEN/TC 352 Nanotechnologies are discussed. E.g. the first technical report of nPSize on full algorithm sequences for nanoparticle detection and size measurement as developed on both a physical basis (SEM, TSEM, AFM and SAXS) and by machine learning is put at disposal. T2 - 29th Meeting of CEN/TC 352 Nanotechnologies CY - Online meeting DA - 25.03.2021 KW - Nanoparticles KW - Electron microscopy KW - CEN/TC 352 Nanotechnologies KW - Particle size distribution KW - Modelling KW - Machine learning PY - 2021 AN - OPUS4-52464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ciornii, Dmitri A1 - Drobne, D. A1 - Novak, S. A1 - Kranjc, E. A1 - Bohmer, N. A1 - Hodoroaba, Vasile-Dan A1 - Reuther, R. T1 - Knowledge, Information and Data Readiness Levels (KaRL) approach for Nanorisk Governance N2 - Nanomaterials may have brought many beneficial innovations with them in our daily lives and and have become indispensable for the society. However, one needs to be concerned of the risks which are still unknown and not sufficietly studied and therefore there is a need for a nanorisk governance. At the core of nanorisk governance is gathering, processing and analysing reliable data which will be used for decision making. The challenge is to assure data reliability and transform it into knowledge. To address this challenge, we used analogy to technology readiness level (TRL) approach (developed by NASA), and elaborated knowledge readiness level (KaRL). KaRL is a nine-scale system to categorize data and knowledge (documents) into levels of readiness for particular purposes and to enhance readiness level by using quality and completeness filters, compliance requirements, nanorisk-related tools, stakeholders’ input. By our approach we addressed key issues in nanotechnology such as societal and ethical concerns, circular economy and sustainability, traceability of data, knowledge and decisions. T2 - EC - HORIZON EUROPE NMBP-13 Joint Conference Risk Governance of nanotechnology CY - Online meeting DA - 12.04.2021 KW - Knowledge Readiness Level KW - Nanorisk KW - Nanomaterials KW - Data PY - 2021 AN - OPUS4-52471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühle, Bastian A1 - Hodoroaba, Vasile-Dan T1 - Automatic Image Segmentation and Analysis using Neural Networks N2 - We present a workflow for obtaining fully trained artificial neural networks that can perform automatic particle segmentations of agglomerated, non-spherical nanoparticles from electron microscopy images “from scratch”, without the need for large training data sets of manually annotated images. This is achieved by using unsupervised learning for most of the training dataset generation, making heavy use of generative adversarial networks and especially unpaired image-to-image translation via cycle-consistent adversarial networks. The whole process only requires about 15 minutes of hands-on time by a user and can typically be finished within less than 12 hours when training on a single graphics card (GPU). After training, SEM image analysis can be carried out by the artificial neural network within seconds, and the segmented images can be used for automatically extracting and calculating various other particle size and shape descriptors. T2 - Machine Learning Workshop CY - Online Meeting DA - 18.03.2021 KW - Electron Microscopy KW - Neural Networks KW - Artificial Intelligence KW - Image Segmentation KW - Automated Image Analysis PY - 2021 AN - OPUS4-52304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Elektronenstrahl-Mikroanalyse (ESMA) an heterogenen Proben N2 - Grundkenntnisse zum besseren Verständnis der Funktionsweise der Elektronenstrahl-Mikroanalyse (ESMA) werden präsentiert und anhand Beispielen diskutiert. Das physikalische Messprinzip von ESMA am REM, das Wechselwirkungs- und Informationsvolum und die Anregung der charakteristischen Röntgenlinien werden erklärt. Verschiedene potentielle Artefakte, wie z.B. Heterogenität der Probenzusammensetzung, Oberflächenbeschaffenheit der Probe und Linienüberlagerung werden eingeführt. Die physikalischen Grenzen der analytischen Methode werden spezifiziert. T2 - Industrietreffen im Forschungs- und Innovationszentrum (FIZ) der BMW Group CY - Munich, Germany DA - 09.01.2018 KW - ESMA KW - REM KW - Elementzusammensetzung KW - REM/EDX PY - 2018 AN - OPUS4-43708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartelmeß, Jürgen A1 - Gawlitza, Kornelia A1 - Kraus, Werner A1 - Chlvi-Iborra, Katherine A1 - Tiebe, Carlo A1 - Noske, Reinhard A1 - Bartholmai, Matthias A1 - Rurack, Knut T1 - Developments Towards a BODIPY-based fluorometric sensing device for multiple hazardous gases N2 - Fluorometric sensing is a versatile approach for trace analysis outside of the laboratory, requiring suitable sensor materials and their integration into sensing devices. The versatility of fluorophores as probes, especially in terms of the possibility to tailor their optical as well as their recognition properties by synthetic modifications in a wide range, renders them as superior active component for the preparation of optical sensing devices. Recent works at BAM in this field include, for example, the detection of nerve gas agents, illustrating impressively the aforementioned benefits of fluorophores in optical sensing applications. In the interdisciplinary project presented here, we target hazardous gases such as ammonia, benzene, and hydrogen sulfide, next to others, which pose a major threat to human health and environmental safety and for which the availability of a sensitive and reliable detection method is highly desirable. The dyes presented follow a “turn-on” fluorescence schematic, which allows for the selective and sensitive detection of the respective gaseous analyte. The immobilization of the probe in polymeric matrices is then the next step toward the fabrication of a prototype device for molecular sensing. Further steps in the project include the assembly of instruments for test-atmosphere generation, the referencing of the sensor system, development and implementation of an optical setup, and the testing of the prototype device under laboratory conditions and in the field. In this presentation, we give an overview over the recent developments on this topic in our groups. Highlights are hydrogen sulfide sensitive, BODIPY based transition metal complexes, which allow for a sensitive as well as selective detection of the toxic gas. In addition, we present a novel class of highly substituted BODIPY derivatives – pocket-BODIPYs – which are of a synthetically high versatility and can readily be modified to create pockets in the periphery of the molecule of defined geometries. This is illustrated on the successful encapsulation of benzene by a pocket-BODIPY derivative, confirmed by X-ray crystallographic analysis as well as by further spectroscopic and analytical methods. T2 - International Conference on Porphyrins and Phthalocyanins (ICPP-10) CY - Munich, Germany DA - 01.07.2018 KW - BODIPY dye KW - Fluorometric sensing KW - Gas sensing PY - 2018 AN - OPUS4-45646 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griepentrog, Michael T1 - Towards the standardization of dynamic instrumented indentation testing N2 - Nowadays the Instrumented Indentation Testing (IIT) is one of the most commonly used methods to determine the mechanical properties of materials in the nano range. This method is already extensive standardized in EN ISO 14577 part 1-4. Because of the great interest of researchers and industries in investigations of time depending material behavior mostly all suppliers of IIT equipment are offering the possibility of dynamic testing. Realizing this development ISO/TC 164/SC3 Hardness Testing has proposed to start the new standardization project “Linear elastic dynamic instrumented indentation testing DIIT”. The development of this standard is accompanied by the first international intercomparing exercise comparing results of dynamic instrumented indentation testing from testing machines using different hardware solutions and different models for data evaluation. The draft of part 5 of ISO 14577 “Linear elastic dynamic instrumented indentation testing DIIT” specifies verification and calibration of testing machines for carrying out the measurement of the dynamic material response when an oscillatory force or displacement, with amplitudes small in comparison to the prescribed target values, is imparted to the indenter while the indenter is continuously loaded to a prescribed target load or target depth or while the load or displacement is held constant at a prescribed target value. In case of a material showing plastic-elastic behavior, the measured dynamic response is used for continuous evaluation of the dynamic stiffness of the contact as a function of depth and frequency. Using the dynamic stiffness of the contact a reduced dynamic modulus will be calculated. In case of a material showing visco-elastic behavior from the measured dynamic response also the dynamic contact damping coefficient as function of depth and frequency is evaluated continuously. Using dynamic contact stiffness and dynamic contact damping coefficient reduced lost and storage modulus for visco-elastic materials will be calculated. The main normative requirements of the draft will be presented and discussed in the light of the first results of the intercomparing excise. T2 - IIW6, International Indentation Workshop 6 CY - Sapporo, Japan DA - 02.07.2018 KW - ISO 14577 KW - Instrumented indentation testing KW - Nanoindentation KW - IIT KW - Mechanical properties KW - Dynamic testing KW - Visco-elastic KW - Loss module KW - Storage module PY - 2018 AN - OPUS4-45850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rauscher, H. A1 - Hodoroaba, Vasile-Dan A1 - Mech, A. A1 - Gaillard, C. A1 - Marvin, H. A1 - Wohlleben, W. A1 - Babick, F. A1 - Friedrich, C. M. A1 - Bruengel, R. A1 - Rückert, J. A1 - Ghanem, A. A1 - Weigel, S. T1 - The NanoDefine Decision Framework and NanoDefiner e-Tool: a practical guide to the identification of nanomaterials N2 - The European Commission's recommendation on the definition of nanomaterial [2011/696/EU] is broadly applicable across different regulatory sectors and requires the quantitative size determination of constituent particles in samples down to 1 nm. A material is a nanomaterial if 50 % or more of the particles are in the size range 1-100 nm. The implementation of the definition in a regulatory context challenges measurement methods to reliably identify nanomaterials and ideally also non-nanomaterials as substance or product ingredient as well as in various matrices. The EU FP7 NanoDefine project [www.nanodefine.eu] addressed these challenges by developing a robust, readily implementable and cost-effective measurement strategy to decide for the widest possible range of materials whether it is a nanomaterial or not. It is based on existing and emerging particle measurement techniques evaluated against harmonized, material-dependent performance criteria and by intra- and inter-lab comparisons. Procedures were established to reliably measure the size of particles within 1-100 nm, and beyond, taking into account different shapes, coatings and chemical compositions in industrial materials and consumer products. Case studies prove their applicability for various sectors, including food, pigments and cosmetics. A main outcome is the establishment of an integrated tiered approach including rapid screening (tier 1) and confirmatory methods (tier 2), a decision support flow scheme and a user manual to guide end-users, such as manufacturers, in selecting appropriate methods. Another main product is the “NanoDefiner” e-Tool which implements the flow scheme in a user-friendly software and guides the user in a semi-automated way through the entire decision procedure. It allows a cost-effective selection of appropriate methods for material classification according to the EC's nanomaterial definition and provides a comprehensive report with extensive explanation of all decision steps to arrive at a transparent identification of nanomaterials as well as non-nanomaterials for regulatory purposes. The project has received funding from the European Union’s Seventh Programme for research, technological development and demonstration under grant agreement No 604347. T2 - BAM-PTB Workshop on Reference Nanomaterials CY - Berlin, Germany DA - 14.05.2018 KW - Definition of nanomaterial KW - Regulation PY - 2018 AN - OPUS4-45633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maurino, V. A1 - Hodoroaba, Vasile-Dan A1 - Pellutiè, L. A1 - Pellegrino, F. A1 - Ortel, Erik A1 - Isopescu, R. T1 - Synthesis of Shape controlled TiO2 N2 - Titanium dioxide is one of the most studied metal oxides due to its chemical, surface, electronic and (photo)catalytic properties, providing this material of multisectorial applications ranging from healthcare, photocatalysis, smart materials with self cleaning and self sterilizing properties and solar energy harvesting. However it is difficult to correlate the functional properties of TiO2 nanomaterials to the properties at single nanoparticle level due to the high polydispersity in shape, size and surface features of the currently available TiO2 nanoparticles (NPs). Although intensive experimental and theoretical studies have been conducted on the reactivity of different surfaces of metal oxides such as TiO2 much less attention is paid on the dependence of functional properties, like photocatalytic activity, dye adsorption, open circuit potential and fill factor in dye sensitized solar cells, on crystal facets in different orientations. One of the goal of SETNanoMetro project was the development of design rules to tune crystal facets of TiO2 NPs in order to optimize and control functional properties. In the present work we have developed a series of design rules in order to obtain sets of anatase TiO2 NPs with low polydispersity and to tune their shape and size by hydrothermal processing of Ti(IV)-Triethanolamine complex in presence of different shape controllers. Through a careful experimental design, a predictive soft model was developed. The model is able to predict the synthesis outcome allowing to tune the shape factor from 5 (prisms) to 1.5 (bipyramids) to 0.2 (platelets). This allows to control the main crystal facets exposed ranging from (100) to (001). Due to the dependence of functional properties of nanomaterials on shape distribution and not only size, the availability of NPs sets with uniform and well defined and tunable shapes can be of paramount relevance in order to produce reference nanomaterials for shape measurement. T2 - NanoWorkshop 2018 (Workshop on reference nanomaterials, current situation and needs: development, measurement, standardization) CY - Berlin, Germany DA - 14.05.2018 KW - Anatase KW - Shape control KW - Hydrothermal synthesis KW - Nanoparticles PY - 2018 AN - OPUS4-45634 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saatz, Jessica A1 - Grunert, Bianca A1 - Jakubowski, Norbert A1 - Hoffmann, Katrin A1 - Resch-Genger, Ute A1 - Emmerling, Franziska T1 - Tagging reagents for imaging mass cytometry N2 - In der klinischen Diagnostik werden für zytometrische Messverfahren bereits eine Reihe von Reagenzien eingesetzt zur Markierung von Antikörper eingesetzt, um die Detektion von Biomarkern mittels Fluoreszenz- oder Flugzeitmassenspektrometrie zu ermöglichen. Seit kurzem ist auch eine Imaging Mass Cytometry Kombination direkt erhältlich, wodurch der Nachweis von Biomarkern in Gewebeschnitten erreicht werden kann. Dazu wird eine Kopplung von Laser Ablation und induktiv gekoppeltem Plasma Massenspektrometrie eingesetzt, wobei ähnlich der Massenzytometrie, zuvor Antikörper mit Metallen markiert, und im Anschluss mit dem Gewebeschnitt inkubiert werden. Durch die hohe Ortsauflösung können die Biomarker lokalisiert, und zukünftig vielleicht auch quantifiziert werden. Insbesondere Lanthanide eignen sich als Markierungsmetalle, da sie einen niedrigen Untergrund und chemisch ähnliches Verhalten zueinander aufweisen. Allein durch diese Elemente können bereits etwa 15 Parameter unterschieden werden, was durch isotopenreine Standards weiter gesteigert werden kann. Vom Markierungsgrad abhängig werden unterschiedlich viele Metalle am Antikörper gebunden, und beeinflussen so die Sichtbarkeit im ICP-MS. Nanopartikel könnten daher eine deutliche Steigerung der Sensitivität bewirken. GdVO4 Nanokristalle scheinen bisher sehr vielversprechend und bieten neben multiparametrischen Anwendungen auch Multimodalität. Die Synthese der Nanokristalle zeigte hohe Homogenität und Reproduzierbarkeit in Partikelgröße in der Zusammensetzung. Ein erstes Experiment mit einer Zellkultur konnte bereits die effiziente Markierung der Zellen unter Beweis stellen, wobei durch hohe Signalstärke auch subzelluläre Auflösung in der LA-ICP-MS erreicht werden konnte. T2 - ICPMS Anwendertreffen 2018 CY - Berlin, Germany DA - 03.09.2018 KW - LA-ICP-MS KW - Immuno assay KW - Bioimaging KW - Nanocrystal KW - Lanthanide KW - Metal-tag PY - 2018 AN - OPUS4-45866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Nanoanalytik-Aktivitäten @ BAM N2 - In dieser Präsentation werden Aktivitäten im Bereich der 'nano'-Charakterisierung bei der BAM vorgestellt. Beispiele von F&E-Projekten und -Kooperationen im nano-Analytik-Bereich bei der BAM werden genannt. Thematische Kooperations-Möglichkeiten zwischen BAM und dem Netzwerk NanoAnalytik und -Messtechnik in der Produktion werden diskutiert. T2 - Treffen des Netzwerkes NanoAnalytik und -Messtechnik CY - Berlin, Germany DA - 06.11.2018 KW - Nanoanalytik KW - Nano-Projekte KW - Nano-Kompetenzzentrum KW - Nano-Charakterisierung PY - 2018 UR - https://www.nanoinitiative-bayern.de/nanoanalytik/ AN - OPUS4-46563 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In situ studies of mechanochemistry: a force of synthesis N2 - Recent results in the field of mechanisms and kinetics of mechanochemical reactions. T2 - Seminar GFZ Potsdam CY - Postdam, Germany DA - 28.03.2018 KW - In situ KW - XRD KW - Rietveld PY - 2018 AN - OPUS4-46992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Synchrotron X-ray Investigations N2 - Summary of the techniques available at the BAMline and µspot BEamline. T2 - Workshop Humboldt University and Hebrew University of Jerusalem CY - Berlin, Germany DA - 09.10.2018 KW - In situ KW - XRD PY - 2018 AN - OPUS4-46993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - New insights in mechanochemical processes using real-time In situ investigations N2 - Mechanochemistry is a fast and efficient method applicable for the synthesis of new organic[1], metal-organic[2], and inorganic[3] compounds. The direct monitoring of milling reactions is still challenging. The underlying reaction mechanisms remain often unclear. In the last years, have established a tandem in situ approach for investigating mechanochemical reactions using time-resolved in situ XRD coupled with Raman spectroscopy.[4] Here, we present an in situ coupling of synchrotron XRD, Raman spectroscopy, and thermography allowing the observation of mechanochemical reactions in real time.[5] Information on the crystalline, molecular, and temperature state of the materials during grinding could be collected. The chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. Furthermore, the presented setup allows the detection of crystalline, amorphous, eutectic as well as liquid intermediates. The resulting deeper kinetic and thermodynamic understanding of milling processes is the key for future optimization of mechanochemical syntheses. T2 - 5th International Conference "Fundamental Bases of Mechanochemical Technologies" CY - Novosibirsk, Russia DA - 25.06.2018 KW - Mechanochemistry KW - XRD KW - Kinetic KW - Coordination polymers PY - 2018 AN - OPUS4-46994 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In situ characterization of nucleation, growth, crystallization and dissolution of nanoscaled iron oxides N2 - Nucleation and growths of iorn oxide nanoparticles studied in situ using XRD, XRF, SAXS and XANES. T2 - International CRC meeting CY - Berlin, Germany DA - 10.10.2018 KW - XRD KW - XANES PY - 2018 AN - OPUS4-46995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schoenhals, Andreas T1 - Structure property relationships of thin polymer films N2 - Polymers at interfaces play a major role in a broad variety of applications ranging from engineering purposes (for instance polymer based nanocomposites) to high tech implications (for instance light emitting diodes). Here, thin films with thicknesses down to few nanometers are prepared on different substrates as model systems for polymer composites. The thin films are investigated by a combination of surface analytical and volume sensitive methods. As surface analytical methods atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and contact angle measurements (CAM) are employed. As volume sensitive broadband dielectric spectroscopy (BDS), specific heat spectroscopy (SHS), and ellipsometry are used. Especially attention is paid to understand the glass transition behavior of thin films because the glass transition is the key phenomenon determines the application of polymers also in thin films. To understand the glass transition behavior of thin films, which is controversially discussed in literature, a three layer model is discussed. Firstly, a mobile surface layer is assumed at polymer air interface of the film due to missing of segment/segment interactions. Secondly, in the middle of the film a bulk-like layer should be expected. Thirdly, for polymers having non-repulsive interactions with the substrate an irreversibly adsorbed layer is expected to be formed. Due the adsorption the molecular mobility of the segments in this layer is slowed down. What is measured for the glass transition of thin films is a complicated average of all of these effects. The different layers are hardly to address separately. Therefore, in the presentation especially model systems are selected and investigated to verify the layer model. T2 - Seminarvortrag Universität Dortmund CY - Dortmund, Germany DA - 29.01.2019 KW - Thin polymer films PY - 2019 AN - OPUS4-47289 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - May the Force be with you - Mechanochemical syntheses studied in situ N2 - Mechanochemistry is a fast and efficient method applicable for the synthesis of new organic, metal-organic, and inorganic compounds. The direct monitoring of milling reactions is still challenging. The underlying reaction mechanisms remain often unclear. In the last years, have established a tandem in situ approach for investigating mechanochemical reactions using time-resolved in situ XRD coupled with Raman spectroscopy. Here, we present an in situ coupling of synchrotron XRD, Raman spectroscopy, and thermography allowing the observation of mechanochemical reactions in real time. Information on the crystalline, molecular, and temperature state of the materials during grinding could be collected. The chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. Furthermore, the presented setup allows the detection of crystalline, amorphous, eutectic as well as liquid intermediates. The resulting deeper kinetic and thermodynamic understanding of milling processes is the key for future optimization of mechanochemical syntheses. T2 - Seminar Universität Montpellier CY - Montpellier, France DA - 24.01.2019 KW - Mechanochemistry KW - In situ PY - 2019 AN - OPUS4-47261 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - New insights in mechanochemical processes using real-time in situ investigations N2 - Use of synchrotron radiation for special sample conditions. Recent work of the group at BESSY II. T2 - DESY Usermeeting Satelite Workshop CY - Hamburg, Germany DA - 22.01.2019 KW - XRD KW - In situ KW - Rietveld KW - Synchrotron PY - 2019 AN - OPUS4-47262 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Hard X-ray spectroscopy and imaging at the BAMline and MySpot beamlines at BESSY II (Berlin, Germany) N2 - Overview of the X-ray based analytical methods conducted at the BAMline and µSpot Beamline for structure analysis. T2 - Pccr2 + AfLS conference CY - Accra, Ghana DA - 29.01.2019 KW - X-ray spectroscopy KW - Synchrotron KW - Beamline KW - Material characterization PY - 2019 AN - OPUS4-47319 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Quantitative biocide profile measurements by calibrated XPS N2 - This presentation provides an update on recent results from quantitative XPS-measurements of real and artificial biofilms. NAP-XPS, lab-based XPS and synchrotron-based XPS was used to obtain a vertical concentration profile of iodine in agarose-films with information depth ranging from 1 to 18 nm. T2 - Project meeting MetVBadBugs CY - Turin, Italy DA - 05.02.2019 KW - Biofilms KW - NAP-XPS KW - XPS KW - Iodine KW - Agarose PY - 2019 AN - OPUS4-47332 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Microplastics: Degradation properties of polymers in the environment N2 - The accumulation of plastics leaked into the environment achieve a high perception in the last years. It is uncontroversial that often an uncontrolled, high consumption of plastic products and a poor waste management resulted in plastic findings all over in the environment. However, less is known about the relevant pathways and fate of plastic in the environment. Especially plastic fragments smaller 5 mmm, so called microplastics, achieve a high attention, because their amount and risks arising from these fragments are still unknown. The basic mechanisms of plastic or more precise, of different polymer degradation processes are often not considered, resulting in unrealistic statements. For generation of fundamental understanding of this problem we developed in the last years a fast thermoanalytical method for identification and mass quantification of microplastics in complex samples. The presentation will also give a short introduction about polymer degradation. T2 - Environmental Geosciences Seminar CY - Vienna, Austria DA - 19.11.2018 KW - Microplastic KW - Analysis KW - Standardisation PY - 2018 AN - OPUS4-47182 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Kunststoffe in der Umwelt: Elastomere, Thermoplaste und Duroplaste – worüber sprechen wir eigentlich und was sind die analytischen Herausforderungen? N2 - Übersichtsvortrag zur Thematik Kunststoffe in der Umwelt. Es werden Aspekte zu Definitionen, Eigenschaften und Analytischen Möglichkeiten und Herrausforderungen angesprochen. T2 - Arbeitsgespräch der Ressortforschungseinrichtungen CY - Berlin, Germany DA - 26.11.2018 KW - Mikroplastik KW - Umwelt KW - Polymere Eigenschaften PY - 2018 AN - OPUS4-47183 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul A1 - Dümichen, E. A1 - Bannick, C. G. A1 - Jekel, M. A1 - Braun, Ulrike T1 - Turning up the heat: a thermoanalytical approach for the detection of microplastics N2 - The presentation deals with the analysis of plastics in environmental samples using the TED-GC-MS method. The method and its working principles are presented, method characteristics and application examples are given. Advantages and disadvantages compared to other methods are highlighted. T2 - Linnaeus Eco-Tech 2018 CY - Kalmar, Sweden DA - 19.11.2018 KW - Microplastics KW - Tire wear KW - Thermoanalysis KW - TED-GC-MS PY - 2018 AN - OPUS4-47185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Career talk & lab tour - Working at BESSY II, a large scale research facility in Adlershof N2 - What exactly does a postdoc do at a research institute? What scientific questions does he or she want to address? What is their daily work routine? During our regular Lab Tours, female postdocs provide insight into their jobs. They also tell us about their career path: How did they get there? And what do they envision for their professional future? This time, Dr. Ana Guilherme Buzanich, a scientist from the Structure Analysis division at the Bundesanstalt für Materialforschung und -prüfung (BAM), will give an overview of her Research areas. She works at the electron storage ring BESSY-II where she conducts experiments at two hard X-ray beamlines (BAMline and µSpot). The tour includes a guided visit of the research facility. T2 - Lab Tour & Career Talk, WiNS CY - Berlin, Germany DA - 11.02.2019 KW - Women in STEM KW - X-ray Spectroscopy KW - Synchrotron KW - Beamline KW - Material characterization PY - 2019 AN - OPUS4-47418 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gollwitzer, Christian A1 - Scholz, Philipp A1 - Ulbricht, Alexander A1 - Joshi, Yogita A1 - Weidner, Steffen T1 - Synchrotron based absorption edge tomography for the analysis of 3D printed polymer MOF N2 - Absorption edge tomography is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element. The beamline BAM line at BESSY II, which is operated by the Federal Institute for Materials Research and Testing, can provide a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%. Together with the microtomography setup, this enables differential tomography sensitive to any element with N >= 24 (Cr) by using an appropriate K- or L-edge in this range. Here, a polymer filament embedding metal organic framework (MOF) was prepared and used for 3D printing. Absorption edge tomography at the copper K edge was employed to perform a non-destructive 3D characterization of the microstructure of the embedded MOF. Data fusion was then used to determine the size distribution of the embedded MOF. T2 - iCT 2019 CY - Padua, Italy DA - 12.02.2019 KW - Synchrotron tomography KW - BAMline KW - MOF KW - Absorption edge tomography PY - 2019 AN - OPUS4-47392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Principles for the development of standards for investigation procedures of plastics in environmental media and materials N2 - An overview about the current status of microplastic analysis is given with scope on hamonisation and standarisation. T2 - Annual ISO/TC 61 Meeting CY - Saitama, Japan DA - 24.09.2018 KW - Standardisation KW - Microplastic KW - Analysis PY - 2018 AN - OPUS4-46457 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Entwicklung einer schnellen und robusten Methode für die Analytik von Mikroplastik in Wasser N2 - Vortrag im Rahmen der Preisverleihung zum Mülheimer Wasser Award 2018, Vorstellung der TED-GC-MS als Methode für Mikroplastik Analyse T2 - 3. Wasseranalytisches Seminar (MWAS 2018) CY - Mülheim a.d. Ruhr, Germany DA - 12.09.2018 KW - Mikroplastik KW - Analytik PY - 2018 AN - OPUS4-46459 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit A1 - Unger, Wolfgang T1 - New work item proposal for a technical report for ISO/TC 201 WG4 “Surface characterization of biomaterials”: Surface chemical analysis – Surface chemical analysis of cells and biofilms N2 - The proposed ISO Technical Report provides a description of a variety of physical methods of analytical chemistry by which bacteria and biofilms can be analysed. The state of the art, sample requirements and strengths associated with each method are identified. Presented at the DIN-meeting for NA 062-08-16 AA „Chemische Oberflächenanalyse und Rastersondenmikroskopie“ T2 - 18. Sitzung des DIN-meeting NA 062-08-16 AA "Chemische Oberflächenanalyse und Rastersondenmikroskopie“ CY - Berlin, Germany DA - 08.11.2018 KW - 3D nano SIMS KW - Fourier transform infrared spectroscopy KW - Raman-spectroscopy KW - Biofilms KW - XPS PY - 2018 AN - OPUS4-46548 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja A1 - Unger, Wolfgang A1 - Wirth, Thomas A1 - Kjaervik, Marit A1 - Cant, D. A1 - Shard, A. A1 - Clifford, C. T1 - Measurement of the thickness and nature of nanoparticle coatings - ISO/PWI TR 23173 N2 - This presentation explains the outline and scientific content of the ISO technical report 23173 "Measurement of the thickness and nature of nanoparticle coatings using electron spectroscopies". This technical report deals with those electron spectroscopy methods that are able to determine the coating thickness of nanoparticles. This specifically includes X-ray photoelectron spectroscopy (XPS), energy-resolved X-Ray photoelectron spectroscopy (ERXPS) using synchrotron radiation, near abient pressure photoelectron spectroscopy (NAPXPS) and Auger electron spectroscopy (AES). T2 - 18. Sitzung des DIN-Normenausschusses 062-08-16 AA CY - Berlin, Germany DA - 08.11.2018 KW - Core-shell nanoparticles KW - Electron spectroscopy KW - XPS KW - Synchrotron radiation KW - AES PY - 2018 AN - OPUS4-46550 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang A1 - Ehlert, Christopher A1 - Donskyi, Ievgen A1 - Girard-Lauriault, P.-L. A1 - Lippitz, Andreas A1 - Illgen, Rene A1 - Haag, R. A1 - Adeli, M. T1 - Chemical modification of graphene and carbon nano tubes as viewed by xps and nexafs spectroscopies with dft spectra simulation N2 - Graphene is a two-dimensional carbon network with unique properties. However, its low solubility, poor reactivity and the limited accessibility of a well-defined basal plane are major challenges for applications. An ideal method to overcome these problems is the covalent attachment of functional molecules to its surface which enable further reactive modifications for specific applications. There are several technologies for surface functionalization of graphene and related CNT materials. To get control on the functionalization process and to optimize the performance of the modified surfaces analytical tools for surface chemical characterization are required. X-ray absorption (NEXAFS) and photoelectron spectroscopy (XPS) have been identified to be rather powerful here [1-3]. Specifically, NEXAFS spectroscopy underpinned by quantum chemical spectrum simulations [4] is unique in a way to address changes of aromaticity and defect formation at the graphene surface during functionalization. For relevant surface modification technologies, we present examples on how NEXAFS and XPS can do a good job. All presented modifications aim on the production of platforms for defined functional 2D nanomaterials, as for example multifunctional hybrid architectures. In detail, we investigated: • A wet chemical method for covalent functionalization of graphene sheets by a one-pot nitrene [2+1] cycloaddition reaction under mild conditions. Here a reaction between 2,4,6-trichloro-1,3,5-triazine and sodium azide with thermally reduced graphene oxide (TRGO) results in defined dichlorotriazine-functionalized graphene sheets. • Graphene and carbon nanotube functionalized by Vacuum-Ultraviolet (VUV) induced photochemical or r.f. cw low pressure plasma processes to introduce amino, hydroxy or brominated functionalities. To underpin finger-print information delivered by C K-edge NEXAFS we studied the effects of selected point and line defects as well as chemical modifications for a single graphene layer model by density functional theory based spectrum simulations. References [1] P.-L. Girard-Lauriault et al., Appl. Surf. Sci., 258 2012 8448-8454, DOI: 10.1016/j.apsusc.2012.03.012 [2] A. Lippitz et al., Surf. Sci., 611 2013 L1-L7, DOI: 10.1016/j.susc.2013.01.020 [3] A. Faghani et al., Angew. Chemie (International ed.), 56 2017 2675-2679, DOI:10.1002/anie.201612422 [4] C. Ehlert, et al., Phys.Chem.Chem.Phys., 16 2014 14083-14095, DOI: 10.1039/c4cp01106f T2 - AVS 65th INTERNATIONAL SYMPOSIUM CY - Long Beach, CA, USA DA - 21.10.2018 KW - Graphene KW - Plasma KW - Nitrene [2+1] cycloaddition KW - XPS KW - NEXAFS PY - 2018 AN - OPUS4-46468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Acquiring and Documenting Reproducible Spectra, Depth Profiles and Images: XPS, AES and SIMS N2 - In this talk sample prep/handling, instrument calibration and data acquisition methods with examples from XPS, Auger and SIMS will be addressed in terms of their contributions to the reproducibility of data delivered by the methods. Active parties in the field are VAMAS TWA 2 “Surface chemical analysis” (http://www.vamas.org/twa2/index.html), ISO/TC 201 “Surface chemical analysis” (https://www.iso.org/committee/54618.html) and the Surface Analysis Working Group (SAWG) at the International Meter Convention (https://www.bipm.org/en/ committees/cc/wg/sawg.html). The tools to improve the reproducibility of spectra, depth profiles and images at these international platforms are inter-laboratory comparisons, validated SOPs, standards and certified reference materials (CRM) as well as uncertainty budgets and establishment of traceability chains. The last point is of specific importance because all the methods, XPS, Auger and SIMS, are not primary methods. To address quantitative XPS, AES and SIMS results of relevant inter-laboratory comparisons organized by SAWG considering measurands as alloy surface composition and thickness of thin films will be introduced. These comparisons delivered results which are viewed to be benchmarking, some of them resulted in ISO/TC 201 standards. For quantitative XPS and AES the principal outline of an uncertainty budget will be discussed together with the audience. Another issue of quantitative XPS which definitely needs consideration are valid methods for a determination of the transmission function of the instruments and even for the emission angle in the respective experiments. Concerning the field of depth profiling it has to be investigated together with the audience whether the ISO (or ASTM) standards we have are sufficient to guarantee comparable results. Having in mind the number of different sputter ion species available today and range of samples of interest (metals, semiconductors, organic films) this might be questionable. And, how do depth profiling by AR-XPS and variable excitation energy XPS compete here? For imaging surface chemical analysis, the characterization of the imaging system is an issue to be investigated. Here the determination of lateral resolution is a relevant topic. Finally, the future needs to develop metrology for new applications e.g., ambient-pressure XPS, bio samples, and core-shell nanoparticles, will be issues raised for a discussion with the audience. T2 - 17th Topical Conference on Quantitative Surface Analysis (QSA 17) CY - Long Beach, CA, USA DA - 21.10.2018 KW - Depth Profiles and Images KW - X-ray Photoelectron Spectroscopy (XPS) KW - Auger Electron Spectroscopy (AES) KW - SIMS KW - Reproducible Spectra PY - 2018 AN - OPUS4-46470 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Von Ägypten bis Hiddensee – Analyse von Gold mit Synchrotronstrahlung - Update 2018 N2 - Gold ist eines der sieben schon im Altertum bekannten Metalle und wurde wg. seines Glanzes und seiner Seltenheit von alters her als Tauschmittel und zur Herstellung von Schmuck benutzt. Außerdem ist es einfach bearbeitbar und weitestgehend gegen chemische Einflüsse resistent. Die Untersuchungen von Gold mit synchrotronstrahlungsangeregter Röntgenfluoreszenzanalyse sind zerstörungsfrei und geben Auskunft über die in der untersuchten Probe vorhandenen chemischen Elemente. Bei den hier vorgestellten Untersuchungen an der BAMline stehen Fragestellungen wie Herkunft, Herstellungsverfahren und Zusammengehörigkeit von Goldfunden im Vordergrund. Die verschiedenen Fragestellungen werden an einer Reihe von Beispielen erläutert die vom Wikingerschatz aus Hiddensee über die Himmelsscheibe von Nebra bis hin zu Funden aus Ägypten langen. Zusätzlich werden die modernen Messmethoden vorgestellt, die am Synchrotron heutzutage zur Verfügung stehen. T2 - Vorlesung FU Berlin Einführung in die Archäometrie CY - Berlin, Germany DA - 01.11.2018 KW - Gold KW - Synchrotron KW - XRF KW - BAMline PY - 2018 AN - OPUS4-46451 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Snow, T. A1 - Pauw, Brian Richard A1 - Smith, A. A1 - Terrill, N. A1 - Thuenemann, Andreas T1 - Modular SAXS data corrections N2 - A standardized methodology for the correction of scattering patterns, the calculation of uncertainties, the subtraction of backgrounds and solvents, optionally followed by the azimuthal averaging/reduction step, is presented. T2 - XVII International Small Angle Scattering Conference - SAS2018 CY - Traverse City, Michigan, USA DA - 07.10.2018 KW - Small-angle scattering KW - Software KW - Sata corrections KW - Quality PY - 2018 AN - OPUS4-46520 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard A1 - Breßler, Ingo T1 - McSAS for SAS analysis: Usage, Benefits and Potential Pitfalls N2 - An introductory lecture for users at the Diamond Light Source, on how to use the McSAS software to analyze their data. T2 - Small Angle Scattering Training School CY - Diamond Light Source, Didcot, United Kingdom DA - 04.06.2018 KW - Small-angle scattering KW - Software KW - Analysis PY - 2018 AN - OPUS4-46517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard A1 - Kaestner, Claudia A1 - Thuenemann, Andreas T1 - How good is SAXS? Results from a large Round Robin on an easy sample N2 - 22 laboratories returned 45 small-angle scattering datasets on a suspension of silver nanoparticles. The variance of the results has been analyzed in order to estimate the expected accuracy and precision of the small-angle scattering technique. T2 - XVII International Small Angle Scattering Conference - SAS2018 CY - Traverse City, Michigan, USA DA - 07.10.2018 KW - Small-angle scattering KW - Round Robin KW - Silver nanoparticles KW - Quality KW - McSAS PY - 2018 AN - OPUS4-46518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas A1 - Madkour, Sherif A1 - Gawek, Marcel A1 - Szymoniak, Paulina A1 - Hertwig, Andreas T1 - Growth kinetics and molecular mobility of irreversibly adsorbed layers in thin polymer films N2 - In well-annealed thin polymer films, with non-repulsive polymer/substrate interactions, an irreversibly adsorbed layer is expected to from. These adsorbed layers have shown greate potential for technological applications. However, their growth kinetics and molecular dynamics are still not fully understood. This is partly due to the hard accessibility of these layers in thin films. Here, the irreversibly adsorbed layers of homopolymer thin films are revealed by solvent-leaching experiments. First, the growth kinetics of these layers is investigated as a function of annealing time, annealing temperature, leaching time and the original filme thickness. The film thickness, topography and the quality of the adsorbed layer is controlled by Atomic Force Microscopy (AFM). Secondly, the molecular mobility of the adsorbed layer is investigated by Broadband Dielectric Spectroscopy (BDS). A recently developed nanostructured capacitor arrangement is employed to measure the layer with a free surface. The results are quantitatively compared and discussed with respect to recently published work. T2 - 10th Conference on Broadband Dielectric Spectroscopy and its Applications CY - Brussles, Belgium DA - 26.08.2018 KW - Thin polymer films PY - 2018 AN - OPUS4-45837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rietz, U. A1 - Lerche, D. A1 - Hielscher, Stefan A1 - Grunwald, Daniel A1 - Beck, Uwe T1 - Determination of coating properties by using analytical centrifugation N2 - The majority of all products have coated surfaces designed to fulfil different requirements. Building constructions are exposed to external influences like a wide temperature and humidity range, rain and UV radiation to name a few. The extension of machine life for metal cutting tools, like drills or milling cutters is another field of application for coated surfaces. The surfaces have to be modified in a way to maintain their specific functionality. Although adhesion testing of coatings is of great interest, it is still a challenge to obtain reliable quantitative results and to meet economic requirements. In this talk we deal with the curing behaviour of different 2-component epoxy paint systems for corrosion protection of metal constructions. After preparation of specimens the strength was determined in specified time intervals during curing. It could be shown that epoxy paints differ significantly on curing time as well as final strength. The second experimental study deals with coating systems on glass fibre reinforced plastics which are used for wind power turbines to reduce abrasive wear and ice adhesion for aerodynamic and safety reasons. All measurements have been carried out by CAT-TechnologyTM (Centrifugal Adhesion Testing), which uses the radially directed centrifugal force as test-load. The multi-sample test instrument analyses up to eight test specimen under identical testing conditions. By varying the rotational speed (100 rpm up to 13,000 rpm), forces from 0.1 N to 6.5 kN are applied. Upon reaching the critical rupture force, the stamp separates from the substrate and a sample related IR-signal is sent from the spinning rotor. For each test specimen breaking force is calculated and displayed in real-time. The innovative measurement principle meets the requirements of DIN EN 15870 and ISO 4624. T2 - EURADH 2018 CY - Lisbon, Portugal DA - 05.07.2018 KW - Adhesive strength determination KW - CAT-technology KW - Centrifugal adhesion testing KW - Metal coatings KW - Decorative coatings on polymer substrates PY - 2018 AN - OPUS4-46001 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Hidde, Gundula A1 - Lange, Thorid A1 - Gargouri, H. A1 - Kärkkänen, I. A1 - Naumann, F. T1 - Plasma Activation and Plasma-assisted ALD Surface Modification of Polymers for Improved Bonding and Adhesive Strength N2 - Bonding strength is crucial on polymers of low surface energy, for clean surfaces limited to 0.5, 1, and 2 MPa for PTFE, PP, and PE. Plasma treatment may improve bonding strength by a factor of 2 (PTFE) or 5 (PP and PE). The efficiency of treatment is usually 10% as both low pressure and atmospheric pressure processes show low topographic conformity. Besides, lifetime of activation/modification is rather short. Hence, bonding has to be carried out immediately after plasma treatment. The concept of plasma-assisted ALD (atomic layer deposition) interlayers was introduced in the project HARFE of SENTECH (modification/deposition/in-situ monitoring) and BAM (bonding, characterization, testing). ALD deposition has a high surface conformity and for dielectric films of Al2O3 also a good long-term stability given that the films are dense enough. Based on TMA and O2/O3 precursors, ALD layer stacks from 60 to 375 monolayers were prepared under different conditions. For a transfer time of 24 hours from deposition to measurement, bonding strength could be increased up to 5 MPa (PTFE) respectively 10 MPa (PP, PE). The huge potential of ALD layers as adhesive interlayers was demonstrated for Al2O3 on stainless steel with bonding strength beyond 15 MPa, i.e. interface strength within the ALD stack is also in this range. This is a prerequisite for subsequent PVD/CVD-deposition in hybrid systems. By means of the SI ALD LL system of SENTECH thermal and plasma-supported ALD processes can be alternatively realized. Ellipsometric in-situ monitoring provides monolayer sensitivity and reveals that the efficient bonding of the lower ALD layers on the polymer has to be further improved. Testing of bonding strength was realized by CAT (centrifugal adhesion testing) technology. It was shown that ALD modification correlates with the increase of surface energy and bonding strength. T2 - PSE 2018 - 16th Conference on Plasma Surface Engineering CY - Garmisch-Partenkirchen, Germany DA - 17.09.2018 KW - Plasma activation KW - Plasma-assisted ALD modification KW - Adhesive ALD interlayer KW - Bonding strength KW - Adhesive strength PY - 2018 AN - OPUS4-46015 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Mechanochemical Syntheses of Metal Phosphonates N2 - Mechanochemistry is a suitable method for synthesizing a variety of metal phosphonates. By varying the ratio of the reactants, it is possible to control the reaction pathway. With this approach targeted synthesis of a certain composition is possible. Several new metal phosphonate structures were solved from the powder X-ray diffraction data including molecular metal phosphonates. The results demonstrate a new fast, facile, and environmental friendly alternative for the preparation of metal phosphonates. In situ investigations of the milling processes provided insights into the formation process of metal phosphonates. A multi-step diffusion mechanism was identified for most systems. Crystalline phases were obtained intermediately, suggesting that the synthesis is following Ostwald’s rules of stages. T2 - 1st European Workshop on Metalphophantes CY - Swanse, UK DA - 18.09.2018 KW - Mechanochemistry PY - 2018 AN - OPUS4-46382 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Hertwig, Andreas A1 - Kormunda, M. A1 - Ryšánek, P. A1 - Ivanov, L. T1 - Characterisation of magnetron sputtered SnZnOx by means of spectroscopic ellipsometry - how can we analyse TCO materials optically? N2 - Transparent conductive oxide (TCO) films are a vital part of a large part of modern technology. The production of TCO materials has sparked much development in plasma coating technology. Quality control measurements of these layers are therefore important in many fields of optics and electronics such as high efficiency thin film photovoltaics. In this presentation, we report on optical measurements of ZnSnOx layers generated by DC/RF magnetron plasma co-sputtering. By changing the respective power on two different targets, the overall power, the gas composition and post-treatment, the properties of this type of layers can be varied in a number of parameters. The optical, electrical, and chemical properties of TCO layers are the technically most important properties together with the layer thickness. The dielectric function of layers is accessible by means of spectroscopic ellipsometry, which also yields the very important value for the layer thickness at the same time. It would be a significant step forward in quality control to use this non-destructive method also as a fast test for electrical properties. Therefore, we report on the optical properties connected to the production parameters, and also on our preliminary results connecting the optical dielectric function (in the visible and near infrared) to the electrical conductivity of the layers. We discuss the effect of deposition parameters on the optical properties of the layers and present an approach for correlating optical and electrical properties. Further, we discuss the question of accuracy of optical properties gained from model-fit-based optical methods and the use of different parameterised models for the dielectric function to achieve this. T2 - PSE 2018 - 16th Conference on Plasma Surface Engineering CY - Garmisch-Partenkirchen, Germany DA - 17.09.2018 KW - Mixed Oxides KW - TCO KW - Quality Control KW - Ellipsometry KW - Optical Constants PY - 2018 AN - OPUS4-46388 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gollwitzer, Christian A1 - Ulbricht, Alexander A1 - Scholz, Philipp A1 - Joshi, Yogita A1 - Weidner, Steffen T1 - 3D printing material filled with metal organic frameworks analyzed by synchrotron based absorption edge tomography N2 - Absorption edge tomography, also known as differential tomography at absorption edges, is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element. Synchrotron radiation is the best source for absorption edge tomography, because of its small bandwidth, high intensity and easily adjustable photon energy. The synchrotron beamline BAMline at the synchrotron radiation facility BESSY II in Berlin, which is operated by the Bundesanstalt für Materialforschung und -prüfung (BAM), provides a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%, when the double multilayer monochromator is used. Together with the microtomography setup, this enables differential tomography with submicron resolution at the K edge of the elements from chromium up to the lanthanides, and up to uranium, when the L edges are used as well. In this work, metal organic frameworks (MOFs) embedded in polymer are characterized using differential tomography. MOFs are microporous structures of metal ions, coordinated by organic linker molecules, that can be used in a broad field of applications, especially in gas storage and catalysis. In this work, polymer embedded MOFs were extruded into filaments, which could be used for 3d-printing to profit from the specific properties of the MOFs in polymeric materials combined with the arbitrary shapes provided by 3d-printing. For the extrusion, different polymer classes like ABS, polyester- and polyetherurethanes, as well as different MOFs (ZIF-8, ZIF-67, HKUST-1) were used to create MOF containing filaments with a nominal diameter of 3.0 mm. Differential tomography at the edges of the Zn, Co, and Cu was then used to find the distribution of the corresponding MOF in the filament and to analyze the shape of the inclusions. T2 - MSE 2018 CY - Darmstadt, Germany DA - 26.09.2018 KW - Absorption edge KW - Tomography KW - Metal organic framework KW - Synchrotron PY - 2018 AN - OPUS4-46429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin A1 - Berger, Achim T1 - Tragbare RFA an Gläsern: Ergebnisse und Grenzen N2 - Vorstellung der Ergebnisse der Messungen an Gläsern von Goethes Prismen. T2 - 3. Goethe/Ritter-Workshop CY - Berlin, Germany DA - 25.05.2018 KW - Goethe KW - Farbenlehre KW - Prisma KW - Handheld KW - XRF PY - 2018 AN - OPUS4-46369 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Witte, Steffen A1 - Radtke, Martin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Grunewald, Christian A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Emmerling, Franziska T1 - XAFS@BAMline N2 - X-ray Absorption fine structure spectroscopy (XAFS) is a frequently employed technique in order to investigate structural composition and Change of chemical compounds such as catalytic species or corrosion processes. These structural properties are essential (i) to understand underlying reaction mechanism and (ii) to further improve the design of materials. While XAFS measurements are usually performed with ionization Chambers or simple fluorescence detectors, we at BAMline specialize in measurements with innovative set-ups that meet Specialrequirements such as time resolution, (3D-) spatial Resolution or demanding sample environments. This contribution presents various available XAFS configurations with their corresponding applications. In particular, these comprise single -shot XAFS for time- resolved measurements, grazing-exit XAFS with energy and a spatially resolved detector for the characterization of thin films and an in situ grazing incidence Setup for the characterization of corrosion layers. Additionally,the possibility of analyzing Minute samples in total-reflection geometry is demonstrated. T2 - EXRS 2018 CY - Ljubljana, Slovenia DA - 24.06.2018 KW - XANES KW - XAFS KW - BAMline KW - Synchrotron KW - TXRF PY - 2018 AN - OPUS4-46361 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Witte, Steffen A1 - Kulow, Anicó A1 - Seeberg, D. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Grunewald, Christian A1 - Riesemeier, Heinrich A1 - Wohlrab, S. T1 - S2XAFS@work: Customization for the Characterization of VOx based Catalysts N2 - X-ray absorption fine structure spectroscopy (XAFS) is a frequently employed technique in order to investigate structural composition and change of chemical compounds such as catalytic species. These structural properties are essential (i) to understand underlying reaction mechanism and (ii) to further improve the design of efficient catalysts. This investigation is based on a newly developed XAFS setup comprising both time- and lateral-resolved XAFS information simultaneously in a single-shot (S2XAFS). The primary broadband beam is generated by a filter/X-ray-mirror combination (bandpass). The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by an area sensitive detector with a theta to 2 theta geometry. This facile, stable and scanningless setup was tested at the BAMline @ BESSY-II (Berlin, Germany). This contribution focuses on further experimental optimizations allowing the characterization of supported vanadium oxide (VOx) based catalysts at the lower hard X-ray regime (5 to 6 keV). First S2XAFS measurements of these catalysts are presented herein. Supported VOx catalysts show promising results in the oxidation of methane to formaldehyde. S2XAFS allows determining the structural composition of the metal (i.e. vanadium) based on a fast and smart setup. It is therefore an ideal tool to identify crucial roles of chemical compounds in catalytic reactions. T2 - XAFS 2018 CY - Cracow, Poland DA - 22.07.2018 KW - XANES KW - XAFS KW - BAMline KW - Synchrotron PY - 2018 AN - OPUS4-46362 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Scharf, o T1 - The colour X-ray camera – Basics and applications of a 2D X-ray detector N2 - The Color X-ray Camera CXC or SLcam® is an energy-resolving X-ray camera capable of energy- and space-resolved measurements. It consists of a high-speed CCD detector coupled to a polycapil-lary optic that conducts the X-ray photons from the probe to distinct pixels onto the detector. The camera is capable of fast acquisition of spatially and energy resolved fluorescence images. A dedicated software enables the acquisition and the online processing of the spectral data for all 69696 pixels, leading to a real-time visualization of the elements distribution in a sample. It was developed in a joint project with BAM, IFG Berlin and PN Sensors. In this contribution we will mainly discuss the use of the CXC at our beamline, the BAMline at BESSY II and imaging applications of the CXC from different areas, like biology and archaeometry. Additionally new developments for the use of the detector without optics, like wavelength dispersive detection or 1shot-XANES, will be presented. T2 - Seminar Strahlenphysikalische Anwendungen in Technik und Medizin CY - ATi Wien, Austria DA - 24.01.2018 KW - XRF KW - Synchrotron KW - BAMline PY - 2018 AN - OPUS4-46365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Hielscher, Stefan A1 - Lange, Thorid A1 - Rietz, U. A1 - Lerche, D. T1 - State-of-the-Art in Multiple-Sample Evaluation of Adhesive and Bonding Strength N2 - The paper addresses the “State-of-the-Art in Multiple-Sample Evaluation of Adhesive and Bonding Strength” and the following points are discussed in more detail: 1. Motivation (coatings, varnishes, tapes, laminates, CFRP, adhesive-bonded joints) 2. Conventional single-sample testing (evaluation of adhesive and bonding strength; failure pattern) 3. Multiple-sample handling (MSH), bonding (MSB), and testing: centrifugal adhesion testing (CAT) (multiple-sample approach, tensile test within a centrifuge) 4. Application examples of CAT-Technology™ (laminates, optical coatings, CFRP joints) Finally, a summary is given regarding status quo and benefits of CAT-technology under tensile stress conditions whereas examples of testing in a centrifuge under compressive stress conditions are mentioned in the outlook. T2 - The 5th International Conference Competitive Materials and Technology Processes CY - Miskolc-Lillafüred, Hungary DA - 08.10.2018 KW - Centrifugal Adhesion Testing KW - CAT KW - Multiple-sample handling (MSH) KW - Multiple-sample bonding (MSB) KW - Tensile strength of laminates KW - Tensile strength of coatings KW - Adhesive strength KW - Bonding strength PY - 2018 AN - OPUS4-46336 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kormunda, M. A1 - Hertwig, Andreas A1 - Rysanek, P. A1 - Ivanov, L. T1 - Optical and Electrical Properties of reactive/nonreactive Magnetron Deposited SnZnOxCoatings Annealed at Various Temperatures N2 - ZnSnOx coatings were deposited from two 2in magnetron targets made of ZnO and SnO2 connected to DC pulsed and RF power supplies, respectively. The pure Ar and reactive gas mixture Ar/O2 were used. DC pulsed power applied on ZnO target was kept constant 50W 50kHz, 20% d.c. and the RF power applied on SnO2 target was set to values from 0W (pure ZnO deposited) up to 150W (up to 8 at.% of Sn in films). The deposited films were investigated by multiple techniques as deposited at RT as well as after annealing at temperatures 200o C and 450o C. The lower annealing temperature is still compatible with many of common polymeric substrates. The amount of Sn in the films is proportional to applied RF power on SnO2 target. But there is also significant influence of the post Deposition annealing on the film compositions. The ratio Zn/Sn is reduced by the annealing process. Therefore the annealing is promoting the migration of Sn toward the surface and Zn to inside. Moreover the films deposited in oxygen rich reactive gas mixture does not reduces the resistivity with added Sn in contrary to films deposited in Ar where the resistivity was reduced by 5 orders of magnitudes. The plasma parameters were investigated and mean energies of dominant species were in DC pulsed only about 3eV and DC + RF powered plasma up to 15eV. The expected higher energetic particles in the RF influenced plasma deliver an additional energy to the growing film. Therefore, we observed systematic differences between refractive indexes in the films deposited with low RF powered SnO2 magnetron at RT and post-annealed at 200 ° and practically no difference between RT and post-annealed film at higher RF power above 50 W. The XRD results proved the transitions from an amorphous to more crystalline structure by post-annealing of the films. T2 - PSE 2018 - 16th Conference on Plasma Surface Engineering CY - Garmisch-Partenkirchen, Germany DA - 17.09.2018 KW - Reactive sputtering KW - Plasma diagnostics KW - Optical films KW - TCO PY - 2018 AN - OPUS4-46347 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saloga, Patrick E. J. T1 - SAXS in Analysis of Ultra-small Size-adjustable Zinc Oxide Nanoparticles for Controlled Band Gap Engineering N2 - Zinc oxide (ZnO) as a wide-bandgap II-VI semiconductor finds application in areas like optoelectronics, photocatalysis as well as in detection systems. While band-gap engineering in macroscopic ZnO can be performed by alloying, the band-gap of ZnO nanoparticles is also dependent on their size. Since small-angle X-ray scattering (SAXS) provides a much higher resolution in terms of ultra-small nanoparticle size analysis compared to other techniques, it allows for a careful examination of the correlation between particle size and band-gap. We report on the microwave-assisted synthesis of oleate-capped, photoluminescent zinc oxide nanoparticles with adjustable size as dispersions in organic solvents. The spherical particles were obtained by hydrolysis of the metal precursor in presence of a strong base at temperatures above the solvent’s boiling point. Hence, the reaction is dramatically accelerated and within seconds – instead of hours at lower temperatures –, narrowly dispersed particle systems are yielded. The particles’ sizes as derived from SAXS strongly depend on the reaction temperature and time. Choosing the right reaction conditions, the particle size and thus their band gap can be finely tuned. A size increase can be achieved both by increasing the reaction temperature and the reaction time. See Figure 1 for an exemplary comparison of five-minute syntheses at different temperatures. Here, the yielded particles display diameters between 5.0 and 7.6 nm and corresponding band-gaps of 3.32 up to 3.41 eV. The size increase is accompanied by a red-shift of the UV/Vis absorption edges and fluorescence emission. Furthermore, these particles can be transferred into water by coating with polysorbates. T2 - SAS2018 XVII International Small Angle Scattering Conference CY - Traverse City, Michigan, USA DA - 07.10.2018 KW - SAXS KW - Zinc oxide nanoparticles KW - Microwave synthesis PY - 2018 AN - OPUS4-46348 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - Hydrogen assisted cracking phenomena in duplex stainless steels elucidated by in- and ex-situ ToF-SIMS experiments N2 - In the presented research, the high potential and abilities of secondary ion mass spectrometry (ToF-SIMS) to detect and locally map the hydrogen distribution in two types of duplex stainless steels are shown. The research validates certain proposed mechanisms by combining ToF-SIMS with high-resolution scanning electron microscopy and electron-backscattered diffraction. The combination of data from several techniques on the same region was conducted in this field for the first time by applying data treatment of the ToF-SIMS raw data and data fusion approach. This powerful combination of methods allows reviewing of the occurring processes related to hydrogen assisted cracking. The step beyond the state of the art in this field was gained here by developing permeation and mechanical loading experiments within the ToF-SIMS during chemometric imaging of the hydrogen distribution in the microstructure. The research presents the necessary correlation between the hydrogen distribution and the resulted structural changes, the diffusion behavior in a duplex microstructure and stress induced diffusion of hydrogen by applying external load at the microscale. T2 - 6th WMRIF Early Career Scientist Summit CY - NPL Teddington UK DA - 18.06.2018 KW - ToF-SIMS KW - Duplex stainless steel KW - LDX KW - EBSD KW - Data-fusion PY - 2018 AN - OPUS4-46865 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded A1 - Böllinghaus, Thomas T1 - BAM’s role in materials science and hydrogen in metals: TOF-SIMS imaging N2 - Due to its low mass and high diffusivity in presence of compositional, thermal and mechanical gradients, hydrogen within a metallic microstructure can result in severe loss in ductility even at low concentrations and might lead eventually to a catastrophic and unpredictable failure of structural components during service. In this context, hydrogen mapping at the microscale is still considered among the most important challenges on the pathway towards a better understanding of the hydrogen transport and assisted cracking phenomena in metals, specifically in structural components, e.g. steels. Among the very few available techniques to localize hydrogen at the microscale, Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was proven to be a reliable tool. Based on the assumption that deuterium influence the microstructure similarly to hydrogen, in the following contribution ToF-SIMS was applied as the main technique to detect and locally map the deuterium distribution in several alloys: lean 2101 and standard 2205 duplex stainless steel (DSS), AISI 304L austenitic stainless steel and titanium 6Al-4V alloy. These alloys were selected as case studies in this work due to the wide use of them in many applications and environments which frequently provide critical conditions for hydrogen absorption and assisted degradation. The innovative design of in-situ and ex-situ experiments enabled us to elucidate the permeation, transport and trapping of deuterium in the microstructure in sub-micron resolution for the first time. In addition to the novel experimental setups, further progress was gained by applying computational multivariate data analysis (MVA) on the raw data and data fusion with high resolution structural characterization methods (scanning electron microscopy and electron back-scattered diffraction – SEM/EBSD). This combination allowed us to correlate the deuterium distribution and the influence on the microstructure. T2 - 4th Symposium on Innovative Measurement and Analysis for Structural Materials CY - Tokyo, Japan DA - 13.11.2018 KW - ToF-SIMS KW - Duplex stainless steel KW - Austenitic stainless steel KW - Principal Component Analysis KW - Data-fusion PY - 2018 UR - https://unit.aist.go.jp/tia-co/project/SIP-IMASM/sympo/2018/index.html AN - OPUS4-46867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Breitfeld, Steffen A1 - Scholz, Gudrun A1 - Emmerling, Franziska A1 - Kemnitz, Erhard T1 - BaF-Coordination polymers: Mechanochemical syntheses of new coordination polymers with a direct Ba-F bond N2 - Metal organic frameworks (MOFs) and coordination polymers (CPs) Play an important role in different fields of applications like e.g. catalysis, separations, gas storages, sensors or optoelectronics. Moreover, particularly fluorinated metal-organic frameworks (FMOFs) are in the focus of interest during the last years. Due to the strong electronegativity of fluorine the FMOFs show beside an enhanced thermal stability excellent optical and electrical properties compared to non-fluorinated frameworks. In most cases fluorine is implemented using perfluorinated organic linkers at the synthesis, usually performed by solvothermal synthesis. However, only few examples are known so far where fluorine is coordinated directly to the metal cation. Recently we reported about successful mechanochemical syntheses and characterization of fluorine-containing coordination polymers of alkaline earth metals by milling M(OH)2 (M: Ca, Sr, Ba) with fluorinated benzene dicarboxylic acids. In the present study, it was shown that it is possible to connect fluorine directly to Barium using a mechanochemical synthesis route. A new phase pure barium coordination polymer, BaF-benzene-dicarboxylate (BaF(p-BDC)0.5), was synthesized by milling starting either from barium hydroxide or from barium acetate as sources for barium cations. In both cases the second reactant was 1,4-benzenedicarboxylic acid (H2(p-BDC)). Ammonium fluoride was used as fluorinating agent directly at milling. Although single crystals are not accessible so far and the structure was not solved yet, both the 19F MAS NMR spectrum and the FT IR spectrum give strong evidence that fluorine as well as 1,4-benzenedicarboxylate are connected to barium. This is the first mechanochemical synthesis of coordination polymers where fluorine is directly coordinated to the metal cation. The new compound BaF(p-BDC)0.5 was characterized by X-ray powder diffraction, FT IR- and 19F, 1H-13C CP MAS NMR spectroscopies, DTA-TG and elemental analysis. T2 - Konferenz CY - Oberjoch, Germany DA - 22.07.20108 KW - Mechanochemical syntheses KW - Coordination polymers KW - Direct fluorine-metal bond KW - Alkaline earth metal PY - 2018 AN - OPUS4-46897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Mechanistic investigations of mechanosyntheses N2 - Mechanochemistry is a fast and efficient method applicable for the synthesis of new organic, metal-organic, and inorganic compounds. The direct monitoring of milling reactions is still challenging. The underlying reaction mechanisms often remain unclear. In the last years, we have established a tandem in situ approach for investigating mechanochemical reactions using time-resolved in situ XRD coupled with Raman spectroscopy. A further development is the in situ coupling of synchrotron XRD, Raman spectroscopy, and thermography allowing the observation of mechanochemical reactions in real time. [5] Information on the crystalline, molecular, and temperature state of the materials during grinding could be collected. The chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. Furthermore, the presented setup allows the detection of crystalline, amorphous, eutectic as well as liquid intermediates. Based on these data, metastable polymorphs of cocrystals and coordination polymorphs could be isolated and struc-turally characterized. A multi-step diffusion mechanism was identified for most systems. Crystalline phases were obtained intermediately, suggesting that the synthesis is following Ostwald’s rules of stages. The resulting deeper kinetic and thermodynamic understanding of milling processes is the key for future optimization of mechanochemical syntheses. T2 - Beilstein Symposium MECHANOCHEMISTRY: MICROSCOPIC AND MACROSCOPIC ASPECTS CY - Rüdesheim, Germany DA - 13.11.2018 KW - Mechanochemistry KW - Phosphonates KW - In situ PY - 2018 AN - OPUS4-46758 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas T1 - BAM and Division 6.1 N2 - This is a short overview of BAM and Division 6.1. We have insight into BAM's roles and responsibilities and the work we are doing in Division 6.1. T2 - Visit at CSEM Landquart CY - Landquart, Switzerland DA - 13.08.2018 KW - ToF-SIMS KW - AES KW - XPS KW - SEM PY - 2018 AN - OPUS4-46765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Broadband dielectric spectroscopy to study soft matter systems N2 - The basics of broadband dielectric spectroscopy were introduced in detail. The analysis of the data was discussed. As application of broadband dielectric spectroscopy the alpha-relaxation (dynamic glass transition) and the chain dynamics of polymers were ilustrated. Further the application of dielectric spectroscopy to polymerbased nanocomposites and high preformance polymers was discussed in detail. T2 - Kolloquiumsvotrag am Karlsruher Instiut of Technology CY - Karlsruhe, Germany DA - 05.12.2018 KW - Broadband dielectric spectroscopy PY - 2018 AN - OPUS4-46910 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In-situ investigations of mechanochemical reactions N2 - Mechanochemistry is a fast and efficient method applicable for the synthesis of new organic[1], metal-organic[2], and inorganic[3] compounds. The direct monitoring of milling reactions is still challenging. The underlying reaction mechanisms remain often unclear. In the last years, have established a tandem in situ approach for investigating mechanochemical reactions using time-resolved in situ XRD coupled with Raman spectroscopy.[4] Here, we present an in situ coupling of synchrotron XRD, Raman spectroscopy, and thermography allowing the observation of mechanochemical reactions in real time.[5] Information on the crystalline, molecular, and temperature state of the materials during grinding could be collected. The chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. Furthermore, the presented setup allows the detection of crystalline, amorphous, eutectic as well as liquid intermediates. The resulting deeper kinetic and thermodynamic understanding of milling processes is the key for future optimization of mechanochemical syntheses. T2 - ACS Conference Boston CY - Boston, USA DA - 19.08.2018 KW - Mechanochemistry KW - In situ KW - Kinetic PY - 2018 AN - OPUS4-46989 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - New insights in mechanochemical processes using real-time in situ investigations N2 - Mechanochemistry is increasingly used for synthesizing various materials including metal organic compounds and cocrystals. Although this synthesis approach offers a fast and pure synthesis in high yields, there is a lack in understanding the mechanisms of milling reactions. The necessary data can only be obtained in in situ experiments, which were only recently established for milling reactions. Herein, we present a novel setup enabling a combined in situ investigation of mechanochemical reactions using synchrotron XRD and Raman spectroscopy. T2 - ECM31 CY - Oviedo, Spain DA - 18.08.2018 KW - Mechanochemistry KW - In situ PY - 2018 AN - OPUS4-46990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In situ investigations of mechanochemical reactions N2 - Presentation of the recent results in the context of in situ investigations of reactions using X-ray diffraction. T2 - Germany Brazil Workshop: New light on mechanisms of chemical reactions CY - Kiel, Germany DA - 31.07.2018 KW - In situ KW - XRD PY - 2018 AN - OPUS4-46991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang A1 - Kjaervik, Marit T1 - New work item proposal for a technical report for ISO/TC 201 WG 4 “Surface characterization of biomaterials”: Surface chemical analysis – Surface chemical analysis of cells and biofilms N2 - The proposed ISO Technical Report provides a description of a variety of physical methods of analytical chemistry by which bacteria and biofilms can be analysed. The state of the art, sample requirements and strengths associated with each method are identified. T2 - 27th Plenary Meeting of ISO/TC 201 CY - Cancun, Mexico DA - 2018-09-20 KW - Surface chemical analysis of biofilms KW - XPS KW - Fourier-Transform Infrared Spectroscopy KW - 3D nano SIMS KW - Raman-spectroscopy PY - 2018 AN - OPUS4-46214 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit A1 - Dietrich, P. A1 - Thissen, A. A1 - Schwibbert, Karin A1 - Unger, Wolfgang T1 - Investigations of biofilms in various conditions by near-ambient pressure XPS N2 - X-ray photoelectron spectroscopy (XPS) provides elemental and chemical information from the outermost ~10 nm of the sample surface. This is in the same order of magnitude as the thickness of the outer bacterial membrane of gram-negative bacteria, as well as outer membrane molecules as exopolysaccharides and lipopolysaccharides, commonly attached to the cell surface. With the development of near-ambient pressure (NAP)-XPS, bacteria can be analysed with minimal sample preparation. EnviroESCA is a laboratory based NAP-XPS instrument, equipped with a monochromated Al Kα radiation source and a differentially pumped energy analyser connected to an exchangeable sample environment. It allows for measurements in various gas-atmospheres, including water vapor, which makes it possible to characterise bacteria and other biological samples close to their natural, hydrated state. Artificial model-biofilms of exopolysaccharides, planktonic Pseudomonas Fluorescens and biofilms of Escherichia Coli have been characterised in hydrated and dried state. High-resolution XPS-spectra from carbon, oxygen, nitrogen and phosphorous can be assigned to carbohydrates, lipids and proteins in general agreement with literature. Especially the carbon 1s peak is of interest. A series of measurements of an E. coli biofilm from 11 mbar in humid environment to 1 mbar air reveal changes in the C1s peak, which suggests that the bacterial surface undergo substantial Change. T2 - BAM PhD-retreat CY - Warnemünde, Germany DA - 28.09.2018 KW - Biofilms KW - E. coli KW - NAP-XPS PY - 2018 AN - OPUS4-46132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja A1 - Saleh, Maysoon I. A1 - Unger, Wolfgang T1 - Investigation of core-shell nanoparticles using a combination of scanning Auger microscopy (SAM) and scanning electron microscopy (SEM) N2 - Products containing engineered nanoparticles already encounter us in most areas of our daily life including cosmetics, clothing, detergents, paints, batteries and displays. In most cases the particles exhibit a core-shell morphology either voluntarily or involuntarily. The properties of the nanoparticle shell determine the interaction with their environment and, thus, reliable control over these properties means reliable control over the particles performance and their toxicity. Therefore, sophisticated techniques to measure thickness and elemental composition of the nanoparticle shell are urgently required. Scanning Auger microscopy (SAM) is a powerful technique with a lateral resolution below 10 nm and a chemical contrast based on the characteristic kinetic energy of Auger electrons related to specific atomic levels and, thus, to a specific element. This work explores the potential of SAM for characterizing the core-shell structure of nanoparticles. A sample system of upconversion NaYF4:Yb,Er cores coated with SiO2 is investigated. Auger spectra, line scans and elemental maps of single nanoparticles will be presented. Challenges encountered will be highlighted, such as damage to the sample by electron beam irradiation. Scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) are performed on the same samples, in order to verify the SAM results. T2 - BAM PhD Retreat CY - Warnemünde, Germany DA - 28.09.2018 KW - Core-shell nanoparticles KW - SAM KW - SEM KW - Surface analysis PY - 2018 AN - OPUS4-46270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cant, D. A1 - Shard, A. A1 - Müller, Anja A1 - Clifford, C. A1 - Wirth, Thomas A1 - Unger, Wolfgang T1 - Surface chemical analysis – Electron spectroscopies – Measurement of the thickness and nature of nanoparticle coatings N2 - Recent years have seen increasing development of nanoparticles for applications in a wide range of fields, including but not limited to areas of great impact such as catalysis, medicine, energy, optoelectronics, cosmetics, and many others. In particular, nanoparticles bearing some form of coating layer, whether by design or due to incidental processes such as contamination or oxidation, are among the most commonly studied and utilised. In the characterisation of nanoparticles, the surface properties are of great importance, because a large proportion of the particle forms a part of the surface or interface. In the case of coated nanoparticles, the thickness of the coating is significant in determining the properties of the nanoparticle, and defines its interactions with its environment. Measurement of surface chemistry and coating thickness of nanoparticles is a challenge to which electron spectroscopies are well suited, due to high surface sensitivity, well-understood physical principles and accessibility. T2 - Annual Meeting of ISO/TC 201/SC7 CY - Cancun, Mexico DA - 21.09.2018 KW - Nanoparticle characterization KW - X-ray Photoelectron Spectroscopy (XPS) KW - Auger Electron Spectroscopy (AES) KW - Core-shell nanoparticles PY - 2018 AN - OPUS4-46259 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian A1 - Emmerling, Franziska T1 - Mechanochemie N2 - In 3 Minuten sollte das Thema der Dissertation ohne zusätzliche Materialien vorgestellt werden. T2 - FameLab Germany 2018 CY - Potsdam, Germany DA - 15.03.2018 KW - Mechanochemie PY - 2018 AN - OPUS4-46319 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas A1 - Müller, Anja A1 - Unger, Wolfgang T1 - Chemical characterisation of (core-shell) nanoparticles using PCA assisted ToF-SIMS and XPS N2 - The analysis of nanomaterials is currently an important task - especially in case of risk assessment – as the properties of these material class are not well understood. The rather high surface area of these objects renders their interactions significantly different to their corresponding bulk. Thus, the surface’s chemical composition must be investigated to get a better understanding and prediction of the nanomaterials’ behavior. ToF-SIMS and XPS have proven to be powerful tools to determine the general chemical composition. The superior surface sensitivity of ToF-SIMS furthermore allows us to study mainly the utmost atomic layers and thus gives us an idea of the interactions involved. Here, we present initial data on the analysis of Hyflon®-polystyrene core-shell nanoparticles which can be used as a model system due to the known preparation and a rather good chemical as well as physical separation of core and shell. Furthermore, results on Au nanoparticles with and without an antibody shell are presented. Principle component analysis (PCA) will be used to detect the influence of sample preparation and for a better separation of different samples. ToF-SIMS imaging is desired to be implemented for single particle detection as well. T2 - 3rd NanoSafety Forum for Young Scientists CY - Valetta, Malta DA - 08.09.2018 KW - Nanoparticles KW - ToF-SIMS KW - XPS PY - 2018 AN - OPUS4-46248 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas A1 - Müller, Anja A1 - Schneider, Markus A1 - Sparnacci, Katja A1 - Unger, Wolfgang T1 - Chemical characterisation and classification of (Core-Shell) nanoparticles using PCA assisted ToF-SIMS N2 - The analysis of nanomaterials is currently an important task - especially in case of risk assessment – as the properties of these material class are not well understood and their growing use in everyday life. The rather high surface area of these objects renders their interactions significantly different to their corresponding bulk. Thus, the surface’s chemical composition must be investigated to get a better understanding and prediction of the nanomaterials’ behaviour. ToF-SIMS and XPS have proven to be powerful tools to determine the general chemical composition. The superior surface sensitivity of ToF-SIMS furthermore allows us to study mainly the utmost atomic layers and thus gives us an idea of possible interactions involved. Supported by multivariate data analysis such as principal component analysis (PCA), the method can also be used for sub-classification of different materials using slight differences in surface chemistry. Here, we present data of the analysis of Hyflon®-polystyrene core-shell nanoparticles which can be used as a model system due to the known preparation and a rather good chemical as well as physical separation of core and shell. Principle component analysis (PCA) will be used to detect the influence of sample preparation and for a better separation of different samples. This is achieved by measurement of a statistically relevant set of samples for every particle sample. We acquired surface spectra under static SIMS conditions with Bi32+ and analysed the resulting spectra by PCA. The carefully selected and refined peaks allow a reasonable categorization and further a reliable allocation of blank feeds. In detail, the fluorine containing, organic fragments are an indication for a heterogeneous shell that has errors. Furthermore, results on Au nanoparticles with and without an antibody shell are presented. ToF-SIMS imaging is desired to be implemented for single particle detection as well. T2 - SIMS-Europe CY - Münster, Germany DA - 16.09.2018 KW - Nanoparticles KW - ToF-SIMS KW - XPS KW - PCA KW - Titania KW - Core-Shell PY - 2018 AN - OPUS4-46249 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Overview on the most advanced and suitable NanoDefine measurement methods N2 - The EC Recommendation on the definition of nanomaterial, based solely on size of the constituent particles, foresees development of harmonised measurement methods ensuring ‘consistent results across materials and over time’. The EU/FP7 research project NanoDefine has been exclusively dedicated to support the implementation of this EC Recommendation for the European Union’s legislation. For the first time, measurement techniques able to determine the size of nanoparticles have been evaluated systematically on a well-defined set of quality control materials (spherical, monodisperse) as well as industrial materials of complex shapes and considerable polydispersity. Particularly based on the analytical performance of the measurement techniques as tested on the challenging real-world particulate materials, it was possible to formulate recommendations for use of a new tiered approach consisting of screening and confirmatory techniques. Thus, a consistent framework of guidance for nanomaterial identification according to the EC Definition has been issued in form of the NanoDefiner e-tool, with a transparent decision flow scheme and an extensive user manual. Selected examples of analysis and classification as nano-/non-nanomaterials will be given, highlighting the limits of applicability of the available measurement techniques in dependence on sample properties. On some recent relevant developments in sample preparation – as a crucial part for an accurate analysis - will be also reported. T2 - VCI-NanoDefine Follow-up Meeting CY - VCI, Frankfurt am Main, Germany DA - 25.09.2018 KW - Nanoparticles KW - Nanomaterial KW - EC definition of nanomaterial KW - Nanoparticle size distribution PY - 2018 AN - OPUS4-46251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - EMPIR nPSize - improved traceability chain of nanoparticle size measurements - Is a liaison to CEN/TC 352 nanotechnologies useful? N2 - The main objectives of the new EMPIR project nPSize are to establish EU capability of traceable measurement of NP size and shape, lower uncertainties of NP size measurement by developement of new nano-CRMs, new models (physical and machine learning), 3D method combination, and also by new ISO and CEN standards on accurate NP size measurement and guidance and knowledge transfer. The envisaged outcomes of the project will be presented and their suitability will be discussed to be taken over as pertinent contributions to normative projects within CEN/TC 352 Nanotechnologies. T2 - Joint Working Groups and 24th CEN/TC 352 Nanotechnologies Meetings CY - DIN, Berlin, Germany DA - 09.10.2018 KW - Nanoparticles KW - Size KW - Particle size distribution KW - Particle shape KW - Traceability KW - Standardisation KW - CEN/TC 352 Nanotechnologies PY - 2018 AN - OPUS4-46252 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Thin polymer films as model systems for polymer nanocomposites N2 - Polymers at interfaces play a major role in a broad variety of applications ranging from engineering purposes (for instance polymer based nanocomposites) to high tech implications (for instance light emitting diodes). Here, thin films with thicknesses down to few nanometers are prepared on different substrates as model systems for polymer composites. The thin films are investigated by a combination of surface analytical and volume sensitive methods. As surface analytical methods atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and contact angle measurements (CAM) are employed. As volume sensitive broadband dielectric spectroscopy (BDS), specific heat spectroscopy (SHS), and ellipsometry are used. Especially attention is paid to understand the glass transition behavior of thin films because the glass transition is the key phenomenon determines the application of polymers also in thin films. To understand the glass transition behavior of thin films, which is controversially discussed in literature, a three layer model is discussed. Firstly, a mobile surface layer is assumed at polymer air interface of the film due to missing of segment/segment interactions. Secondly, in the middle of the film a bulk-like layer should be expected. Thirdly, for polymers having non-repulsive interactions with the substrate an irreversibly adsorbed layer is expected to be formed. Due the adsorption the molecular mobility of the segments in this layer is slowed down. What is measured for the glass transition of thin films is a complicated average of all of these effects. The different layers are hardly to address separately. Therefore, in the presentation especially model systems are selected and investigated to verify the layer model. T2 - Kolloquiumsvortrag and der Universität des Saarlandes CY - Saarbrücken, Gemany DA - 20.11.2018 KW - Thin polymer films PY - 2018 AN - OPUS4-46692 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René A1 - Hertwig, Andreas A1 - Hodoroaba, Vasile-Dan A1 - Krähnert, R. T1 - Multi-method analysis of pore-controlled mesoporous oxide materials N2 - Determining the porosity of catalytic layers is crucial for quality assurance. We present results of a multi-method study to determine thickness, porosity, dielectric function and other properties of pure and mixed iridium and titanium oxide layers used in electrocatalytic water splitting. T2 - European Optical Society Biennial Meeting (EOSAM) 2018 CY - Delft, The Netherlands DA - 08.10.2018 KW - Multi-method analysis KW - Mesoporous oxide materials KW - Electro catalytic water splitting KW - Electron probe X-ray microanalysis (EPMA) KW - Spectroscopic ellipsometry (SE) KW - Optical porosimetry PY - 2018 AN - OPUS4-46740 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - About Standardization and Analytics of Microplastics N2 - Presentation about national and international standardization of microplastic analysis, as well as the project RUSEKU T2 - Industrievereinigung Chemiefaser e.V. CY - Frankfurt, Germany DA - 26.02.2019 KW - Standardisation KW - Microplastic KW - Analysis PY - 2019 AN - OPUS4-47577 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Mikroplastik in der Umwelt und im Trinkwasser: Einordnung der Relevanz und der Methodik N2 - Überblick zur Thematik Mikroplastik mit speziellem Fokus auf Trinkwasser T2 - 20. Jahrestagung Trinkwasserringversuche Nordrhein-Westfalen – Niedersachsen CY - Osnabrück, Germany DA - 06.03.2019 KW - Trinkwasser KW - Umwelt KW - Mikroplastik PY - 2019 AN - OPUS4-47578 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Müller, Axel A1 - Grathwohl, P. A1 - Vogler, M. A1 - Scholz, K. T1 - Plastik im Boden, Aktueller Forschungsstand N2 - Der Vortrag gibt einen Überblick über ein laufendes Vorhaben zum Thema Mikroplastik in Böden. T2 - NUA-Veranstaltung "Plastik in Natur und Umwelt" CY - Münster, Germany DA - 08.03.2019 KW - Mikroplastik KW - Böden KW - Analytik PY - 2019 AN - OPUS4-47579 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Bannick, C. G. T1 - Harmonisierung von Untersuchungsverfahren für (Mikro-)Plastik in der Umwelt N2 - Im Rahmen der Thematik "Recycling von Kunststoffen" wird die Thematik "Mikroplastik" vorgestellt T2 - Berliner Recycling- und Rohstoffkonferenz CY - Berlin, Germany DA - 11.03.2019 KW - Mikroplastik KW - Standarisierung KW - Analytik PY - 2019 AN - OPUS4-47582 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike A1 - Eisentraut, Paul A1 - Dümichen, E. T1 - Analytik von Mikroplastik mittels Thermoextraktion Desorption Gas Chromatographie Massen Spektrometrie (TED-GC-MS): Nun auch die Luft? N2 - Der Vortrag gibt eine Überblick über die Messung von Mikroplastik mittels TED-GC-MS mit speziellem Fokus auf Luftgetragene Partikel T2 - Odour and Emissions of Plastic Materials CY - Kassel, Germany DA - 19.03.2019 KW - Mikroplastik KW - Standarisierung KW - Analytik PY - 2019 AN - OPUS4-47583 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska T1 - Structure analytics with Hard X-rays at the BAMline and µSpot beamlines N2 - An overview of the research areas at the structure analysis division is given. Specifically the in situ characterization of dynamic processes with hard X-ray diffraction and absorption spectroscopy at the BAMline and µSpot beamlines (BESSY-II). T2 - BAM-IFW Workshop CY - Dresden, Germany DA - 28.03.2019 KW - Structure analysis KW - X-ray Spectroscopy KW - Synchrotron KW - Beamline KW - Material characterization PY - 2019 AN - OPUS4-47695 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hertwig, Andreas T1 - Multi-methods surface analysis involving spectroscopic ellipsometry: New measurements for optical and energy applications N2 - Surface analysis is still gaining importance, as most modern technology is in essence surface and thin film technology. In microelectronics and optics but also in many fields of energy storage and conversion, thin surface layers or structured surfaces are key components. Optical surface measurements are useful because of their reliability, robustness, and scalability – properties, which are especially desirable in a production environment. However, many of these methods take require considerable effort in data analysis. Spectroscopic ellipsometry (SE) is maybe the prime example of this class of methods. To combine the advantages of SE with metrological trueness and traceability, we combine it in a group of other methods, such as electron microscopy, instrumental surface analysis, X-ray diffraction. This presentation will give an overview on the principles of SE, its available quantities and the general properties of this measurement technique. Several examples from current and past projects of BAM-6.7 will show how a measurement community involving ellipsometry can benefit many fields of interest, from polymer science to energy applications. In the context of creating a “measurement landscape”, standardisation and standard compliance play an important role. The efforts of BAM in standardisation and accrediting of ellipsometry will be shown demonstrating the possible impact on quality assurance in different fields of technology. T2 - Abteilungskolloquium 2018, BAM CY - BAM, Berlin, Germany DA - 12.12.2018 KW - Spectroscopic ellipsometry KW - Surface analysis KW - Thin film technology KW - Reference materials PY - 2018 AN - OPUS4-47671 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Daniel A1 - Beck, Uwe A1 - Schneider, S. A1 - Duwe, M T1 - Visualisierung von mikro- und nanoskalierten Oberflächenstrukturen mittels abbildender Ellipsometry N2 - In den letzten Jahren hat die Einbindung der abbildenden Ellipsometrie in die Gruppe der optischen Verfahren zur Oberflächencharakterisierung ein enormes Potential bei der Analyse von topologischen Strukturänderungen gezeigt. Der dabei abgebildete Kon-trast wurde typischerweise auf Änderungen im Brechungsindex, Absorptionseffekte oder Schichtdickenänderungen zurückgeführt. In späteren Studien wurde festgestellt, dass auch andere Faktoren, wie etwa die Krümmung der Oberfläche oder Kanten von Struktu-ren einen signifikanten Einfluss auf die Messung der ellipsometrischen Paramater haben. Um diese Effekte aus der ellipsometrischen Messung extrahieren zu können, wird auf die Analyse der Müller-Matrix zurückgegriffen. In dem hier vorliegenden Beitrag wird gezeigt, wie die Müller-Matrix-Imaging Ellipsomet-rie (MM-IE) zur Charakterisierung von Oberflächenstrukturen verwendet werden kann. Dazu werden mikro- und nanoskaliert gekrümmte Oberflächen zunächst mit verschiede-nen Referenzmethoden, wie Rasterelektronenmikroskopie (SEM), Lichtmikroskopie (OM), Weißlichtinterferenzmikroskopie (WLIM) und Rasterkraftmikroskopie (AFM) vali-diert erfasst. Der anschließende Vergleich mit den Ergebnissen der Müller-Matrix-Ima-ging-Ellipsometrie ermöglicht eine Korrelation der zugrunde liegenden Strukturphäno-mene mit den ellipsometrischen Daten. In diesem Artikel wird das Prinzip an drei industriell relevanten Strukturgruppen demonstriert: Sub-Mikropartikel, Mikropartikel und sub-mikroskalierte Vertiefungen. T2 - 14. ThGOT Thementage Grenz- und Oberflächentechnik CY - Zeulenroda, Germany DA - 12.03.2019 KW - Ellipsometrie KW - Nanoskaliert KW - Mikroskaliert KW - Oberflächengeometrie KW - Brechungsindex KW - Müller-Matrix-Ellipsometrie PY - 2019 AN - OPUS4-47645 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulow, Anicó A1 - Witte, S. A1 - Beyer, S. A1 - Streli, C. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - de Oliveira Guilherme Buzanich, Ana T1 - Time- and lateral-resolved X-ray absorption fine structure spectroscopy N2 - X-ray absorption fine structure (XAFS) spectroscopy is a powerful and widely used tool for material characterization. It is non-destructive, element-sensitive and requires no long-range order of the sample, making it suitable for the investigation of amorphous phases. XAFS includes the X-ray absorption near edge structure (XANES) and the extended X-ray absorption fine structure (EXAFS), providing information about the electronical state of the absorbing atom and the spatial order of the neighboring atoms respectively. Our new approach presented here is derived from the classical dispersive XAFS setup. The aim is to have a scanningless, stable and reproducible setup for applications, in which dynamic processes occur in the second time scale. A broad polychromatic beam passes through the sample and is dispersed afterwards by a convexly bent Si (111) crystal. All energies are reflected under different angles and thus spatially separated, allowing a position sensitive detector to record a spectrum over the energy range of the incoming beam in a single shot. Tests of this setup were performed at the BAMline @ BESSY-II (Berlin, Germany) with different metal foils. First in situ measurements comprised the investigation of the early stages of the zinc(II)2-methylimidazolate (ZIF-8) crystallization. This topic of metal-organic-frameworks (MOF) research is of interest for medical applications. Structural changes with a time resolution of 1 s could be followed. The second dimension of the broad beam can be used for a lateral resolution. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - X-ray absorption fine structure KW - Synchrotron based methods KW - X-ray spectroscopy PY - 2019 AN - OPUS4-47660 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Hielscher-Hofinger, Stefan A1 - Lange, Thorid A1 - Weise, Matthias A1 - Lerche, D. A1 - Rietz, U. T1 - CAT-Technologie zur Bestimmung der Haftfestigkeit Dünner Schichten N2 - Der Vortrag widmet sich der „CAT-TECHNOLOGIE ZUR BESTIMMUNG DER HAFTFESTIGKEIT DÜNNER SCHICHTEN“ und beschreibt die Punkte „Motivation –CAT-Technologie“ (CAT: Centrifugal Adhesion Testing) und die „Haftfestigkeit von Schichten“, (Ag-Schichten auf N-BK7 Glas, Cr- und Al-Schichten auf Borofloat 33 Glas, Au-Schichten auf N-BK7 Glas und SiO2-Schichten auf CR39 Polymer) im Einzelnen. T2 - EFDS, Workshop: Haft- und Antihaftschichten CY - Dresden, Germany DA - 31.01.2019 KW - CAT-Technologie KW - Centrifugal Adhesion Testing KW - Dünne Schichten KW - Haftfestigkeit PY - 2019 AN - OPUS4-47489 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen A1 - Lauer, F. A1 - Seifert, S. A1 - Diehn, S. A1 - Kneipp, Janina T1 - MALDI-TOF MS und MALDI-MSI zur Identifikation und Klassifizierung von Pollen N2 - Es werden die letzten Ergebnisse präsentiert, die es ermöglichen, einzelne Pollenkörner unterschiedlicher Arten in Mischungen mittels MALDI-TOF Massenspektrometrie bzw. MALDI-TOF Imaging zu messen und unter Zuhilfenahme multivariater Auswertemethoden zu klassifizieren. T2 - 24. Bruker MALDI Anwendertreffen CY - Leipzig, Germany DA - 18.02.2019 KW - MALDI-TOF Massenspektrometrie KW - Pollenkörner KW - Klassifizierung KW - MALDI Imaging KW - Multivariate Analyse PY - 2019 AN - OPUS4-47441 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kunz, Valentin T1 - Surface chemical transformations of nanoparticles N2 - Nanomaterials are a relatively new class of materials for which a regulatory framework still has to be established and regulators require comprehensive datasets of well characterized nanomaterials for the implementation. Especially information about the surface chemistry of nanoparticles is crucial, since it largely determines their biological and environmental fate. How the surface chemistry changes under relevant ageing conditions is of particular interest, because exposure will normally occur not to the pristine material but to a nanoform that underwent some kind of transformation. In this talk, first a short overview about the contributions of division 6.1 to multiple European-funded projects will be presented, in which surface analytical techniques are used to improve the physical-chemical characterization of nanomaterials. Secondly, a study investigating the surface-chemical transformations of a representative set of titanium dioxide nanoparticles is discussed in more detail. The ageing has partly been performed at the BAM division 7.5, and the surface chemistry was analyzed using time-of-flight secondary ion mass spectrometry (ToF-SIMS) and X-ray photoelectron spectroscopy (XPS). By analyzing the complex mass spectra with principal component analysis (PCA), it was possible to identify even subtle changes that occur upon ageing. T2 - Abteilungsseminar CY - BAM, Berlin, Germany DA - 25.2.2019 KW - Nanoparticles KW - Surface Chemistry KW - Ageing KW - Titanium Dioxide KW - ToF-SIMS PY - 2019 AN - OPUS4-47444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Hielscher-Hofinger, Stefan A1 - Lange, Thorid A1 - Hidde, Gundula A1 - Lerche, D. A1 - Rietz, U. T1 - CAT-Technologie zur Bestimmung der Klebfestigkeit N2 - Der Vortrag widmet sich der „ CAT-TECHNOLOGIE ZUR BESTIMMUNG DER KLEBFESTIGKEIT“ und beschreibt die Punkte „Motivation –CAT-Technologie (Centrifugal Adhesion Testing), Klebfestigkeit ( Materialscreening verschiedener Werkstoffklassen, Klebstoffscreening fürV2A gegenV2A als Referenz, Klebstoffscreening für Niedrigenergie-Polymere und Oberfächenmodifizierung von Niedrigenergie-Polymeren) und Verbundfestigkeit (“Stirnabzug vs. Zug-Scher-Prüfung an CFK) im Einzelnen. T2 - 17. Praxisseminar KLEBEN CY - IWF Jena, Germany DA - 30.01.2019 KW - CAT-Technologie KW - Klebfestigkeit KW - Verbundfestigkeit KW - Niedrigenergie-Polymeren PY - 2019 AN - OPUS4-47466 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Repräsentative Untersuchungsstrategien für ein integratives Systemverständnis von spezifischen Einträgen von Kunststoffen in die Umwelt (RUSEKU) N2 - Im Rahmen des Statuskonferenz der BMBF Fördermassnahme wurde über den Projektfortschritt berichtet. T2 - Statusfonferenz der BMBF Fördermassnahme "Plastik in der Umwelt" CY - Berlin, Germany DA - 09.04.2019 KW - Sedimenttaionskasten KW - Probenahme KW - Mikroplastik KW - TED-GC-MS PY - 2019 AN - OPUS4-47796 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Mikroplastik Analytik: Probennahme, Probenaufbereitung, Detektionsverfahren N2 - Das Diskussionspapier zur Mikroplastik Analytik wurde vorgestellt. Es entstand im Rahmen des Querschnitthemas 1 des BMBF Forschungsschwerpunktes Plastik in der Umwelt. T2 - Statuskonferenz der BMBF Fördermassnahme "Plastik in der Umwelt" CY - Berlin, Germany DA - 09.04.2019 KW - Harmonisierung KW - Mikroplastik KW - Probenahme KW - Detektion KW - Aufbereitung PY - 2019 AN - OPUS4-47797 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steinhoff, U. A1 - Hodoroaba, Vasile-Dan T1 - EMPIR Erläuterung der Fördermaßnahme und Beispiele aus der Nanotechnologie N2 - Das EMPIR-Förderprogramm wird kurz erläutert und laufende Projekte aus der Nanotechnologie werden vorgestellt. Der Schwerpunkt liegt auf Standardisierungsprojekten, die gemeinsam mit ISO/TC 229 'Nanotechnologies' und CEN/TC 352 'Nanotechnologies' zu neuen Normen führen sollten. Als Beispiel für laufende Nanotechnologie-Projekte mit Koordination aus Deutschland werden MagNaStand (PTB) und nPSize (BAM) gegeben. T2 - Treffen des Normungsausschusses NA 062-08-17 AA Nanotechnologien CY - KIT, Karlsruhe, Germany DA - 07.03.2019 KW - EMPIR KW - Nanoparticles KW - Reference materials KW - Particle size distribution KW - Traceability KW - Standardisation PY - 2019 AN - OPUS4-47859 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Surface and Microbeam Analytical Methods @BAM N2 - An overview of the activities in the field of surface and microbeam analysis at BAM-6.1 is given with focus on physico-chemical characterization at the nanoscale. Ideas of potential joint activities are presented: structural and chemical analysis of graphene, deposition techniques for nanoparticles, EBSD on steel for a broader range of methods, instruments and types of steel, soft X-ray Analysis of low-Z materials, analysis of mesoporous thin films, etc. T2 - BAM-IFW Workshop CY - Dresden, Germany DA - 28.03.2019 KW - PC characterisation KW - Nanoscale KW - Nanoparticles PY - 2019 AN - OPUS4-47860 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana A1 - Epping, Ruben T1 - View into the depths of copolymer microstructure by a special approach of LC-MS data evaluation N2 - It is a well-known story that copolymers beside their molar mass distribution (MMD) can exhibit a functionality type distribution (FTD), a copolymer composition distribution (CCD), a monomer sequence distribution (MSD) and additionally different topologies within one sample. This is and will remain a challenge for analysts. First a very short overview will be given concerning the common liquid separation techniques for polymers (SEC, LAC, LCCC, GELC) coupled to soft ionization mass spectrometric methods like MALDI and ESI-MS with focus on their limitations. For very broadly distributed samples or chemical very similar species the superposition of different separation mechanisms in chromatography is unavoidable or the separation efficiency cannot be optimized. Different ionization probabilities and species of the same nominal mass with completely different structures are just two problems of mass spec of complex polymer mixtures. Subsequently, different examples will be shown how these limitations in some cases could be outsmarted. First example will be the separation of statistical EO-PO copolymers of different chemical compositions by end group functionality and the quantification of end group fractions over the whole CCD. Here an UP-LCCC / ESI-TOF-MS coupling is applied. Further for different kinds of polymers it will be shown how it could be realized to obtain information on small isobaric/isomeric topological heterogeneities by coupling UP-SEC / ESI-TOF-MS. All results are based on the data processing of reconstructed ion chromatograms of single mass traces of complex ESI-MS spectra. T2 - SCM-9 CY - Amsterdam, The Netherlands DA - 29.01.2019 KW - Reconstructed ion chromatograms KW - Copolymer KW - Microstructure KW - LC x ESI-TOF-MS PY - 2019 AN - OPUS4-47836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulow, Anicó T1 - X-ray imaging with coded apertures N2 - Coded aperture imaging systems are in use in astrophysics since the 1960's. We want to adapt this technique for full field x-ray fluorescence imaging in combination with a color-x-ray-camera. T2 - Seminar des Atominstituts der TU Wien CY - Vienna, Austria DA - 14.05.2019 KW - Reconstruction KW - X-ray spectroscopy KW - X-ray fluorescence KW - Spectroscopy KW - Imaging KW - Coded apertures PY - 2019 AN - OPUS4-47997 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard A1 - Breßler, Ingo A1 - Smales, Glen Jacob A1 - Laskina, Sofya A1 - Snow, T. A1 - Smith, A. T1 - 30.000+ datasets in an underground SciCat instance: the good, the bad, and the improvables. N2 - For the last four years, we have been running a SciCat instance to manage the projects and data in our X-ray scattering laboratory. We here report on the configuration of this SciCat instance, how it connects to the scientific workflow, and how it is integrated in the data pipeline. T2 - SciCat 2023 CY - Didcot, UK DA - 18.07.2023 KW - Scicat KW - X-ray scattering KW - Laboratory management KW - Research Data Management KW - Laboratory organization KW - RunDeck PY - 2023 AN - OPUS4-57958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane A1 - Menneken, Martina A1 - Nützmann, Kathrin A1 - Falk, Florian A1 - de Oliveira Guilherme Buzanich, Ana A1 - Witte, Steffen A1 - Radtke, Martin T1 - Early stages of high temperature oxidation/sulfidation studied by synchrotron x-ray diffraction and spectroscopy N2 - Ferritic high temperature alloys are widely used as boiler tube and heat exchanger materials in coal, biomass and co-fired power plants. All technologies have in common that the applied materials are exposed to different temperatures, process pressures and reactive atmospheres that lead to a change of the material properties and a further degradation of the material. Material changes caused by aging in highly corrosive and toxic gases such as SO2 are mainly studied ex situ after the reaction is finished. The solid material is deposited in the atmosphere for a certain period of time, and material changes are then examined by various microscopic techniques such as optical microscopy (OM), electron microprobe analysis (EMPA), scanning electron microscopy (SEM and TEM) and X-ray diffraction (XRD). Nevertheless, extensive efforts were made to study material changes of high temperature alloys under oxidizing and reducing atmospheres by environmental scanning electron microscopy or in situ TEM techniques However, the possibilities of microscopic in situ techniques are very limited for the use of highly corrosive and toxic gases such as SO2. Since Sulfur induced corrosion at temperatures relevant for coal and biomass fired power plants, which is causing breakaway oxidation and sulfide precipitation at grain boundaries, is still of scientific interest, the current work focuses on the effect of SO2 in an initial stage of corrosion of ferritic alloys. For the analysis of early stages of combined oxidation and sulphidation processes of Fe-Cr model alloys the usage of a light furnace to conduct a rapid reactive annealing experiment is feasible. Previous studies presented distinct results of the influence of chromium on early high temperature corrosion by SO2 by this technique and subsequent classical metallographic analyses. However, it is still not possible to trace the corrosion mechanism in real time by conducting single aging experiments. The current work introduces two different approaches to study the initial stages of high temperature oxidation processes by applying above state of the art X-ray diffraction and spectroscopy methods. One part focuses on the real time observation of the formation of corrosion products such as oxides and sulfides by energy dispersive X-ray diffraction (EDXRD). The potential of this technique to study crystallization and growth processes of thin films in a reactive environment in real time was previously shown for different compound semiconductors. This approach was now applied to follow oxidation and sulphidation processes of ferritic model alloys in SO2 and SO2/H2O environments. The diffraction signals of the X-rays were detected during the corrosion process and the peak area and positions were analyzed as a function of time. This procedure enables monitoring external oxide growth and material loss in real time in an early stage of corrosion. The other part of the current work presents the possibilities of X-ray absorption near edge structure spectroscopy (XANES) to characterize oxide scales and their growth mechanisms. Precise phase identification and quantification of corrosion products in a multi-phase oxide/sulfide scale is a pre-requisite to understand diffusion paths of metal ions and gas components. It is a challenging task to distinguish structurally similar reaction products such as Fe3O4 and FeCr2O4 especially in thin films with texture effects by diffraction. To illustrate for example Cr-out diffusion of an alloy throughout an inner and external oxide scale the differentiation of Fe3O4 and FeCr2O4 is indispensable. XANES uses the photoionization effect at the metal absorption edge in an aging product and accesses by this structural and chemical information. The current work uses XANES at the Fe-K and Cr-K absorption edge to identify various aging products grown as thin layers on alloys after short time aging experiments. A reaction chamber for combining high temperature oxidation experiments with surface sensitive X-ray absorption near edge structure spectroscopy will be introduced and first results of XANES on scales at high temperatures will be presented. T2 - ISHOC 2018 CY - Matsue, Japan DA - 22.10.2018 KW - Corrosion KW - Sulfidation KW - In situ KW - Diffraction KW - XANES PY - 2018 AN - OPUS4-47278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane A1 - Nützmann, Kathrin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Menneken, Martina A1 - Falk, Florian T1 - High temperature oxidation/sulfidation meets X-ray absorption near edge structure spectroscopy (XANES) N2 - Ferritic-martensitic alloys with 12-16 % Cr in weight are subject to devices for various energy systems, such as coal power plants and waste incineration plants. These materials are exposed to a highly corrosive environment which lead to a degradation of the material. Especially the simultaneous oxidation and sulfidation is thereby of special interest. Proper spatially resolved measurements that determine not only chemical compositions but phases are rare. However, precise phase identification and quantification of corrosion products within the multi-phase corrosion scales is a key aspect to understand diffusion paths of metal ions and gas ions/molecules. This study investigated Fe-Cr model alloys with Cr contents from 0 to 13 % in weight in 0.5 % SO2 and 99.5 % Ar atmosphere to aim in a fundamental and systematic analysis. Samples were aged at 650 °C for time scales from 12 h to 250 h. The results presented here correspond to depth dependent phase identification of oxide and sulphide phases in the corrosion scales by using X-ray absorption near edge spectroscopy (XANES). Per sample a series of ca. 20 spots (1-5 µm spot size) from scale-gas to scale-metal interface were measured. XANES spectroscopy was performed at the Fe-K edge (7.11 keV) on polished cross sections. The collected spectra were fitted to a combination of reference materials to quantify the present phases at different positions within the scale.The phase distribution differs with Cr content and the Cr diffusion through pure Fe-oxide and mixed Fe-Cr-oxide phases is discussed. T2 - EFC Workshop "High Temperature Corrosion" CY - Frankfurt am Main, Germany DA - 26.09.2018 KW - High temperature corrosion KW - XANES PY - 2018 AN - OPUS4-47277 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saadeh, Qais A1 - Pauw, Brian Richard A1 - Thünemann, Andreas A1 - Günster, Jens T1 - In-Situ SAXS Techniques N2 - Our project's aim is to enhance the capabilities of additive manufacturing techniques, where enabling a Two-Photon-Polymerization (TPP) 3D printer of producing arrays of precisely aligned nanoparticles is of an enormous value. As heterogeneous functional nanostructures with arrays of oriented nanoparticles are very promising in many fields; electrochemistry, energy storage, nanoelectronics among other vital fields. The feasibility and the convenience of orienting nanoparticles using magnetic, electric fields and ultrasonic vibrations will be systematically investigated, using Small Angle X-ray Scattering (SAXS), since SAXS can provide detailed information about the orientation characteristics of nano-Ensembles. Corresponding to our prerequisites, a set ad hoc functional sample holders, sample stages and other In-Situ SAXS solutions were developed, and incorporated to be compatible with a state-of-the-arts SAXS machine, called Multi-scale Analyzer for Ultrafine Structures (MAUS). The MAUS has been customized and engineered to serve as a miniaturized synchrotron, and that is exactly what we need. Experiments attempting to orient superparamagnetic nanoparticles will be discussed, where the outcomes will not only help in understanding the mechanics of field-particle interactions, it will also help in further developing the adequate needed set of corrections to the SAXS data, that is especially regards oriented samples. T2 - XVII International Small Angle Scattering Conference – SAS 2018 CY - Traverse City, Michigan, USA DA - 07.10.2018 KW - In-Situ Techniques KW - SAXS KW - Magnetic nano-particles PY - 2018 AN - OPUS4-46443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dalgic, Mete-Sungur T1 - Lösemittelfreie Probenpräparation zur Untersuchung von Polymerblends mittels MALDI-TOF MS N2 - Die Probenpräparation ist ein wichtiger Schritt für die Qualität der Massenspektren in MALDI-TOF MS. Es werden Polymerproben, die lösungsmittelbasiert und lösungsmittelfrei präpariert worden sind, verglichen. Dabei werden die Intensitätsverhältnisse von ternären Mischungen von PEG-, PS- und PMMA-Polymeren beachtet. T2 - 28. Kolloquium - Massenspektrometrische Techniken zur Untersuchung synthetischer Polymere CY - Berlin, Germany DA - 14.05.2024 KW - Polymere KW - Massenspektrometrie KW - Probenpräparation PY - 2024 AN - OPUS4-60032 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna A1 - Milczewski, Frank A1 - Ciornii, Dmitri A1 - Hodoroaba, Dan T1 - Preliminary results of an interlaboratory comparison on microplastics organised by plasticsfate N2 - Microplastics are everywhere in the environment, but analytics is challenging. Since harmonisation is missing as well es suitable reference materials, BAM did under th umbrella of VAMAS funded by the EU Horizon 2020 project PlasticsFate a ILC for microplastic detection methods. Methods adressed were IR, Raman, Py-GC/MS and TED-GC/MS. The talk gives a first presentation and evaluation on the results. T2 - CUSP annual meeting and conference CY - Utrecht, Netherlands DA - 12.09.2023 KW - Microplastics KW - TED-GC/MS KW - Polymer 3R KW - Reference material KW - ILC on detection methods PY - 2023 AN - OPUS4-60036 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -