TY - JOUR A1 - Yin, Huajie A1 - Chua, Y. Z. A1 - Yang, B. A1 - Schick, C. A1 - Harrison, W. A1 - Budd, P. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - First clear cut experimental evidence for a glass transition in a polymer with intrinsic microporosity: PIM-1 N2 - Polymers with intrinsic microporosity (PIMs) represent a novel, innovative class of materials with great potential in various applications from high-performance gas separation membranes to electronic devices. Here for the first time, for PIM-1, as the archetypal PIM, fast scanning calorimetry provides definitive evidence for a glass transition (Tg=715 K, heating rate 3·10^4 K/s) by decoupling the time-scales responsible for glass transition and decomposition. As the rigid molecular structure of PIM-1 prevents any conformational changes, small-scale bend and flex fluctuations must be considered the origin of its glass transition. This result has strong implications for the fundamental understanding of the glass transition and for the physical aging of PIMs and other complex polymers, both topical problems of materials science. KW - Polymers with intrinsic microporosity KW - Fast Scanning Calorimetry PY - 2018 DO - https://doi.org/10.1021/acs.jpclett.8b00422 SN - 1948-7185 VL - 9 IS - 8 SP - 2003 EP - 2008 PB - ACS AN - OPUS4-44683 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tuma, Dirk A1 - Moreau, A. A1 - Polishuk, I. A1 - Segovia, J. J. A1 - Vega-Maza, D. A1 - Martín, M. C. T1 - Measurements and predictions of densities and viscosities in CO2 + hydrocarbon mixtures at high pressures and temperatures: CO2 + n-pentane and CO2 + n-hexane blends N2 - This work reports new experimental data on densities and viscosities of (CO2 + n-pentane) and (CO2 + n-hexane) mixtures at high pressures and temperatures. The densities were measured by a vibrating-tube densimeter with an expanded uncertainty (k = 2) smaller than 1.8 kg/m3 at six isotherms (from 273.15 K to 373.15 K), twelve pressures starting at 5 MPa up to 100 MPa, and at six CO2 molar compositions (from 0 to 0.6). The viscosities were measured by a vibrating-wire viscometer with the corresponding relative expanded uncertainty (k = 2) smaller than 0.016 at five isotherms (from 273.15 K to 373.15 K), twelve pressures (from 5 MPa up to 100 MPa), and at two CO2 molar compositions (0.1 and 0.3). The densities were fitted by the semiempirical Tammann-Tait equation for density data and the Vogel-Fulcher-Tammann (VFT) equation for viscosity data, respectively. The Groupe Européen de Recherches Gazières (GERG-2008) equation of state was also applied for modelling the densities. Over-all robustness and reliability of the Perturbed-Chain Statistical Association Fluid Theory (PC-SAFT) and its critical point-based modification (CP-PC-SAFT) were examined. Accuracies of the Modified Yarranton-Satyro (MYS) coupled with CP-PC-SAFT and the NIST Reference Fluid Thermodynamic and Transport Properties Database (REFPROP 10) in predicting the viscosities were evaluated. KW - CO2 + n-alkanes KW - thermophysical properties KW - Perturbed-Chain Statistical Association Fluid Theory PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555728 DO - https://doi.org/10.1016/j.molliq.2022.119518 SN - 0167-7322 VL - 360 SP - 1 EP - 15 PB - Elsevier CY - Amsterdam AN - OPUS4-55572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Gruskovà, J. A1 - Martin, G. A1 - Kresten, O. A1 - Mitthoff, F. A1 - Kaska, K. A1 - Hofmann, C. A1 - Kreuzer, W. A1 - Phelps, M. A1 - Boydston, K. A1 - Easton Jr., R. L. A1 - Knox, K. T. A1 - Kelbe, D. A1 - Kasotakis, D. A1 - Christens-Barry, W. A. A1 - Stewart, D. A1 - Rabin, Ira A1 - Hahn, Oliver A1 - Glaser, L. A1 - Garrevoet, J. A1 - Shevchuk, I. A1 - Klumpp, S. A1 - Deckers, D. A1 - Buck, J. ED - Cronier, M. ED - Mondrain, B. T1 - Insights-into-the-Digital-Recovery-of-the-Scythica-Vindobonesia N2 - The Scythica Vindobonensia, the new fragments on Gothic incursions into Roman provinces in the Balkans in the middle of the third century AD that were revealed some years ago in a Greek palimpsest at the Austrian National Library in Vienna (ÖNB), are commonly considered as one of the most important additions of the last decades to the corpus of texts from classical Antiquity. Tere is a high degree of confdence among scholars in supposing that the fragments come from the lost work Scythica written in Greek by the third-century historian P. Herennius Dexippus (Δέξιππος) of Athens. The new fragments have hence also been called Dexippus Vindobonensis. In his Scythica, Dexippus recorded wars of the Romans with the Goths (and other tribes) whom he called Scythians. The work had been hitherto known only from excerpts and quotes by later authors. Eight pages of a Byzantine manuscript copy of the ancient text have survived hidden underneath the visible surface of the last four parchment folios of the Vienna manuscript Historicus graecus 73, f. 192r -195v4. The copy is written in a Greek calligraphic minuscule which has been estimated by palaeographers to be of the middle or the second half of the eleventh century. In the thirteenth century, the text (on each of the eight pages arranged in one column, with 30 lines per page) was washed of the parchment and the valuable material made from animal skin was re-used for Christian texts. The new writing largely covered the faded remnants of the original text. It thus became hidden from the human eye for more than seven hundred years. Its discovery by Jana Grusková, a classical philologist specialized in the transmission of Greek texts, resulted from a systematic review of all Greek palimpsests kept at the Austrian National Library in Vienna at the beginning of the twenty-first century and a detailed examination of the four folios in 2007-20097. KW - Scythica Vindobonensia, KW - Gothic incursions KW - A Greek palimpsest KW - Antiquity KW - Byzantine manuscript KW - Vienna manuscript PY - 2020 SN - 978-2-916716-81-7 SN - 0577-1471 VL - 2020 IS - 24/1 SP - 945 EP - 967 PB - Association des Amis du Centre d’Histoire et Civilisation de Byzance CY - Paris ET - 1 AN - OPUS4-53843 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chan, George C.-Y. A1 - Hieftje, Gary M. A1 - Omenetto, Nicoló A1 - Axner, Ove A1 - Bengtson, Arne A1 - Bings, Nicolas H. A1 - Blades, Michael W. A1 - Bogaerts, Annemie A1 - Bolshov, Mikhail A. A1 - Broekaert, José A.C. A1 - Chan, WingTat A1 - Costa-Fernández, José M. A1 - Crouch, Stanley R. A1 - De Giacomo, Alessandro A1 - D’Ulivo, Alessandro A1 - Engelhard, Carsten A1 - Falk, Heinz A1 - Farnsworth, Paul B. A1 - Florek, Stefan A1 - Gamez, Gerardo A1 - Gornushkin, Igor B. A1 - Günther, Detlef A1 - Hahn, David W. A1 - Hang, Wei A1 - Hoffmann, Volker A1 - Jakubowski, Norbert A1 - Karanassios, Vassili A1 - Koppenaal, David W. A1 - Kenneth Marcus, R. A1 - Noll, Reinhard A1 - Olesik, John W. A1 - Palleschi, Vincenzo A1 - Panne, Ulrich A1 - Pisonero, Jorge A1 - Ray, Steven J. A1 - Resano, Martín A1 - Russo, Richard E. A1 - Scheeline, Alexander A1 - Smith, Benjamin W. A1 - Sturgeon, Ralph E. A1 - Todolí, José-Luis A1 - Tognoni, Elisabetta A1 - Vanhaecke, Frank A1 - Webb, Michael R. A1 - Winefordner, James D. A1 - Yang, Lu A1 - Yu, Jin A1 - Zhang, Zhanxia T1 - Landmark Publications in Analytical Atomic Spectrometry: Fundamentals and Instrumentation Development N2 - The almost-two-centuries history of spectrochemical analysis has generated a body of literature so vast that it has become nearly intractable for experts, much less for those wishing to enter the field. Authoritative, focused reviews help to address this problem but become so granular that the overall directions of the field are lost. This broader perspective can be provided partially by general overviews but then the thinking, experimental details, theoretical underpinnings and instrumental innovations of the original work must be sacrificed. In the present compilation, this dilemma is overcome by assembling the most impactful publications in the area of analytical atomic spectrometry. Each entry was proposed by at least one current expert in the field and supported by a narrative that justifies its inclusion. The entries were then assembled into a coherent sequence and returned to contributors for a round-robin review. KW - Analytical atomic spectrometry KW - Spectroscopy KW - Instrumental analysis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621588 DO - https://doi.org/10.1177/00037028241263567 SN - 1943-3530 VL - 78 SP - 1 EP - 456 PB - Sage CY - London AN - OPUS4-62158 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lozano-Martín, D. A1 - Moreau, A. A1 - Vega-Maza, D. A1 - Chamorro, C. R. T1 - High-pressure density data of binary (carbon dioxide + oxygen) mixtures for the development of equation-of-state models N2 - On the way to a low carbon economy mixtures containing carbon dioxide become increasingly important. Processing of such gas mixtures requires reliable thermodynamic models that can accurately describe the state of matter over an extended range. Mixtures with oxygen for example, are frequently encountered in carbon capture and storage (CCS) processes. This work reports new experimental (p, rho, T) data at T = (250 to 375 K) and up to a maximum pressure pmax = 20 MPa for five binary (CO2 + O2) mixtures which cover the entire composition range. T2 - 31st European Symposium on Applied Thermodynamics CY - Online meeting DA - 05.07.2021 KW - Binary mixtures CO2 + O2 KW - Density measurements KW - Equations of state PY - 2021 AN - OPUS4-53990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Voss, Heike A1 - Zahedi-Azad, Setareh A1 - Ernst, Owen C. A1 - Lucaßen, Jan A1 - Mann, Guido A1 - Bonse, Jörn A1 - Boeck, Torsten A1 - Martin, Jens A1 - Schmid, Martina A1 - Krüger, Jörg T1 - Chemical vapor deposition of indium precursors for solar microabsorbers using continuous laser radiation BT - A, Materials science & processing N2 - Localized deposition of indium on an amorphous glass surface covered with a thin molybdenum layer is demonstrated utilizing laser-assisted chemical vapor deposition. A continuous-wave laser causes a temperature rise on the molybdenum layer resulting in the selective aggregation of liquid and ultimately crystalline structures of indium. The formation sites of the indium are determined by the decomposition of gaseous trimethylindium. The deposited indium islands can serve as precursors and could be further processed into compound semiconductors like CuInSe2 for micro-concentrator solar cells. The experimental investigations were supported by theoretical simulations of the laser heating process to calculate the local temperature distribution on the surface of the molybdenum-covered glass substrate. KW - Laser-assisted Chemical Vapor Deposition KW - CW Laser KW - Indium Islands KW - Micro-concentrator Solar Cell PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641069 DO - https://doi.org/10.1007/s00339-025-08895-z SN - 0947-8396 VL - 131 SP - 1 EP - 10 PB - Springer CY - Berlin ; Heidelberg [u.a.] AN - OPUS4-64106 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lezhnina, M.M. A1 - Kätker, H. A1 - Kaiser, Martin A1 - Stegemann, L. A1 - Voss, E. A1 - Resch-Genger, Ute A1 - Strassert, C. A1 - Kynast, U. T1 - Chemical behavior and spectroscopic properties of rare earth borates in glazes N2 - Efficient Near UV excited materials (350<λ<400 nm) responding with green line emission are sparse in comparison to higher energy UV excited emitters (λ<350 nm), while corresponding red line emitters are more abundant, albeit typically also restricted to excitation wavelengths below 400 nm. This situation is disadvantageous for several important actual and potential applications. Among these, excitation with high power UV-LEDs and laser diodes are of particular interest. Here we present results on green emitting YBO3:Ce, Tb, which can be excited with 370–380 nm radiation at quantum efficiencies of up to 60% and decay times in excess of 2 ms. Moreover, as powderous phosphors typically require stable matrices to be hosted in, we investigated low melting, lead- and fluoride-free glasses for their capability to accommodate the phosphor and yet retain its optical properties. In these, we even observed an increase of the quantum efficiencies of up to 70% at decay times approaching 3 ms. Finally, we characterized the thermal quenching behavior, which showed a clear advantage of the phosphors in glassy matrices. KW - Rare earth phosphors KW - Energy transfer KW - Luminescent glasses and glazes PY - 2016 DO - https://doi.org/10.1016/j.jlumin.2015.05.005 SN - 0022-2313 SN - 1872-7883 VL - 170 SP - 387 EP - 394 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-35131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Wiesler, F. A1 - Hund-Rinke, K. A1 - George, E. A1 - Greef, J.-M. A1 - Holz, F. A1 - Hölze, L.E. A1 - Hülsbergen, K.-J. A1 - Martin, S. A1 - Severin, K. A1 - Spielvogel, S. A1 - Geiger, P. A1 - Nawotke, C. A1 - Kehlenbeck, H. A1 - Schenkel, H. A1 - Adam, Christian A1 - Bloem, E. A1 - Frank, D. A1 - Goldbach, H.E. A1 - Heene, M. A1 - Kratz, S. A1 - Kruse, A. A1 - Möller, K. A1 - Pinnekamp, J. A1 - Schoumans, O.F. A1 - Vogel, Christian A1 - Wulf, S. T1 - Recyclingphosphate in der Düngung – Nutzen und Grenzen N2 - Weltweit werden etwa 80–85 % aller abgebauten Rohphosphate für die Produktion von Düngemitteln verwendet. Bei noch steigendem Bedarf an Phosphor (P) geht man derzeit davon aus, dass die weltweiten P-Reserven noch über 200 Jahre ausreichen. Um den P-Vorrat langfristig abzusichern, sollte der in Reststoffen enthaltene Phosphor möglichst umfänglich genutzt werden. Dieser Forderung trägt das von der Bundesregierung 2012 erstmals beschlossene Deutsche Ressourceneffizienzprogramm ProgRess Rechnung. Rohphosphat wird auch seitens der Europäischen Kommission aufgrundseiner ökonomischen Bedeutung und des unsicheren Angebots als „kritischer Rohstoff“ eingestuft. Vor diesem Hintergrund hat die Bundesregierung in der Verordnung zur Neuordnung der Klärschlammverwertung vom 27. September 2017 in Deutschland eine verpflichtende technische Rückgewinnung von Phosphor für Abwasserbehandlungsanlagen ab einer Ausbaugröße von 100.000 Einwohnerwerten (12 Jahre nach Inkrafttreten der Verordnung) bzw. ab einer Ausbaugröße von über 50.000 Einwohnerwerten (15 Jahre nach Inkrafttreten der Verordnung) vorgeschrieben. Die Verordnung enthält keine Vorgaben hinsichtlich der anzuwendenden Technologie bei der Phosphorrückgewinnung. Ausgenommen von der Rückgewinnungspflicht sind Klärschlämme mit niedrigen Phosphorgehalten (weniger als 20 Gramm Phosphor je Kilogramm Klärschlamm-Trockenmasse). Auch die im Jahre 2017 verabschiedeten neuen Rechtsvorschriften für die Düngung verlangen zukünftig einen nachhaltigen und ressourceneffizienten Umgang mit Nährstoffen bei der landwirtschaftlichen Erzeugung und schränken die P-Zufuhr insbesondere auf hoch versorgten Böden ein (Düngeverordnung vom 26. Mai 2017). Dies wird zu einem mehr am Pflanzenbedarf orientierten und ggf. vermehrt überbetrieblichen Einsatz von wirtschaftseigenen Düngern führen. Um den politischen und gesetzlichen Anforderungen gerecht zu werden, müssen einerseits wirksame und kosteneffiziente technische Verfahren zum P-Recycling (weiter)entwickelt werden. Andererseits müssen die Recyclingprodukte die Anforderungen für eine direkte Verwendung in der Landwirtschaft oder als Rohstoff für die Herstellung von Düngemitteln erfüllen. In dem vorliegenden Standpunkt wird zunächst der potenzielle Beitrag von Reststoffen zur Deckung des P-Bedarfs in der deutschen Pflanzenproduktion geschätzt. Für die wichtigsten Reststoffe werden technische Verfahren zur P-Rückgewinnung bzw. Aufarbeitung skizziert. Auf Basis der Anforderungen der Landwirtschaft bzw. der Düngemittelindustrie an die P-Recyclingprodukte werden deren Herstellungsverfahren bewertet. Schließlich wird der Regelungs- und Forschungsbedarf formuliert. KW - Phosphor KW - Düngemittel KW - Diffusive Gradients in thin films (DGT) PY - 2020 SP - 1 EP - 19 PB - Bundesministerium für Ernährung und Landwirtschaft (BMEL) CY - Berlin AN - OPUS4-51011 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markwart, Jens C. A1 - Battig, Alexander A1 - Zimmermann, Lisa A1 - Wagner, Martin A1 - Fischer, Jochen A1 - Schartel, Bernhard A1 - Wurm, Frederik R. T1 - Systematically controlled decomposition mechanism in phosphorus flame retardants by precise molecular architecture: P−O vs P−N N2 - Flame retardants (FR) are inevitable additives to many plastics. Halogenated organics are effective FRs but are controversially discussed due to the release of toxic gases during a fire or their persistence if landfilled. Phosphorus-containing compounds are effective alternatives to halogenated FRs and have potential lower toxicity and degradability. In addition, nitrogencontaining additives were reported to induce synergistic effects with phosphorus-based FRs. However, no systematic study of the gradual variation on a single phosphorus FR containing both P−O and P−N moieties and their comparison to the respective blends of phosphates and phosphoramides was reported. This study developed general design principles for P−O- and P−N-based FRs and will help to design effective FRs for various polymers. We synthesized a library of phosphorus FRs that only differ in their P-binding pattern from each other and studied their decomposition mechanism in epoxy resins. Systematic control over the decomposition pathways of phosphate (PO(OR)3), phosphoramidate (PO(OR)2(NHR)), phosphorodiamidate (PO(OR)(NHR)2), phosphoramide (PO(NHR)3), and their blends was identified, for example, by reducing cis-elimination and the formation of P−N-rich char with increasing nitrogen content in the P-binding sphere. Our FR epoxy resins can compete with commercial FRs in most cases, but we proved that the blending of esters and amides outperformed the single molecule amidates/diamidates due to distinctively different decomposition mechanisms acting synergistically when blended. KW - Phosphorus KW - Flame retardants KW - Epoxies KW - Mechanistic study KW - Toxicity PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-481549 DO - https://doi.org/10.1021/acsapm.9b00129 SN - 2637-6105 VL - 1 IS - 5 SP - 1118 EP - 1128 PB - ACS AN - OPUS4-48154 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - Witte, S. A1 - Beyer, S. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, H. A1 - Streli, C. T1 - A new experimental setup for time- and laterally-resolved X-ray absorption fine structure spectroscopy in a 'single shot' N2 - In this work, a new setup for dispersive XAFS measurements is presented. This reproducible and scanningfree setup yields both time- and laterally-resolved XAFS experiments in a ‘single-shot’. It allows a straightforward adjustment for probing different elements covering many relevant applications in materials science. An incoming energetic broadband beam is diffracted by a Si (111) crystal after passing through the sample and collected by an area sensitive detector. Depending on the energy range of the incoming beam, XANES and/or EXAFS spectra can be recorded with a time resolution down to 1 s. The feasibility of this setup was demonstrated at the BAMline at BESSY II (Berlin, Germany) with reference Fe and Cu foils and the results are hereby presented and discussed. Additionally, an application where time resolution on the second scale is required is briefly evaluated. The presented example concerns studying early stages of zinc(II)2-methylimidazolate (ZIF-8) crystallization. This is particularly important for biomedical applications. KW - X-ray spectroscopy KW - X-ray absorption fine structure KW - Time-resolved KW - Laterally-resolved KW - Experimental setup PY - 2019 DO - https://doi.org/10.1039/c8ja00313k SN - 0267-9477 SN - 1364-5544 VL - 34 IS - 1 SP - 239 EP - 246 PB - Royal Society of Chemistry CY - London AN - OPUS4-47207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - De Samber, B. A1 - Scharf, Oliver A1 - Buzanich, Günter A1 - Garrevoet, J. A1 - Tack, P. A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Reinholz, Uwe A1 - Evens, R. A1 - De Schamphelaere, K. A1 - Falkenberg, G. A1 - Janssen, C. A1 - Vincze, L. T1 - Three-dimensional X-ray fluorescence imaging modes for biological specimens using a full-field energy dispersive CCD camera N2 - Besides conventional scanning X-ray fluorescence imaging at synchrotron sources, full-field X-ray fluorescence (FF-XRF) imaging techniques that do not implicitly require spatial scanning of the sample have become available. FF-XRF has become achievable thanks to the development of a new type of energy dispersive CCD-based 2D detector, also referred to as a 'color X-ray camera (CXC)' or 'SLcam'. We report on different imaging schemes for biological samples using FF-XRF imaging: (a) 2D 'zoom' imaging with pinhole optics using the 'camera obscura' principle; (b) 2D 'fixed magnification' imaging using magnifying polycapillary optics; and (c) 3D-FF-XRF imaging using an X-ray sheet beam or computed tomography (CT). The different FF-XRF imaging modes are illustrated using the crustacean Daphnia magna, a model organism for investigating the effects of metals on organism/ecosystem health, and foraminifera, a class of amoeboid protist. Detailed analytical characterization of the set-up is performed through analyzing various reference materials in order to determine limits of detection (LODs) and sensitivities. Experiments were performed using the BAMline at the BESSY synchrotron (Berlin, Germany) and using the P06 Hard X-ray Microprobe at the PETRAIII synchrotron (Hamburg, Germany). KW - CXC KW - BAMline KW - Maia detector KW - Synchrotron PY - 2019 DO - https://doi.org/10.1039/c9ja00198k VL - 34 IS - 10 SP - 2083 EP - 2093 PB - Royal Society of Chemistry CY - Cambridge, United Kingdom AN - OPUS4-49359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - López de Ipina, J.-M. A1 - Arevalillo, A. A1 - Martín, A. A1 - Caillard, B. A1 - Marcoulaki, E. A1 - Aguerre- Charol, O. A1 - van Duuren-Stuurman, B. A1 - Hodoroaba, Vasile-Dan A1 - Viitanen, A.-K. A1 - Witters, H. A1 - Vercauteren, S. A1 - Persson, K. A1 - Bard, D. A1 - Evans, G. A1 - Jensen, K.A. A1 - Himly, M. A1 - Scalbi, S. A1 - Papin, A. A1 - Le Bihan, O. A1 - Kanerva, T. A1 - Tirez, K. A1 - Frijns, E. A1 - Niga, P. A1 - Eleftheriadis, K. A1 - Travlos, A. A1 - Geppert, M. A1 - Himly, M. A1 - Radnik, Jörg A1 - Kuchenbecker, Petra A1 - Resch-Genger, Ute A1 - Fraboulet, I. A1 - Bressot, C. A1 - Rissler, J. A1 - Gaucher, R. A1 - Binotto, G. A1 - Krietsch, Arne A1 - Braun, A. A1 - Abenet, S. A1 - Catalan, J. A1 - Verstraelen, S. A1 - Manier, N. A1 - Manzo, S. A1 - Fransman, S. A1 - Queron, J. A1 - Charpentier, D. A1 - Taxell, D. A1 - Säämänen, A. A1 - Brignon, J.-M. A1 - Jovanovic, A. A1 - Bisson, M A1 - Neofytou, P. T1 - EC4Safenano - Catalogue of Services N2 - The publicly available document encapsulates the first version of the Catalogue of Services of the future EC4Safenano Centre (CoS 2019). The CoS 2019 is structured in 12 Service Categories and 27 Service Topics, for each of the 12 categories considered. This architecture configures a 12 x 27 matrix that allows ordering the potential EC4Safenano offer in 324 types of services/groups of services. Each type of service/group of services is described, in a simple and friendly way, by means of a specific service sheet: the EC4Safenano - Service Data Sheet (EC4-SDS). These EC4-SDSs allow structuring and summarizing the information of each service, providing the customer with a concise view of characteristics of the service and also the contact details with the service provider. The CoS 2019 deploys a map of services consisting of a set of 100 EC4-SDSs, covering 7 of the 12 Service Categories and 17 of the 27 Service Topics. The harmonization of services is visualized as a future necessary step in EC4Safenano, in order to strengthen the offer and provide added value to customers with a growing offer of harmonized services in future versions of the CoS. The information contained in this document is structured in 3 main sections, as follows: • Catalogue structure. This section describes in short the main characteristics of the CoS 2019. • Catalogue content. This section represents the core part of the document and encapsulates the set of 100 SDSs displaying the offer proposed by the CoS 2019. • Online Catalogue. This section describes the resources implemented by EC4Safenano to facilitate the on-line consultation of the CoS 2019 by customers and other interested parties. KW - Nano-safety KW - Analytical services KW - Nanomaterials KW - Catalogue of services KW - EC4SafeNano KW - European Centre PY - 2021 UR - https://ec4safenano.eu-vri.eu/Public/Guidance SP - 1 EP - 72 PB - EU-VRi – European Virtual Institute for Integrated Risk Management CY - Stuttgart, Germany AN - OPUS4-52943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Manso, M. A1 - Pessanha, S. A1 - Guerra, M. A1 - Reinholz, Uwe A1 - Afonso, C. A1 - Radtke, Martin A1 - Lourenco, H. A1 - Carvalho, M. L. A1 - de Oliveira Guilherme Buzanich, Ana T1 - Assessment of Toxic Metals and Hazardous Substances in Tattoo Inks Using Sy-XRF, AAS, and Raman Spectroscopy N2 - Synchrotron radiation X-ray fluorescence spectroscopy, in conjunction with atomic absorption and Raman spectroscopy, was used to analyze a set of top brand tattoo inks to investigate the presence of toxic elements and hazardous substances. The Cr, Cu, and Pb contents were found to be above the maximum allowed levels established by the Council of Europe through the resolution ResAP(2008)1 on requirements and criteria for the safety of tattoos and permanent makeup. Raman analysis has revealed the presence of a set of prohibited substances mentioned in ResAP(2008)1, among which are the pigments Blue 15, Green 7, and Violet 23. Other pigments that were identified in white, black, red, and yellow inks are the Pigment White 6, Carbon Black, Pigment Red 8, and a diazo yellow, respectively. The present results show the importance of regulating tattoo ink composition. KW - Synchrotron KW - Tattoo inks KW - XRF KW - Toxic metals KW - Hazardous substances PY - 2019 DO - https://doi.org/10.1007/s12011-018-1406-y VL - 187 IS - 2 SP - 596 EP - 601 PB - Springer AN - OPUS4-47369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Constantinescu, B. A1 - Bugoi, R. A1 - Cojocaru, V. A1 - Radtke, Martin A1 - Calligaro, T. A1 - Salomon, J. A1 - Pichon, L. A1 - Röhrs, S. A1 - Ceccato, D. A1 - Oberländer-Târnoveanu, E. A1 - Ionescu, C. A1 - Pop, D. T1 - Dacian bracelets and Transylvanian gold: ancient history and modern analyses KW - SRXRF KW - Gold KW - Archaeometrie KW - Authentication KW - Provenance KW - XRF KW - Micro-PIXE KW - Micro SR-XRF KW - Or KW - Authentification KW - FX PY - 2009 SN - 0399-1237 VL - 33 SP - 221 EP - 225 PB - Groupe CY - Rennes AN - OPUS4-23172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Buzanich, Günter A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Thünemann, Andreas A1 - Streli, C. T1 - Impurities in multicrystalline silicon wafers for solar cells detected by synchrotron micro-beam X-ray fluorescence analysis N2 - We report on the trace analysis of copper and iron impurities in multicrystalline silicon wafers with the microbeam X-ray fluorescence (µ-XRF) technique. The efficiency of solar cells, which are based on multicrystalline silicon wafers, is strongly influenced by minor contamination with metals such as copper and iron. Application of compound refractive lenses (CRLs) in µ-XRF allows versatile two-dimensional mapping of relevant contaminations and localization of their sites of deposition. In this context, the measured bulk average limit of detection (LOD) was one picogram of iron and copper per gram of silicon. We suggest that µ-XRF is a valuable tool for non-destructive spatial (3D) quantification of metal impurities in a wide range of materials and devices whose functioning could be critically affected by impurities. KW - X-ray micro beam KW - Compound refractive lens KW - Solar cell KW - Silicon impurities PY - 2012 DO - https://doi.org/10.1039/c2ja30188a SN - 0267-9477 SN - 1364-5544 VL - 27 IS - 11 SP - 1875 EP - 1881 PB - Royal Society of Chemistry CY - London AN - OPUS4-26791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lutz, C. A1 - Hampel, S. A1 - Beuermann, S. A1 - Turek, T. A1 - Kunz, U. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Fittschen, U. E. A. T1 - Investigation on Vanadium Species Distribution in Nafion™ 117 after Cyclization in a Vanadium Redox Flow Battery N2 - The vanadium redox flow battery (VRFB) is currently a potential candidate for stationary energy storage. A major challenge is the unintended vanadium transport through the separator, which results in a fade of capacity. To overcome this issue, it is necessary to understand the transport processes in the membrane on a more fundamental level. In this work, the vanadium species distribution in Nafion™ 117 after cyclization was investigated. Two membranes, one from a charged VRFB and another from a discharged VRFB, were analyzed using ultraviolet–visible spectroscopy (UV/VIS) and X-ray absorption near edge structure spectroscopy (XANES). Little difference between the two membranes was recognizable according to the UV/VIS results. In comparison, the XANES results showed that the membrane from the charged VRFB contains more V3+ than VO2+, whereas for the discharged case, more VO2+ is present in the membrane. KW - Synchrotron KW - BAMline KW - XANES KW - Vanadium redox flow battery PY - 2021 VL - 64 SP - 1 EP - 8 AN - OPUS4-54144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lutz, C. A1 - Hampel, S. A1 - Ke, X. A1 - Beuermann, S. A1 - Turek, T. A1 - Kunz, U. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Fittschen, U. T1 - Evidence for redox reactions during vanadium crossover inside the nanoscopic water-body of Nafion 117 using X-ray absorption near edge structure spectroscopy N2 - A major source of capacity fade of the common vanadium redox flow battery (VRFB) is the vanadium ion transport through the separator. However, different transport models disagree significantly in the diffusion coefficient for the different V species and the influence of different transport mechanisms. The underlying hypothesis of this work is that reactions inside the membrane are partly responsible for these discrepancies. Accordingly, it was investigated if redox reactions inside the nanoscopic water body of Nafion 117 can occur. X-ray absorption near edge structure spectroscopy (XANES) was used to distinguish between the different V species inside hydrated Nafion 117 and novel PVDF-based membranes. It was validated that the speciation of vanadium can be performed using the pre-edge peak energy and intensity. The experiments were performed as follows: strips of the membrane were exposed from one site to a V3+ solution (green) and from the other site to a VO2+ solution (yellow). The ions could diffuse into the membrane from both sides. A change of color of the membrane strip was observed. The blue color in the middle of the strip indicated that VO2+ was formed where V3+ and VO2+ got in contact. Using XANES this reaction inside Nafion was proven. KW - PVDF-Based membrane KW - VRFB KW - Vanadium speciation KW - XANES KW - Nafion 117 PY - 2020 DO - https://doi.org/10.1016/j.jpowsour.2020.229176 VL - 483 SP - 229176 PB - Elsevier B.V. AN - OPUS4-51719 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grengg, C. A1 - Koraimann, G. A1 - Ukrainczyk, N. A1 - Rudic, O. A1 - Luschnig, S. A1 - Gluth, Gregor A1 - Radtke, Martin A1 - Dietzel, M. A1 - Mittermayr, F. T1 - Cu- and Zn-doped alkali activated mortar – Properties and durability in (bio)chemically aggressive wastewater environments N2 - Metakaolin-based alkali activated mortars (AAM) - with and without CuSO4·5H2O and ZnO addition (mass ratio Mn+/solid binder 0.08% to 1.7%) - were casted and exposed within an extensive long-term field campaign over the period of 20 months to a sewer basin, strongly affected by biogenic acid corrosion. (Un-)exposed AAM were tested regarding their physicochemical and microstructural properties, bioreceptivity and overall durability. Metal addition led to a retarding effect during alkali-activation reaction, as well as to an increase in open porosity of up to 3.0% and corresponding lower compressive strength of up to 10.9%. Reduced microbial colonization and diversity were observed on AAM with Cu, while Zn addition led to increased biodiversity. We propose that the observed higher durability of Cu-doped AAM is due to antibacterial effects and associated reduction of biogenic acid production, superseding overall negative effects of metal-dosage on physical material properties. Observed lower durability of Zn-doped AAM was related to combined negative physicochemical and microbial effects. KW - Microbially induced corrosion KW - Alkali-activated materials KW - Biogenic acid corrosion KW - Biogene Schwefelsäurekorrosion KW - MIC PY - 2021 DO - https://doi.org/10.1016/j.cemconres.2021.106541 SN - 0008-8846 VL - 149 SP - 1 EP - 15 PB - Elsevier CY - Oxford AN - OPUS4-53070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fittschen, U.E.A. A1 - Menzel, M. A1 - Scharf, O. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Buzanich, Günter A1 - Lopez, V.M. A1 - McIntosh, K. A1 - Streli, C. A1 - Havrilla, G.J. T1 - Observation of X-ray shadings in synchrotron radiation-total reflection X-ray fluorescence using a color X-ray camera N2 - Absorption effects and the impact of specimen shape on TXRF analysis has been discussed intensively. Model calculations indicated that ring shaped specimens should give better results in terms of higher counts per mass signals than filled rectangle or circle shaped specimens. One major reason for the difference in signal is shading effects. Full field micro-XRF with a color X-ray camera (CXC) was used to investigate shading, which occurs when working with small angles of excitation as in TXRF. The device allows monitoring the illuminated parts of the sample and the shaded parts at the same time. It is expected that sample material hit first by the primary beam shade material behind it. Using the CXC shading could be directly visualized for the high concentration specimens. In order to compare the experimental results with calculation of the shading effect the generation of controlled specimens is crucial. This was achieved by 'drop on demand' technology. It allows generating uniform, microscopic deposits of elements. The experimentally measured shadings match well with those expected from calculation. KW - TXRF KW - Full field micro-XRF KW - Color X-ray camera PY - 2014 DO - https://doi.org/10.1016/j.sab.2014.06.025 SN - 0584-8547 SN - 0038-6987 VL - 99 SP - 179 EP - 184 PB - Elsevier CY - Amsterdam AN - OPUS4-31180 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pogány, A. A1 - Balslev-Harder, D. A1 - Braban, Ch. F. A1 - Cassidy, N. A1 - Ebert, V. A1 - Ferracci, V. A1 - Hieta, T. A1 - Leuenberger, D. A1 - Martin, N. A. A1 - Pascale, C. A1 - Peltola, J. A1 - Persijn, S. A1 - Tiebe, Carlo A1 - Twigg, M. M. A1 - Vaittinen, Olavi A1 - van Wijk, J. A1 - Wirtz, K. A1 - Niederhauser, B. T1 - A metrological approach to improve accuracy and reliability of ammonia measurements in ambient air N2 - The environmental impacts of ammonia (NH3) in ambient air have become more evident in the recent decades, leading to intensifying research in this field. A number of novel analytical techniques and monitoring instruments have been developed, and the quality and availability of reference gas mixtures used for the calibration of measuring instruments has also increased significantly. However, recent inter-comparison measurements show significant discrepancies, indicating that the majority of the newly developed devices and reference materials require further thorough validation. There is a clear need for more intensive metrological research focusing on quality assurance, intercomparability and validations. MetNH3 (Metrology for ammonia in ambient air) is a three-year project within the framework of the European Metrology Research Programme (EMRP), which aims to bring metrological traceability to ambient ammonia measurements in the 0.5–500 nmol mol−1 amount fraction range. This is addressed by working in three areas: (1) improving accuracy and stability of static and dynamic reference gas mixtures, (2) developing an optical transfer standard and (3) establishing the link between high-accuracy metrological standards and field measurements. In this article we describe the concept, aims and first results of the project. KW - Ammonia in ambient air KW - Traceability KW - Reference gas standards KW - Optical transfer standard KW - Validation and testing infrastructure PY - 2016 DO - https://doi.org/10.1088/0957-0233/27/11/115012 SN - 0957-0233 VL - 27 IS - 11 SP - 115012 EP - 115026 PB - IOP Publishing Ltd. AN - OPUS4-39130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ordavo, I. A1 - Ihle, S. A1 - Arkadiev, V. A1 - Scharf, Oliver A1 - Soltau, H. A1 - Bjeoumikhov, A. A1 - Bjeoumikhova, S. A1 - Buzanich, Günter A1 - Gubzhokov, R. A1 - Günther, A. A1 - Hartmann, R. A1 - Holl, P. A1 - Kimmel, N. A1 - Kühbacher, M. A1 - Lang, M. A1 - Langhoff, N. A1 - Liebel, A. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Schaller, G. A1 - Schopper, F. A1 - Strüder, L. A1 - Thamm, C. A1 - Wedell, R. T1 - A new pnCCD-based color X-ray camera for fast spatial and energy-resolved measurements N2 - We present a new high resolution X-ray imager based on a pnCCD detector and a polycapillary optics. The properties of the pnCCD like high quantum efficiency, high energy resolution and radiation hardness are maintained, while color corrected polycapillary lenses are used to direct the fluorescence photons from every spot on a sample to a corresponding pixel on the detector. The camera is sensitive to photons from 3 to 40 keV with still 30% quantum efficiency at 20 keV. The pnCCD is operated in split frame mode allowing a high frame rate of 400 Hz with an energy resolution of 152 eV for Mn Kα (5.9 keV) at 450 kcps. In single-photon counting mode (SPC), the time, energy and position of every fluorescence photon is recorded for every frame. A dedicated software enables the visualization of the elements distribution in real time without the need of post-processing the data. A description of the key components including detector, X-ray optics and camera is given. First experiments show the capability of the camera to perform fast full-field X-Ray Fluorescence (FF-XRF) for element analysis. The imaging performance with a magnifying optics (3×) has also been successfully tested. KW - X-ray CCD camera KW - pnCCD KW - Fast X-ray imaging KW - XRF KW - Full-field X-ray fluorescence KW - Elemental analysis KW - High quantum efficiency KW - High energy resolution KW - Polycapillary optics PY - 2011 DO - https://doi.org/10.1016/j.nima.2011.05.080 SN - 0168-9002 SN - 0167-5087 VL - 654 SP - 250 EP - 257 PB - North-Holland CY - Amsterdam AN - OPUS4-24370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Görner, Wolf A1 - Berger, Achim A1 - Merchel, Silke A1 - Pernicka, E. A1 - Radtke, Martin A1 - Reiche, I. A1 - Reinholz, Uwe A1 - Riederer, J. A1 - Riesemeier, Heinrich A1 - Wunderlich, C. H. T1 - Kunst- und Kulturgüter unter "Beschuss" T2 - Jahrestagung Zerstörungsfreie Materialprüfung 2004 CY - Salzburg, Österreich DA - 2004-05-17 KW - SY-RFA KW - PIXE KW - PIGE KW - PAA KW - Zerstörungsfreie Analyse KW - Silberstiftzeichnungen KW - Himmelsscheibe von Nebra KW - Indische Moghulmalereien PY - 2004 UR - http://www.ndt.net/article/dgzfp04/papers/p46/p46.htm SN - 3-931381-55-2 SP - 1(?) EP - 11(?) PB - DGZfP CY - Berlin AN - OPUS4-6897 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - von Bohlen, A. A1 - Hergenröder, R. A1 - Sternemann, C. A1 - Paulus, M. A1 - Radtke, Martin A1 - Riesemeier, Heinrich T1 - Wavelenght Dispersive Synchrotron Microprobe Used for Material Analysis N2 - Synchrotron radiation (SR) has been used in recent years as an excellent excitation source for X-ray fluorescence spectrometry. SR offers, in contrast to conventional X-ray sources, highly brilliant polychromatic, polarized radiation with which micro-domain X-ray fluorescence spectrometry becomes possible. A feasibility study of utility, conducted at BESSY (Berlin) and at DELTA (Dortmund), both synchrotron facilities of the third generation, to evaluate the use of wavelength dispersive X-ray fluorescence spectrometry in combination with synchrotron radiation is presented. First results for material analysis, obtained by combining the synchrotron radiation and a commercially available spectrometer commonly attached to a scanning electron microscope, are presented. The spectrometer, of the linear type, uses curved focusing Bragg-crystals of the Johann type which leads to a high spectral resolution up to 3 eV. Examples of micro-domain analyses are presented and compared with those obtained by synchrotron radiation induced energy dispersive X-ray fluorescence. KW - Synchrotron radiation KW - WDXRF KW - EDXRF KW - Micro analysis KW - Material analysis PY - 2005 DO - https://doi.org/10.1081/CI-200048048 SN - 1073-9149 SN - 1525-6030 VL - 33 IS - 2 SP - 137 EP - 150 PB - Dekker CY - New York, NY AN - OPUS4-14235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reifschneider, O. A1 - Vennemann, A. A1 - Buzanich, Günter A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Hogeback, J A1 - Köppen, C. A1 - Großgarten, M. A1 - Sperling, M. A1 - Wiemann, M. A1 - Karst, U. T1 - Revealing Silver Nanoparticle Uptake by Macrophages Using SR-μXRF and LA-ICP-MS N2 - To better study the impact of nanoparticles on both in vitro and in vivo models, tissue distribution and cellular doses need to be described more closely. Here silver nanoparticles were visualized in alveolar macrophages by means of synchrotron radiation micro X-ray fluorescence spectroscopy (SR-μXRF) with high spatial resolution of 3 × 3 μm2. For the spatial allocation of silver signals to cells and tissue structures, additional elemental labeling was carried out by staining with eosin, which binds to protein and can be detected as bromine signal with SR-μXRF. The method was compatible with immunostaining of macrophage antigens. We found that the silver distribution obtained with SR-μXRF was largely congruent with distribution maps from a subsequent laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) of the same tissue sites. The study shows a predominant, though not exclusive uptake of silver into alveolar macrophages in the rat lung, which can be modeled by a similar uptake in cultured alveolar macrophages. Advantages and limitations of the different strategies for measuring nanoparticle uptake at the single cell level are discussed. KW - Synchrotron KW - BAMline KW - XRF KW - Nanoparticle KW - Macrophagen PY - 2020 DO - https://doi.org/10.1021/acs.chemrestox.9b00507 VL - 33 IS - 5 SP - 1250 EP - 1255 PB - American Chemical Society AN - OPUS4-50855 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gauert, C. A1 - Schannor, M. A1 - Hecht, L. A1 - Radtke, Martin A1 - Reinholz, Uwe T1 - A comparison of in situ analytical methods for trace element measurement in gold samples from various South African gold deposits N2 - Trace element concentrations in gold grains from various geological units in South Africa were measured in situ by field emission-electron probe microanalysis (FE-EPMA), laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) and synchrotron micro X-ray fluorescence spectroscopy (SR-µ-XRF). This study assesses the accuracy, precision and detection limits of these mostly non-destructive analytical methods using certified reference materials and discusses their application in natural sample measurement. FE-EPMA point analyses yielded reproducible and discernible concentrations for Au and trace concentrations of S, Cu, Ti, Hg, Fe and Ni, with detection limits well below the actual concentrations in the gold. LA-ICP-MS analyses required larger gold particles (> 60 µm) to avoid contamination during measurement. Elements that measured above detection limits included Ag, Cu, Ti, Fe, Pt, Pd, Mn, Cr, Ni, Sn, Hg, Pb, As and Te, which can be used for geochemical characterisation and gold fingerprinting. Although LA-ICP-MS measurements had lower detection limits, precision was lower than FE-EPMA and SR-µ-XRF. The higher variability in absolute values measured by LA-ICP-MS, possibly due to micro-inclusions, had to be critically assessed. Non-destructive point analyses of gold alloys by SR-µ-XRF revealed Ag, Fe, Cu, Ni, Pb, Ti, Sb, U, Cr, Co, As, Y and Zr in the various gold samples. Detection limits were mostly lower than those for elements measured by FE-EPMA, but higher than those for elements measured by LA-ICP-MS. N2 - Les concentrations en éléments traces de grains d'or provenant de différentes unités géologiques d'Afrique du Sud ont été mesurées in situ par microsonde électronique à émission de champ (FE-EPMA), spectrométrie de masse couplée à une source plasma et un système d'ablation laser (LA-ICP-MS) et micro spectroscopie de fluorescence des rayons X au Synchrotron (SR-µ-XRF). Cette étude évalue l'exactitude, la précision et les limites de détection de ces méthodes d'analyse pour la plupart non-destructives en utilisant des matériaux de référence certifiés, et discute de leur application dans les mesures sur échantillon naturel. Les points d'analyses FE-EPMA ont fournis des concentrations reproductibles et discernables pour l'Au et des concentrations en traces de S, Cu, Ti, Hg, Fe et Ni, avec des limites de détection bien inférieures aux concentrations réelles dans l'or. Les analyses LA-ICP-MS ont nécessitées des particules d'or de plus grande taille (> 60 µm) pour éviter toute contamination pendant la mesure. Les éléments mesurés au-dessus des limites de détection inclus Ag, Cu, Ti, Fe, Pt, Pd, Mn, Cr, Ni, Sn, Hg, Pb, A et Te, qui peuvent être utilisés pour les caractérisations géochimique et le «fingerprinting» de l'or. Bien que les mesures LA-ICP-MS aient des limites de détection plus basses, la précision est inférieure par rapport à celles de la microsonde FE et de la SR-µ-XRF. La plus grande variabilité des valeurs absolues mesurées par LA-ICP-MS, probablement reliée à la présence de micro-inclusions, a du être évaluée de manière critique. Les points d'analyse non-destructifs des alliages d'or par SR-µ-XRF ont révélés la présence de Ag, Fe, Cu, Ni, Pb, Ti, Sb, U, Cr, Co, As, Y et Zr dans les différents échantillons. Les limites de détection ont été pour la plupart inférieures à celles des éléments mesurés par FE-EPMA, mais supérieures à celles des éléments mesurés par LA-ICP-MS. KW - Trace elements KW - Gold KW - FE-EPMA KW - LA-ICP-MS KW - SR-µ-XRF KW - Precision KW - Précision KW - Comparison of techniques KW - Éléments traces PY - 2016 DO - https://doi.org/10.1111/j.1751-908X.2015.00362.x SN - 1639-4488 SN - 1751-908X VL - 40 IS - 2 SP - 267 EP - 289 PB - Blackwell CY - Oxford AN - OPUS4-34882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Constantinescu, B. A1 - Vasilescu, A. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Pacheco, C. A1 - Pichon, L. A1 - Oberländer-Târnoveanu, E. T1 - SR XRF and micro-PIXE studies on ancient metallurgy of thirteen Dacian gold bracelets N2 - A thorough microscopic investigation by SR XRF and micro-PIXE brings insight into the probable techniques used in the manufacture of thirteen Dacian gold bracelets, one of the most spectacular archaeological finds ever on the territory of Romania. KW - Micro-SR-XRF KW - Micro-PIXE KW - Archaeometry KW - Gold KW - Romania PY - 2012 DO - https://doi.org/10.1007/s00339-012-7306-7 SN - 0947-8396 VL - 109 IS - 2 SP - 395 EP - 402 PB - Springer CY - Berlin AN - OPUS4-26902 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilhelm, Stefan A1 - Kaiser, Martin A1 - Würth, Christian A1 - Heiland, J. A1 - Carrillo-Carrion, C. A1 - Muhr, V. A1 - Wolfbeis, Otto S. A1 - Parak, W.J. A1 - Resch-Genger, Ute A1 - Hirsch, T. T1 - Water dispersible upconverting nanoparticles: effects of surface modification on their luminescence and colloidal stability N2 - We present a systematic study on the effect of surface ligands on the luminescence properties and colloidal stability of β-NaYF4:Yb3+,Er3+ upconversion nanoparticles (UCNPs), comparing nine different surface coatings to render these UCNPs water-dispersible and bioconjugatable. A prerequisite for this study was a large-scale synthetic method that yields ~2 g per batch of monodisperse oleate-capped UCNPs providing identical core particles. These ~23 nm sized UCNPs display an upconversion quantum yield of ~0.35% when dispersed in cyclohexane and excited with a power density of 150 W cm-2, underlining their high quality. A comparison of the colloidal stability and luminescence properties of these UCNPs, subsequently surface modified with ligand exchange or encapsulation protocols, revealed that the ratio of the green (545 nm) and red (658 nm) emission bands determined at a constant excitation power density clearly depends on the surface chemistry. Modifications relying on the deposition of additional (amphiphilic) layer coatings, where the initial oleate coating is retained, show reduced non-radiative quenching by water as compared to UCNPs that are rendered water-dispersible via ligand exchange. Moreover, we could demonstrate that the brightness of the upconversion luminescence of the UCNPs is strongly affected by the type of surface modification, i.e., ligand exchange or encapsulation, yet hardly by the chemical nature of the ligand. KW - upconverting nanoparticles (UCNPs) KW - Luminescence KW - surface modification PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-324071 DO - https://doi.org/10.1039/c4nr05954a SN - 2040-3364 SN - 2040-3372 VL - 7 IS - 4 SP - 1403 EP - 1410 PB - RSC Publ. CY - Cambridge AN - OPUS4-32407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fittschen, U. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Böttger, S. A1 - Rosenberg, D. A1 - Menzel, M. A1 - Jensen, W. A1 - Busker, M. A1 - Gotlib, Z. A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Wobrauschek, P. A1 - Streli, C. ED - de Oliveira Guilherme Buzanich, Ana T1 - A setup for synchrotron-radiation-induced total reflection X-ray fluorescence and X-ray absorption near-edge structure recently commissioned at BESSY II BAMline N2 - An automatic sample changer chamber for total reflection X-ray fluorescence (TXRF) and X-ray absorption near-edge structure (XANES) analysis in TXRF geometry was successfully set up at the BAMline at BESSY II. TXRF and TXRF-XANES are valuable tools for elemental determination and speciation, especially where sample amounts are limited (<1 mg) and concentrations are low (ng ml⁻¹ to μg ml⁻¹). TXRF requires a well defined geometry regarding the reflecting surface of a sample carrier and the synchrotron beam. The newly installed chamber allows for reliable sample positioning, remote sample changing and evacuation of the fluorescence beam path. The chamber was successfully used showing accurate determination of elemental amounts in the certified reference material NISTwater 1640. Low limits of detection of less than 100 fg absolute (10 pg ml⁻¹) for Ni were found. TXRF-XANES on different Re species was applied. An unknown species of Re was found to be Re in the +7 oxidation state. KW - TXRF KW - TXRF-XANES KW - Sample changer KW - BAMline KW - Re-XANES PY - 2016 DO - https://doi.org/10.1107/S1600577516001995 SN - 1600-5775 VL - 23 IS - 3 SP - 820 EP - 824 PB - International Union of Crystallography AN - OPUS4-38656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Buzanich, Günter A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Streli, C. T1 - Micro-X-ray absorption spectroscopy with compound refractive lenses N2 - A study regarding the possibility to use compound refractive lenses (CRLs) for X-ray absorption spectroscopy (XAS) was conducted. For XAS measurements the energy of the monochromatic incident beam has to be tuned over an energy range which is broader than the energy bandwidth of a CRL. To prove that µ-XAS with compound refractive lenses is possible, it had to be investigated how changes in the energy influence the beam parameters. This was done by tuning the energy around the nominal energy of the lens and recording images with a high resolution X-ray imaging setup. To investigate the changes in the spot size the scintillator was placed at the nominal focal distance and scans along the beam axis were performed. The effect on the photon flux of the incident beam due to absorption in the lens was investigated by performing XANES measurement on different reference materials with and without CRL. The results of these measurements using a CRL designed for 9 keV are shown and discussed. KW - Micro-XAS KW - Compound refractive lens PY - 2012 DO - https://doi.org/10.1039/c2ja30130j SN - 0267-9477 SN - 1364-5544 VL - 27 IS - 10 SP - 1803 EP - 1808 PB - Royal Society of Chemistry CY - London AN - OPUS4-26790 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Menzel, M. A1 - Scharf, O. A1 - Novak, S. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Hischenhuber, P. A1 - Buzanich, Günter A1 - Meyer, A. A1 - Lopez, V. A1 - McIntosh, K. A1 - Streli, C. A1 - Havrilla, G. A1 - Fittschen, U. T1 - Shading in TXRF: calculations and experimental validation using a color X-ray camera N2 - Absorption effects in total reflection X-ray fluorescence (TXRF) analysis are important to consider, especially if external calibration is to be applied. With a color X-ray camera (CXC), that enables spatially and energy resolved XRF analysis, the absorption of the primary beam was directly visualized for mL-droplets and an array of pL-droplets printed on a Si-wafer with drop-on-demand technology. As expected, deposits that are hit by the primary beam first shade subsequent droplets, leading to a diminished XRF signal. This shading effect was quantified with enhanced precision making use of sub-pixel analysis that improves the spatial resolution of the camera. The measured absorption was compared to simulated results using three different model calculations. It was found they match very well (average deviation < 10%). Thus errors in quantification due to absorption effects can be accounted for in a more accurate manner. KW - absorption KW - X-ray Fluorescence analysis PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-359000 DO - https://doi.org/10.1039/C5JA00127G IS - 10 SP - 2184 EP - 2193 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-35900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rauwolf, M. A1 - Turyanskaya, A. A1 - Roschger, A. A1 - Prost, J. A1 - Simon, R. A1 - Scharf, O. A1 - Radtke, Martin A1 - Schoonjans, Tom A1 - de Oliveira Guilherme Buzanich, Ana A1 - Klaushofer, K. A1 - Wobrauschek, P. A1 - Hofstaetter, J. G. A1 - Roschger, P. A1 - Streli, C. T1 - Synchrotron radiation micro X-ray fluorescence spectroscopy of thin structures in bone samples: comparison of confocal and color X-ray camera setups N2 - In the quest for finding the ideal synchrotron-radiation-induced imaging method for the investigation of trace element distributions in human bone samples, experiments were performed using both a scanning confocal synchrotron radiation micro X-ray fluorescence (SR-mXRF) (FLUO beamline at ANKA) setup and a full-field color X-ray camera (BAMline at BESSY-II) setup. As zinc is a trace element of special interest in bone, the setups were optimized for its detection. The setups were compared with respect to count rate, required measurement time and spatial resolution. It was demonstrated that the ideal method depends on the element of interest. Although for Ca (a major constituent of the bone with a low energy of 3.69 keV for its K alpha XRF line) the color X-ray camera provided a higher resolution in the plane, for Zn (a trace element in bone) only the confocal SR-µXRF setup was able to sufficiently image the distribution. KW - Synchrotron KW - BAMline KW - BESSY KW - XRF KW - X-ray Color Camera PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-391944 DO - https://doi.org/10.1107/S1600577516017057 SN - 1600-5775 VL - 24 SP - 307 EP - 311 PB - International Union of Crystallography AN - OPUS4-39194 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Iro, M. A1 - Ingerle, D. A1 - Radtke, Martin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Kregsamer, P. A1 - Streli, C. T1 - Investigation of polycapillary half lenses for quantitative confocal micro-X-ray fluorescence analysis N2 - The use of polycapillary optics in confocal micro-X-ray fluorescence analysis (CMXRF) enables the destruction-free 3D investigation of the elemental composition of samples. The energy-dependent transmission properties, concerning intensity and spatial beam propagation of three polycapillary half lenses, which are vital for the quantitative interpretation of such CMXRF measurements, are investigated in a monochromatic confocal laboratory setup at the Atominstitut of TU Wien, and a synchrotron setup on the BAMline beamline at the BESSY II Synchrotron, Helmholtz-Zentrum-Berlin. The empirically established results, concerning the intensity of the transmitted beam, are compared with theoretical values calculated with the polycap software package and a newly presented analytical model for the transmission function. The resulting form of the newly modelled energy-dependent transmission function is shown to be in good agreement with Monte Carlo simulated results for the complete energy regime, as well as the empirically established results for the energy regime between 6 keV and 20 keV. An analysis of possible fabrication errors was conducted via pinhole scans showing only minor fabrication errors in two of the investigated polycapillary optics. The energy-dependent focal spot size of the primary polycapillary was investigated in the laboratory via the channel-wise evaluation of knife-edge scans. Experimental results are compared with data given by the manufacturer as well as geometric estimations for the minimal focal spot size. Again, the resulting measurement points show a trend in agreement with geometrically estimated results and manufacturer data. KW - BAMline KW - Synchrotron KW - Capillary KW - confocal PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562430 DO - https://doi.org/10.1107/S1600577522009699 SN - 1600-5775 VL - 29 SP - 1376 EP - 1384 PB - International Union of Crystallography CY - Chester AN - OPUS4-56243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grengg, C. A1 - Gluth, Gregor A1 - Mittermayr, F. A1 - Ukrainczyk, N. A1 - Bertmer, M. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Leis, A. A1 - Dietzel, M. T1 - Deterioration mechanism of alkali-activated materials in sulfuric acid and the influence of Cu: A micro-to-nano structural, elemental and stable isotopic multi-proxy study N2 - In this study, a multi-proxy approach combining 29Si, 27Al and 1H MAS-NMR, FEG-EPMA, XANES at the Cu K-edge and XRD analytics with hydrochemical tools such as ICP-OES analyses, oxygen-isotope signatures, and thermodynamic modelling was applied to K-silicate-activated metakaolin specimens - with and without CuSO4·5H2O addition - exposed to sulfuric acid at pH = 2 for 35 days. The results revealed a multistage deterioration mechanism governed by (i) acid diffusion, (ii) leaching of K-A-S-H, (iii) microstructural damage related to precipitation of expansive (K,Ca,Al)-sulfate-hydrate phases (iv) complete dissolution of the K-A-S-H framework, (v) and formation of silica gel in the outermost corroded regions. Copper ions were mainly located in layered spertiniite-chrysocolla-like phases in the as-cured materials. The results demonstrate an overall negative effect of Cu addition on chemical material durability, implying that the reported higher durability of Cu-doped AAM in biocorrosion environments can be best explained by bacteriostatic effects. KW - Alkali-activated materials KW - Acid resistance KW - Microbially induced corrosion KW - MIC PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520567 DO - https://doi.org/10.1016/j.cemconres.2021.106373 SN - 0008-8846 VL - 142 SP - 1 EP - 15 PB - Elsevier CY - Oxford AN - OPUS4-52056 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Streli, C. A1 - Radtke, Martin T1 - On the way to full-field X-ray fluorescence spectroscopy imaging with coded apertures N2 - Imaging with X-rays is a challenging field, due to the optical properties of X-rays. The fabrication of appropriate optics is usually expensive and requires an elaborate manufacturing process. One simpler and less expensive possibility of imaging high energy radiation is coded aperture imaging, a technique well established in astrophysics and also used in nuclear medicine or radiation detection, e.g., for nuclear decommissioning. Our aim is to adapt coded aperture imaging for X-ray fluorescence spectroscopy in the nearfield. In this work we show theoretical considerations and preliminary simulations of Image formation through a coded aperture and three different reconstruction methods to prepare the experiments. We used a new mask based on an inverted modified uniformly redundant array (MURA) that could be used for the construction of a decoding mask for all investigated geometrical arrangements. The most commonly used reconstruction method, convoluting the detected image with a Decoding mask, does not always deliver satisfactory results. This is more noticeable for small distances between the object, mask and detector. Hence, we developed two new reconstruction methods, one based on iterative algebraic optimization and another one based on a genetic algorithm. Both show good performance even in those cases where the convolution method fails. This provides a basis for further investigations of the ideal parameters for near field coded aperture imaging and refinements of the algorithms. We performed first measurements with a coded aperture at the BAMline at BESSY II and could successfully reconstruct a test object from the obtained recorded images. KW - X-ray fluorescence spectroscopy KW - Coded aperture KW - Imaging KW - Iterative reconstruction PY - 2020 DO - https://doi.org/10.1039/c9ja00232d VL - 35 IS - 2 SP - 347 EP - 356 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-50459 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Kulow, Anicó A1 - Kabelitz, Anke A1 - Grunewald, C. A1 - Seidel, R. A1 - Chapartegui-Arias, Ander A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Beyer, S. T1 - Observation of early ZIF-8 crystallization stages with X-ray absorption spectroscopy N2 - The present study investigates early stages of ZIF-8 crystallization up to 5 minutes post mixing of precursor solutions. Dispersive X-ray Absorption Spectroscopy (DXAS) provides a refined understanding of the evolution of the coordination environment during ZIF-8 crystallization. Linear Combination Fiting (LCF) suggests tetrakis(1-methylimidazole)zinc2+ to be a suitable and stable mononuclear structure analogue for some early stage ZIF-8 intermediates. Our results pave the way for more detailed studies on physico-chemical aspects of ZIF-8 crystallization to better control tailoring ZIF-8 materials for specific applications. KW - In-situ KW - XANES KW - ZIF-8 KW - Crystallization PY - 2020 DO - https://doi.org/10.1039/D0SM01356K SN - 1744-6848 VL - 17 IS - 2 SP - 331 EP - 334 PB - Royal Scociety of Chemistry AN - OPUS4-51723 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lutz, C. A1 - Breuckmann, M. A1 - Hampel, S. A1 - Kreyenschmidt, M. A1 - Ke, X. A1 - Beuermann, S. A1 - Schafner, K. A1 - Turek, T. A1 - Kunz, U. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Fittschen, U. E. A. T1 - Characterization of Dimeric Vanadium Uptake and Species in Nafion™ and Novel Membranes from Vanadium Redox Flow Batteries Electrolytes N2 - A core component of energy storage systems like vanadium redox flow batteries (VRFB) is the polymer electrolyte membrane (PEM). In this work, the frequently used perfluorosulfonic-acid (PFSA) membrane Nafion™ 117 and a novel poly (vinylidene difluoride) (PVDF)-based Membrane are investigated. A well-known problem in VRFBs is the vanadium permeation through the membrane. The consequence of this so-called vanadium crossover is a severe loss of capacity. For a better understanding of vanadium transport in membranes, the uptake of vanadium ions from electrolytes containing Vdimer(IV–V) and for comparison also V(II), V(III), V(IV), and V(V) by both membranes was studied. UV/VIS spectroscopy, X-ray absorption near edge structure spectroscopy (XANES), total reflection X-ray fluorescence spectroscopy (TXRF), inductively coupled plasma optical emission spectrometry (ICP-OES), and micro X-ray fluorescence spectroscopy (microXRF) were used to determine the vanadium concentrations and the species inside the membrane. The results strongly support that Vdimer(IV–V), a dimer formed from V(IV) and V(V), enters the nanoscopic water-body of Nafion™ 117 as such. This is interesting, because as of now, only the individual ions V(IV) and V(V) were considered to be transported through the membrane. Additionally, it was found that the Vdimer(IV–V) dimer partly dissociates to the individual ions in the novel PVDF-based membrane. The Vdimer(IV–V) dimer concentration in Nafion™ was determined and compared to those of the other species. After three days of equilibration time, the concentration of the dimer is the lowest compared to the monomeric vanadium species. The concentration of vanadium in terms of the relative uptake λ = n(V)/n(SO3 ) are as follows: V(II) [λ = 0.155] > V(III) [λ = 0.137] > V(IV) [λ = 0.124] > V(V) [λ = 0.053] > Vdimer(IV–V) [λ = 0.039]. The results show that the Vdimer(IV–V) dimer Needs to be considered in addition to the other monomeric species to properly describe the transport of vanadium through Nafion™ in VRFBs. KW - MicroXRF KW - VRFB KW - PVDF-based membrane KW - UV/VIS KW - XANES KW - TXRF KW - ICP-OES PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530676 DO - https://doi.org/10.3390/membranes11080576 VL - 11 IS - 8 SP - 576 PB - MDPI AN - OPUS4-53067 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Guerra, M.F. A1 - Martinón-Torres, M. A1 - Lemasson, Q. A1 - Moignard, B. A1 - Pacheco, C. A1 - Pichon, L. A1 - Macdonald, L. A1 - Hess, M. A1 - Tissot, I. ED - Guerra, M. F. ED - Martinón-Torres, M. ED - Quirke, S. T1 - Analytical approaches to Egyptian goldwork N2 - The structure and composition of ancient gold objects retain information about their long history of manufacture, from the exploitation of the ore to the finishing touches, as well as evidence of their use, deposition, and degradation. By developing an efficient analytical strategy, it is possible to retrieve that information. This chapter sets the necessary foundation 131to explore fully the analytical results presented in the following chapters of this volume. The techniques employed in the analyses of the Egyptian jewellery are described and the analytical parameters provided. For more established techniques, only brief introductions are presented, while more recent developments are presented in greater detail. KW - Gold KW - Synchrotron KW - D2XRF KW - Egypt PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586039 DO - https://doi.org/10.17863/CAM.99681 SP - 131 EP - 191 AN - OPUS4-58603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - C. Pardo Pérez, L. A1 - Arndt, A. A1 - Stojkovikj, S. A1 - Y. Ahmet, I. A1 - T. Arens,, J. A1 - Dattila, F. A1 - Wendt, R. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Davies, V. A1 - Höflich, K. A1 - Köhnen, E. A1 - Tockhorn, P. A1 - Golnak, R. A1 - Xiao, J. A1 - Schuck, G. A1 - Wollgarten, M. A1 - López, N. A1 - T. Mayer, M. T1 - Determining Structure-Activity Relationships in Oxide Derived CuSn Catalysts During CO2 Electroreduction Using X-Ray Spectroscopy N2 - The development of earth-abundant catalysts for selective electrochemical CO2 conversion is a central challenge. Cu-Sn bimetallic catalysts can yield selective CO2 reduction toward either CO or formate. This study presents oxide-derived Cu-Sn catalysts tunable for either product and seeks to understand the synergetic effects between Cu and Sn causing these selectivity trends. The materials undergo significant transformations under CO2 reduction conditions, and their dynamic bulk and surface structures are revealed by correlating observations from multiple methods—X-ray absorption spectroscopy for in situ study, and quasi in situ X-ray photoelectron spectroscopy for surface sensitivity. For both types of catalysts, Cu transforms to metallic Cu0 under reaction conditions. However, the Sn speciation and content differ significantly between the catalyst types: the CO-selective catalysts exhibit a surface Sn content of 13 at. % predominantly present as oxidized Sn, while the formate-selective catalysts display an Sn content of ≈70 at. % consisting of both metallic Sn0 and Sn oxide species. Density functional theory simulations suggest that Snδ+ sites weaken CO adsorption, thereby enhancing CO selectivity, while Sn0 sites hinder H adsorption and promote formate production. This study reveals the complex dependence of catalyst structure, composition, and speciation with electrochemical bias in bimetallic Cu catalysts. KW - Electrochemical CO2 conversion KW - Cu catalysts KW - X-ray absorption spectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547116 DO - https://doi.org/10.1002/aenm.202103328 SN - 1614-6832 VL - 12 IS - 5 SP - 2103328 PB - Wiley-VCH GmbH AN - OPUS4-54711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steglich, P. A1 - Bondarenko, S. A1 - Mai, C. A1 - Paul, Martin A1 - Weller, Michael G. A1 - Mai, A. T1 - CMOS-Compatible Silicon Photonic Sensor for Refractive Index Sensing Using Local Back-Side Release N2 - Silicon photonic sensors are promising candidates for lab-on-a-chip solutions with versatile applications and scalable production prospects using complementary metal-oxide semiconductor (CMOS) fabrication methods. However, the widespread use has been hindered because the sensing area adjoins optical and electrical components making packaging and sensor handling challenging. In this work, a local back-side release of the photonic sensor is employed, enabling a separation of the sensing area from the rest of the chip. This approach allows preserving the compatibility of photonic integrated circuits in the front-end of line and metal interconnects in the back-end of line. The sensor is based on a micro-ring resonator and is fabricated on wafer-level using a CMOS technology. We revealed a ring resonator sensitivity for homogeneous sensing of 106 nm/RIU. KW - Photonic biosensor KW - Lab-on-a-chip KW - Ring resonator KW - Resonance wavelength shift KW - PIC technology KW - Back-side integration PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517139 DO - https://doi.org/10.1109/LPT.2020.3019114 VL - 32 IS - 19 SP - 1241 EP - 1244 PB - IEEE AN - OPUS4-51713 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steglich, Patrick A1 - Paul, Martin A1 - Mai, C. A1 - Böhme, A. A1 - Bondarenko, S. A1 - Weller, Michael G. A1 - Mai, A. T1 - A monolithically integrated microfluidic channel in a silicon-based photonic-integrated-circuit technology for biochemical sensing N2 - In this work, a cost-effective optofluidic system is proposed and preliminary experimental results are presented. A microfluidic channel monolithically integrated into a photonic integrated circuit technology is used in conjunction with a cyclic olefin copolymer (COC) substrate to provide fluidic in- and output ports. We report on initial experimental results as well as on the simple and cost-effective fabrication of this optofluidic system by means of micro-milling. KW - Biosensors KW - Biophotonics KW - Optical sensors KW - Photonic sensors KW - Ring resonators KW - Silicon photonics KW - Lab-on-a-chip KW - Microfluidics KW - Chip KW - Biochip PY - 2021 DO - https://doi.org/10.1117/12.2588791 VL - 11772 SP - 1 EP - 5 PB - SPIE AN - OPUS4-53559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steglich, P. A1 - Mai, C. A1 - Bondarenko, S. A1 - Paul, Martin A1 - Weller, Michael G. A1 - Schrader, S. A1 - Mai, A. T1 - BioPIC - Integration of Biosensors based on Photonic Integrated Circuits by Local-Backside Etching N2 - Silicon photonic sensors are promising candidates for lab-on-a-chip solutions with versatile applications and scalable production prospects using complementary metal-oxide semiconductor (CMOS) fabrication methods. However, the widespread use has been hindered because the sensing area adjoins optical and electrical components making packaging and sensor handling challenging. In this work, a local back-side release of the photonic sensor is employed, enabling a separation of the sensing area from the rest of the chip. This approach allows preserving the compatibility of photonic integrated circuits in the front-end of line and metal interconnects in the back-end of line. T2 - ATTRACT online Conference CY - Online meeting DA - 22.09.2020 KW - Silicon Photonics KW - Photonic Sensor KW - Photonic Integrated Circuits KW - Point-Of-Care-Diagnostics KW - CMOS KW - Microfluidics KW - Lab-on-a-chip KW - Ring resonator PY - 2020 UR - https://attract-eu.com/showroom/project/integration-of-biosensors-based-on-photonic-integrated-circuits-by-local-backside-etching-biopic/ SP - 1 EP - 5 AN - OPUS4-51735 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fünning, Tabea A1 - Peczek, Anna A1 - Kroh, Aleksandra A1 - Mai, Christian A1 - Paul, Martin A1 - Thomsen, Florian A1 - Tannenberg, Robert A1 - Schumann, Christoph A1 - Weller, Michael G. A1 - Mai, Andreas A1 - Steglich, Patrick C. ED - Lieberman, Robert A. ED - Baldini, Francesco ED - Homola, Jiri T1 - Optimization of local backside released micro-ring resonators for sensing applications using silicon photonic integrated circuits in a SOI technology N2 - Photonic micro-ring resonators (MRR) are widely studied for their high sensitivity across applications like environmental monitoring, healthcare, and chemical analysis. Their evanescent field sensing requires partially unembedded waveguides compatible with CMOS processing. Our approach uses local backside etching with an additional buried oxide (BOX) etch to release waveguides while preserving the back-end of line (BEOL) structure, enabling spatial separation of the sensing area and electronics. The BOX etch critically affects sensor performance, as waveguide surface roughness can alter MRR properties and coupling. We analyzed MRR design variations, comparing wet and dry etching techniques for their effects on optical performance across rib and strip waveguides in quasi-TE and quasi-TM modes. Wafer-level measurements show that backside-released MRR achieve high extinction ratios with slightly reduced quality factors, advancing high-sensitivity photonic sensors. T2 - SPIE Optics + Optoelectronics 2025 CY - Prague, Czech Republic DA - 23.05.2025 KW - Photonic sensors KW - Micro-ring resonator (MRR) KW - Silicon on insulator (SOI) KW - CMOS KW - Local backside etching PY - 2025 SN - 978-1-5106-8851-3 DO - https://doi.org/10.1117/12.3056481 VL - 13527 SP - 1 EP - 8 PB - SPIE CY - Bellingham, WA , USA AN - OPUS4-63585 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Hampel, S. A1 - Fittschen, U.E.A. A1 - Streli, C. A1 - Radtke, Martin T1 - Comparison of three reconstruction methods based on deconvolution, iterative algorithm and neural network for X-ray fluorescence imaging with coded apertures N2 - X-ray imaging methods are used in many fields of research, as they allow a non-destructive Investigation of the elemental content of various samples. As for every imaging method, for X-ray imaging the optics are of crucial importance. However, these optics can be very expensive and laborious to build, as the requirements on surface roughness and precision are extremely high. Angles of reflection and refraction are often in the range of a few mrad, making a compact design hard to achieve. In this work we present a possibility to simplify X-ray imaging. We have adapted the coded aperture method, a high energy radiation imaging method that has its origins in astrophysics, to full field X-ray fluorescence imaging. In coded aperture imaging, an object is projected through a known mask, the coded aperture, onto an area sensitive detector. The resulting image consists of overlapping projections of the object and a reconstruction step is necessary to obtain the information from the recorded image. We recorded fluorescence images of different samples with an energy-dispersive 2D detector (pnCCD) and investigated different reconstruction methods. With a small coded aperture with 12 holes we could significantly increase the count rate compared to measurements with a straight polycapillary optic. We show that the reconstruction of two different samples is possible with a deconvolution approach, an iterative algorithm and a neural network. These results demonstrate that X-ray fluorescence imaging with coded apertures has the potential to deliver good results without scanning and with an improved count rate, so that measurement times can be shortened compared to established methods. KW - X-ray fluorescence imaging KW - Coded apertures KW - Imaging KW - Elemental mapping KW - Image reconstruction PY - 2020 DO - https://doi.org/10.1039/d0ja00146e VL - 35 IS - 7 SP - 1423 EP - 1434 PB - Royal Society of Chemistry CY - United Kingdom AN - OPUS4-51518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Hampel, S. A1 - Fittschen, UEA A1 - Streli, C. A1 - Radtke, Martin T1 - Reconstruction for coded aperture full-field x-ray fluorescence imaging N2 - X-ray fluorescence imaging is a well-established tool in materials characterization. In this work, we present the adaption of coded aperture imaging to full-field X-ray fluorescence imaging at the synchrotron. Coded aperture imaging has its origins in astrophysics, and has several advantages: Coded apertures are relatively easy to fabricate, achromatic, allow a high photon throughput, and high angular acceptance. Coded aperture imaging is a two-step-process, consisting of the measurement process and a reconstruction step. Different programs have been written, for the raytracing/forward projection and the reconstruction. Experiments with coded aperture in combination with a Color X-ray Camera and an energy-dispersive area detector, have been conducted at the BAMline. Measured samples were successfully reconstructed, and gave a 9.1-fold increase in count rate compared to a polycapillary optic. KW - Synchrotron KW - BAMline KW - Coded Aperture PY - 2022 SN - 1097-0002 VL - 65 SP - 57 EP - 70 PB - Cambridge University Press CY - Cambridge AN - OPUS4-56350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cakir, Cafer Tufan A1 - Piotrowiak, T. A1 - Reinholz, Uwe A1 - Ludwig, A. A1 - Emmerling, Franziska A1 - Streli, C. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin T1 - Exploring the Depths of Corrosion: A Novel GE-XANES Technique for Investigating Compositionally Complex Alloys N2 - In this study, we propose the use of nondestructive, depth-resolved, element-specific characterization using grazing exit X-ray absorption near-edge structure spectroscopy (GE-XANES) to investigate the corrosion process in compositionally complex alloys (CCAs). By combining grazing exit X-ray fluorescence spectroscopy (GE-XRF) geometry and a pnCCD detector, we provide a scanning-free, nondestructive, depth-resolved analysis in a sub-micrometer depth range, which is especially relevant for layered materials, such as corroded CCAs. Our setup allows for spatial and energy-resolved measurements and directly extracts the desired fluorescence line, free from scattering events and other overlapping lines. We demonstrate the potential of our approach on a compositionally complex CrCoNi alloy and a layered reference sample with known composition and specific layer thickness. Our findings indicate that this new GE-XANES approach has exciting opportunities for studying surface catalysis and corrosion processes in real-world materials. KW - Degradation mechanisms KW - Grazin exit XANES KW - Depth resolved XANES KW - Compositional complex alloys KW - Corrosion PY - 2023 DO - https://doi.org/10.1021/acs.analchem.3c00404 VL - 95 SP - 4810 EP - 4818 PB - ACS Publications AN - OPUS4-57823 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vigna, L. A1 - Gottschalk, Martin A1 - Cacocciola, N. A1 - Verna, A. A1 - Marasso, S. L. A1 - Seeger, Stefan A1 - Pirri, C.F. A1 - Cocuzza, M. T1 - Flexible and reusable parylene C mask technology for applications in cascade impactor air quality monitoring systems N2 - The development of traceable new methodologies to quantify elemental air pollutants in particulate matter (PM) supports modernization of methods used in air quality monitoring networks in Europe. In the framework of the EURAMET EMPIR AEROMET II project, the combination of cascade impactor aerosol sampling and total reflection X-ray fluorescence elemental spectroscopy (TXRF) was investigated. This technique requires a traceable calibration based on reference samples. This paper describes a new, simple and effective method to produce such reference samples using flexible, reusable, and low-cost parylene C shadow masks, fabricated by photolithographic steps. These shadow masks can be used to produce reference samples that mimic the Dekati cascade impactor’s deposition patterns by applying as-prepared micro stencils to 30 mm acrylic substrates and evaporating a reference material (Ti) in arrangements of thin circular dots. The highly flexible direct patterning of acrylic discs with reference material, otherwise impossible with conventional photolithography, allows multiple reusing of the same micro stencils. The aspect ratios of the dots could be repeated with an error less than 4 %. A first set of standard reference samples for the 13 stages of the Dekati cascade impactor was produced and preliminary TXRF measurements of the deposited Ti masses were performed. The centricity of the deposition patterns turned out to be an important parameter for the quality of the TXRF results. The parylene mask technology for the production of reference samples turns out to be a promising new approach for the traceable calibration of TXRF spectrometers for the quantification of element concentrations in environmental aerosol samples but, due to its great versatility, it could be used for several other micropatterning applications on conventional and unconventional substrates. KW - AEROMET II KW - Aerosol KW - Parylene C KW - Reference samples KW - Flexible shadow masks KW - Cascade impactor KW - Air quality monitoring KW - Micropatterning KW - Mask fabrication KW - Elemental aerosol analysis KW - TXRF PY - 2022 DO - https://doi.org/10.1016/j.mne.2022.100108 SN - 2590-0072 VL - 14 SP - 1 EP - 19 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-54252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schischke, Karsten A1 - Rückschloss, Jana A1 - Schlegel, Moritz-C. A1 - Zöllinger, Jonathan A1 - Nissen, Nils F. A1 - Schneider-Ramelow, Martin T1 - The European Union’s Energy Label for Smartphones: Does it guide consumers to make environmentally sustainable choices? N2 - The European Commission adopted an EU Energy Label for smartphones and tablets in June 2023. For the first time, the EU Energy Label will depict, among energy efficiency, also a reparability score, battery endurance, battery lifetime, drop resistance and dust and water ingress protection. However, does the multitude of parameters bear the risk to confuse consumers instead of triggering environmentally sustainable purchase decisions? In a survey in Germany, consumers were asked to make a choice when the label does not clearly identify the environmentally better product. Instead, energy efficiency has to be valued against reparability, reliability against energy efficiency, and reparability against reliability. The sustainability lever of the different aspects is not the same, as e.g. lifetime extension has a much more positive environmental impact than energy efficiency in case of mobile devices. Therefore, the question remains, whether consumers intuitively make the right choice. Results of the survey indicate that consumers interpret the complex label in the desired manner and value those aspects higher, which indeed have a more positive effect on the environment. T2 - 13th International Conference on Consumer Electronics CY - Berlin, Germany DA - 03.09.2023 KW - Energy efficiency KW - EU Energy Labelling KW - Reparability KW - Reliability KW - ESPR PY - 2023 UR - https://ieeexplore.ieee.org/document/10375619 DO - https://doi.org/10.1109/ICCE-Berlin58801.2023.10375619 SP - 1 EP - 6 PB - IEEE AN - OPUS4-59318 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kim, Y.S. A1 - Li, Y.-C. A1 - Pitts, W.M. A1 - Werrel, Martin A1 - Davis, R.D. T1 - Rapid growing clay coatings to reduce the fire threat of furniture N2 - Layer-by-layer (LbL) assembly coatings reduce the flammability of textiles and polyurethane foam but require extensive repetitive processing steps to produce the desired coating thickness and nanoparticle fire retardant content that translates into a fire retardant coating. Reported here is a new hybrid bi-layer (BL) approach to fabricate fire retardant coatings on polyurethane foam. Utilizing hydrogen bonding and electrostatic attraction along with the pH adjustment, a fast growing coating with significant fire retardant clay content was achieved. This hybrid BL coating exhibits significant fire performance improvement in both bench scale and real scale tests. Cone calorimetry bench scale tests show a 42% and 71% reduction in peak and average heat release rates, respectively. Real scale furniture mockups constructed using the hybrid LbL coating reduced the peak and average heat release rates by 53% and 63%, respectively. This is the first time that the fire safety in a real scale test has been reported for any LbL technology. This hybrid LbL coating is the fastest approach to develop an effective fire retardant coating for polyurethane foam. KW - Layer-by-layer assembly KW - Polyurethane foam KW - Sodium montmorillonite KW - Flame retardant KW - Real scale mockup PY - 2014 DO - https://doi.org/10.1021/am405259n SN - 1944-8244 SN - 0013-936X SN - 1944-8252 VL - 6 IS - 3 SP - 2146 EP - 2152 PB - ACS Publ. CY - Washington, DC, USA AN - OPUS4-31489 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Everard, C.D. A1 - Schmidt, Martin A1 - McDonnell, K.P. A1 - Finnan, J. T1 - Heating processes during storage of Miscanthus chip piles and numerical simulations to predict self-ignition N2 - Miscanthus x Giganteus (Miscanthus) energy crop was examined at laboratory scale to assess its self-heating and self-ignition risks during storage. Chipped Miscanthus (18 mm) from February and March harvests, in 2012, were assessed as well as ground Miscanthus (3 mm) from the March harvest. February and March crops had moisture contents of 41.6 and 20.2%, respectively. Self-ignition temperatures were independent of moisture although moisture did affect the time from the beginning of storage until storage temperature was reached. Ground Miscanthus had lower self-ignition temperatures than chipped Miscanthus. Isothermal respirometric tests carried out showed increase risk of self-heating in the February crop compared to the March crop due to increased microbial activity. Numerical simulations were used to determine critical enhanced start temperatures, e.g. caused by microbial decomposition, of the stored Miscanthus. Safe storage conditions have been derived from the investigations. The numerical simulations demonstrated that self-ignition was possible in Miscanthus chip piles with a height greater than 6 m if there was significant heat release from microbiological activity. Reliable assessment of self-heating and self-ignition risks in large scale Miscanthus energy crop clamps or piles are required to prevent losses due to decomposition and fire damage. KW - Miscanthus x Giganteus KW - Hot storage test KW - Respirometric rates KW - Self-heating KW - Self-ignition KW - Numerical simulations KW - Biomass storage PY - 2014 DO - https://doi.org/10.1016/j.jlp.2014.06.003 SN - 0950-4230 SN - 1873-3352 VL - 30 SP - 188 EP - 196 PB - Butterworth CY - Guildford, Surrey AN - OPUS4-31149 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Seewald, J.S. A1 - Reeves, E.P. A1 - Bach, W. A1 - Saccocia, P.J. A1 - Craddock, P.R. A1 - Shanks III, W.C. A1 - Sylva, S.P. A1 - Pichler, T. A1 - Rosner, Martin A1 - Walsh, E. T1 - Submarine venting of magmatic volatiles in the Eastern Manus Basin, Papua New Guinea N2 - The SuSu Knolls and DESMOS hydrothermal fields are located in the back-arc extensional transform zone of the Eastern Manus Basin. In 2006, highly acidic and ΣSO4-rich vent fluids were collected at both sites and analyzed for the chemical and isotopic composition of major and trace species. Fluids exiting the seafloor have measured temperatures from 48 to 215 °C and are milky white in appearance due to precipitation of elemental S0. Vent fluid concentrations of Na, K, and Mg are depleted by as much as 30% relative to seawater, but have the same relative abundance. In contrast, the fluids are highly enriched in dissolved ΣCO2, Cl, SiO2(aq), Fe, and Al relative to seawater. Measured pH (25 °C) ranged from 0.95 to 1.87 and aqueous ΣSO4 ranged from 35 to 135 mmol/kg. The chemical and isotopic composition points to formation via subsurface mixing of seawater with a Na-, K-, Mg-, and Ca-free, volatile-rich magmatic fluid exsolved from subsurface magma bodies during a process analogous to subaerial fumarole discharge. Estimates of the magmatic end-member composition indicate a fluid phase where H2O > SO2 > CO2 ≈ Cl > F. The hydrogen and oxygen isotopic composition of H2O and carbon isotopic composition of ΣCO2 in the vent fluids strongly suggest a contribution of slab-derived H2O and CO2 to melts generated in the mantle beneath the Eastern Manus volcanic zone. Abundant magmatically-derived SO2 undergoes disproportionation during cooling in upflow zones and contributes abundant acidity, SO42-, and S0 to the venting fluids. Interaction of these highly acidic fluids with highly altered mineral assemblages in the upflow zone are responsible for extensive aqueous mobilization of SiO2(aq), Fe, and Al. Temporal variability in the speciation and abundance of aqueous S species between 1995 and 2006 at the DESMOS vent field suggests an increase in the relative abundance of SO2 in the magmatic end-member that has mixed with seawater in the subsurface. Results of this study constrain processes responsible for the formation of hot-spring fluids in magmatically active back-arc environments and the resulting chemical exchange between the lithosphere and water column. PY - 2015 DO - https://doi.org/10.1016/j.gca.2015.04.023 SN - 0016-7037 SN - 1872-9533 VL - 163 SP - 178 EP - 199 PB - Elsevier Science CY - New York, NY AN - OPUS4-33433 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -