TY - CONF A1 - Müller, Anja A1 - Schneider, Markus A1 - Heinrich, Thomas T1 - Surface chemical analysis of engineered nanoparticles by means of transmission x-ray microscopy and mass spectrometry N2 - PTFE/PS core-shell-nanoparticles were characterised by STXM, T-SEM, and ToF-SIMS. Shell-thicknesses were calculated and compared. Preliminary results from ToF-SIMS showed the capabilities of this method. T2 - BAM-BfR Seminar CY - Berlin, Germany DA - 15.02.2018 KW - STXM KW - NEXAFS KW - ToF-SIMS KW - SEM KW - Nanoparticles PY - 2018 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-44181 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen A1 - Kricheldorf, H. A1 - Scheliga, F. T1 - Cyclic polylactides via ring-expansion polymerization N2 - We will report on a new kind of ring-expansion polymerization (REP) of cyclic esters based of three classes of catalysts. In contrast to REP described previously these new polymerizations are characterized by a self-extrusion of the catalysts resulting in cyclic homopolyesters as the only reaction product. These REP of L-lactide were performed in bulk at temperatures between 100 and 180°C without racemization. A simplified scheme of a REP catalyzed by BuCa or SnBi is presented below. With meso-lactide temperatures down to 60°C were realized. Depending on catalyst, time and temperature with equal quantities of even and odd-numbered cycles a strong predominance of either even or odd-numbered cycles was found. T2 - 255th ACS National Meeting CY - New Orleans, LA, USA DA - 18.03.2018 KW - MALDI-TOF MS KW - Poly(lactide) KW - Polymerisation KW - Catalysts PY - 2018 AN - OPUS4-44833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Lessons on measurement of nanoparticle size and shape learnt from NanoDefine N2 - The EC Recommendation on the definition of nanomaterial1, 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 large research project NanoDefine (http://www.nanodefine.eu) 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 (https://labs.inf.fh-dortmund.de/NanoDefiner), 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 - RSC-NPL Symposium: Nanoparticle concentration – critical needs and state-of-the-art measurement CY - London, UK DA - 24.04.2018 KW - Nanoparticles KW - Nanomaterial KW - Particle size distribution KW - EU definition of nanomaterial PY - 2018 AN - OPUS4-44804 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Hielscher, Stefan A1 - Lange, Thorid A1 - Grunwald, Daniel A1 - Stockmann, Jörg M. A1 - Lerche, D. A1 - Rietz, U. T1 - Die Zentrifuge als universelles Prüfsystem für Beanspruchungen auf Zug und Druck N2 - Mit der Zentrifugentechnologie ist seit einigen Jahren ein neuartiges Mehr-Proben-Prüf-verfahren auf dem Markt etabliert, welches die klassische Zugprüfung in den Trommelrotor einer Tischzentrifuge überträgt. In der Beanspruchung auf Zug ist die Prüfung der Verbundfestigkeit mittels CAT-Technologie (centrifugal adhesion testing) an der BAM seit 2017 nach DIN EN ISO/IEC 17025 akkreditiert, wobei die Verbundfestigkeit von Klebungen direkt bestimmt wird und in Abhängigkeit von den Versagensformen Rückschlüsse auf die Klebfestigkeit von Klebstoffen/Klebebändern oder die Haftfestigkeit von Beschichtungen gezogen werden können. T2 - 13. ThGOT Thementage Grenz- und Oberflächentechnik und 11. Thüringer Biomaterial-Kolloquium CY - Zeulenroda, Germany DA - 13.03.2018 KW - Zentrifugentechnologie KW - Haftfestigkeit KW - Härteprüfung KW - Mehr-Proben-Prüfung KW - Beanspruchung auf Zug und Druck PY - 2018 AN - OPUS4-44570 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Baier, Jennifa A1 - Hidde, Gundula A1 - Sahre, Marion A1 - Weise, Matthias T1 - Particles in PVD-coatings: Imperfection or functional add-on feature? N2 - The application of PVD-coatings ranges from mechanical engineering, i.e. thicker tribological coatings, to precision optics, i.e. thinner optical coatings. For physical vapor deposition (PVD) technologies such as evaporation, sputtering, ion beam assisted/driven deposition, vacuum is a prerequisite for two reasons: at first process-related ones (evaporation source, plasma discharge, and mean free path) and at second coating-related ones (pure, perfect, and dense films). Usually, the goal is a homogenous coating of defined stoichiometry and micro-structure without any imperfection. However, the implementation of micro- or nano-particles may occur accidentally or delibe-rately. Independent of the particle origin, there are two fundamental rules regarding coating functionality: at first, the larger the particle diameter to coating thickness ratio the more affected the functionality of the coating, and at second, the larger the material contrast in terms of the functional feature of interest the more affected the coating performance. Hence, embedded particles have to be avoided for the majority of thin films by all means. The unintended implementation of particles usually results in a malfunction of the coating from the beginning or is at least considered as a weak point of the coating creating a time-dependent defect under service conditions. The intended implementation of particles on surfaces and in coatings may create add-on features, topographic ones and functional ones, however, the facts mentioned hold true. Examples of particle-initiated coating defects are demonstrated in dependence on the origin and the field of application. Strategies for deliberate attachment/embedding of particles on surfaces/in coatings are discussed regarding process compatibility and coating integrity. For industrial applications, both the validation of process compatibility of particle injection and the plasma resistance of particles under vacuum and plasma conditions have to be confirmed. Further points of interest are the homogeneity of particle distribution and the avoidance of particle agglomeration which is still a crucial point for dry dispersed particles. So far, technical applications are limited to PVD hybrid coatings, plasma dispersion coatings are still a challenge except for applications where homogeneity is not required as in case of product authentication. T2 - ICMCTF 2018, International Conference on Metallurgical Coatings and Thin Films CY - San Diego, CA, USA DA - 23.04.2018 KW - PVD-coatings KW - PVD-processes KW - Unintended particle generation KW - Particles as imperfections KW - Deliberate particle implementation KW - Particles as add-on features PY - 2018 AN - OPUS4-44973 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Yamamoto, K. A1 - Grulke, E. A. A1 - Maurino, V. T1 - Shape controlled TiO2 nanoparticles as candidates for nano-CRM’s – an ISO case study N2 - Extraction of true, 3D shape (and size) of non-spherical nanoparticles (NPs) is associated with errors by conventional 2D electron microscopy using projection images. Significant efforts within the ISO technical committee TC 229 ‘Nanotechnologies’ are aimed at establishing accurate TEM and SEM measurement of NP size and shape as robust, standard procedures. Study groups have been organizing inter-laboratory comparisons on well-selected NP systems according to the market needs, such as aggregated titania nano-powder for which size and shape distribution of primary crystallites of irregular shape must be measured accurately. To be noticed is e. g. the fact that the measurement procedure allows only manual selection of the particles clearly distinguishable for analysis as well as manual definition of the contour of the imaged NPs. An inter-laboratory exercise on titania NPs (pure anatase, grown by hydrothermal synthesis) of well-defined non-spherical shape, i.e. bipyramidal has been recently started within ISO/TC 229 under similar conditions as for the irregular shaped titania. Overlapped particles were allowed to be considered, as long as they are clearly distinguishable. One decisive NP selection criterion was to analyze only those NPs with a roundness value below 0.7, i.e. the NPs laying on the support foil and, hence, with projection areas clearly deviating from perfect circles (R=1). The overall evaluation (for 15 labs) of the size descriptors (area, Feret, minFeret, perimeter) and shape descriptors (aspect ratio, roundness, compactness, extent) by analysis of variance is just to be finished and included in ISO/WD 21363 Nanotechnologies -- Protocol for particle size distribution by transmission electron microscopy. T2 - NanoWorkshop 2018 (Workshop on reference nanomaterials, current situation and needs: development, measurement, standardization) CY - Berlin, Germany DA - 14.05.2018 KW - Titanium oxide KW - Nanoparticles KW - Shape-controlled KW - Electron microscopy KW - Reference material PY - 2018 AN - OPUS4-44996 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saloga, Patrick E. J. T1 - Messdatenauswertung mittels Origin in der Nanopartikelanalyse N2 - Die Anwendung der Software Origin zur Datenauswertung in der Nanopartikelanalyse wird anhand eines Beispiels vom Importieren der Daten über deren Verarbeitung bis zur graphischen Ausgabe demonstriert. T2 - ADDITIVE Origin Anwendertage 2018 CY - Berlin, Germany DA - 12.03.2018 KW - Silbernanopartikel KW - Origin KW - SAXS PY - 2018 AN - OPUS4-44458 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Measurement of nanoparticle size and shape distribution – Current situation and outlook 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. Further, ISO/TC 229 ‘Nanotechnologies’ activities aiming at establishing accurate TEM and SEM measurement of NP size and shape as robust, traceable, standard procedures are highlighted. With participation of BAM, study groups have been organizing inter-laboratory comparisons on well-selected NP systems according to the market needs, such as aggregated or shape-controlled titania nano-powder for which size and shape distribution of primary particles must be measured accurately. T2 - Symposium Preparation, Characterization and Processing of Nano and Submicron Powders CY - Berlin, Germany DA - 14.06.2018 KW - Nanoparticles KW - Nanomaterial KW - EC definition KW - Nanoparticle size distribution PY - 2018 AN - OPUS4-45191 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Glass transition of thin polymeric films as revealed by calorimetric and dielectric techniques N2 - The structure and dynamics of thin polymeric films is reviewed and discussed in the frame work of novel theoretical approaches T2 - Lähnwitzseminar on Calorimetry CY - Rostock-Warnemünde, Germany DA - 03.06.2018 KW - Thin polymeric films KW - Dielectric spectroscopy KW - Thermal süectroscopy PY - 2018 AN - OPUS4-45164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - Observations of the deuterium distribution and the structural changes in standard and lean duplex stainless steels by ToF-SIMS and EBSD N2 - Duplex (DSS) and austenitic stainless steels (ASS) are frequently used in many energy related applications. The duplex grade is considered to have outstanding mechanical properties as well as good corrosion resistance. The austenitic phase combines high ductility, even at low temperatures, with sufficient strength, and therefore such materials are applied in storage and transport of high-pressure hydrogen. During service in acidic environments large amounts of hydrogen can ingress into the microstructure and induce many changes in the mechanical properties of the steel. Embrittlement of steels by hydrogen remains unclear even though this topic has been intensively studied for several decades. The reason for that lies in the inability to validate the proposed theoretical models in the sub-micron scale. Among the very few available methods nowadays, Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) enables a highly accurate mapping of hydrogen in the microstructure in a spatial resolution below 100 nm. In the present work ToF-SIMS was used as a main tool in order to investigate the effect of deuterium on a duplex microstructure of lean and standard DSSs during and after the electrochemical charging process. Electrochemical charging simulates the service of a component in acidic environments under conditions of cathodic protection that are commonly applied to prevent corrosion reactions. ToF-SIMS after multivariate data analysis (MVA) was combined with high resolution topographic images and electron back-scattered diffraction (EBSD) data to characterize the structural changes. It was observed that the ferritic phase was affected almost identical in all steels whereas in the austenitic phase significant differences were obtained in the lean duplex in comparison to the standard DSS. The obtained results have been compared to similar investigations on a AISI 304L austenitic stainless steel. The advantage of the combined techniques is reflected by the ability to correlate the hydrogen distribution in the microstructure and the resulted phase transformation. T2 - Third International Conference on Metals & Hydrogen CY - Ghent, Belgien DA - 29.05.2018 KW - Data-fusion KW - ToF-SIMS KW - PCA KW - DSS KW - LDX KW - EBSD PY - 2018 AN - OPUS4-45094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -