TY - CONF A1 - Radtke, Martin T1 - X-ray camera with high energy and spital resolution: Sterography with a colour X-ray camera T2 - European Conference on X-ray Spectrometry CY - Figueira da Foz, Portugal DA - 2010-06-20 PY - 2010 AN - OPUS4-21205 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Von Ägypten bis Hiddensee – Analyse von Gold mit Synchrotronstrahlung - Update 2018 N2 - Gold ist eines der sieben schon im Altertum bekannten Metalle und wurde wg. seines Glanzes und seiner Seltenheit von alters her als Tauschmittel und zur Herstellung von Schmuck benutzt. Außerdem ist es einfach bearbeitbar und weitestgehend gegen chemische Einflüsse resistent. Die Untersuchungen von Gold mit synchrotronstrahlungsangeregter Röntgenfluoreszenzanalyse sind zerstörungsfrei und geben Auskunft über die in der untersuchten Probe vorhandenen chemischen Elemente. Bei den hier vorgestellten Untersuchungen an der BAMline stehen Fragestellungen wie Herkunft, Herstellungsverfahren und Zusammengehörigkeit von Goldfunden im Vordergrund. Die verschiedenen Fragestellungen werden an einer Reihe von Beispielen erläutert die vom Wikingerschatz aus Hiddensee über die Himmelsscheibe von Nebra bis hin zu Funden aus Ägypten langen. Zusätzlich werden die modernen Messmethoden vorgestellt, die am Synchrotron heutzutage zur Verfügung stehen. T2 - Vorlesung FU Berlin Einführung in die Archäometrie CY - Berlin, Germany DA - 01.11.2018 KW - Gold KW - Synchrotron KW - XRF KW - BAMline PY - 2018 AN - OPUS4-46451 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Tragbare RFA an Gläsern: Ergebnisse und Grenzen N2 - Vorstellung der Ergebnisse der Messungen an Gläsern von Goethes Prismen. T2 - 3. Goethe/Ritter-Workshop CY - Berlin, Germany DA - 25.05.2018 KW - Goethe KW - Farbenlehre KW - Prisma KW - Handheld KW - XRF PY - 2018 AN - OPUS4-46369 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Röntgenfluoreszenzanalyse mit Synchrotronstrahlung an der Bundesanstalt für Materialforschung und -prüfung (BAM), Berlin T2 - Seminar: "Strahlenphysikalische Anwendungen in Technik und Medizin" CY - Wien, Österreich DA - 2015-01-14 PY - 2015 AN - OPUS4-34014 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Experiences with the Color X-Ray Camera at the BAMline T2 - X-ray Spectroscopy Detectors for Present and Future Synchrotron Storage rings: Opportunities for Horizon 2020 CY - Paris, Frankreich DA - 2015-03-16 PY - 2015 AN - OPUS4-34009 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Double Dispersive X-ray Fluorescence T2 - EXRS 2014 CY - Bologna (Italien) DA - 2014-06-15 PY - 2014 AN - OPUS4-32370 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Imaging with the Color X-ray Camera - Basics and Examples T2 - HZB Industry Workshop CY - Berlin DA - 2015-02-19 PY - 2015 AN - OPUS4-34023 LA - deu 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 - Rodrigues, M. A1 - Schreiner, M. A1 - Melcher, M. A1 - Guerra, M. A1 - Salomon, J. A1 - Radtke, Martin A1 - Alram, M. A1 - Schindel, N. T1 - Analysis of the hoard of Becin using X-ray-based techniques N2 - Four hundred and sixteen silver coins stemming from the Ottoman Empire (16th and 17th centuries) were analyzed to confirm the fineness of the coinage as well as to study the provenance of the alloy used for the coins. As most of the coins showed the typical green patina on their surfaces due to corrosion processes that have led to the depletion of copper in the near surface domains of the silver coins in comparison to their core composition, small samples had to be taken, embedded in synthetic resin, and cross sectioned to investigate the true-heart metal composition. µ-synchrotron micro X-ray fluorescence analysis and µ-proton-induced X-ray emission were applied to determine the silver contents as well as the minor and trace elements. The type of the alloy was investigated as well as if coins minted in different locations demonstrated homogeneous traits concerning the predominant impurities (Au and Bi), which could suggest a common ore. Finally, energy-dispersive microanalysis in a scanning electron microscope was applied to study the homogeneity/heterogeneity of the coins and the presence of surface enrichments and to explain differences between the µ-synchrotron micro X-ray fluorescence analysis and µ-proton-induced X-ray emission measurements concerning the main component. In general, the silver content of the analyzed specimen varies between 90 and 95%. These outcomes have not supported the historical interpretations, which predict that during the period studied, a debasement of approximately 44% of the silver content of the coins should have occurred. KW - SRXRF KW - Silber KW - BAMline PY - 2012 DO - https://doi.org/10.1002/xrs.2415 SN - 0049-8246 VL - 41 IS - 6 SP - 416 EP - 424 PB - Wiley CY - Chichester AN - OPUS4-27723 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 - Kühn, Andreas A1 - Scharf, Oliver A1 - Ordavo, I. A1 - Riesemeier, Heinrich A1 - Reinholz, Uwe A1 - Radtke, Martin A1 - Berger, Achim A1 - Ostermann, Markus A1 - Panne, Ulrich T1 - Pushing the limits for fast spatially resolved elemental distribution patterns N2 - A new setup for fast spatially resolved measurements of elemental trace amounts under total reflection conditions using a new colour X-ray camera is described. Samples prepared on conventional total reflection X-ray fluorescence (TXRF) reflectors were measured at BESSY II synchrotron. A spatial resolution of 50 × 50 µm² was obtained, while the required time for the investigation of a 10 × 10 mm² sample is 30 seconds. The set-up is up to 350 times faster than conventional X-ray fluorescence systems for elemental traces. The major components of the X-ray camera are polycapillary optics and a pn-CCD chip with an active area of 13 × 13 mm². This area is divided into 264 × 264 pixels of 48 × 48 µm². A full X-ray spectrum with a resolution of 152 eV @ 5.9 keV and a chip temperature of 246 K is recorded for each pixel. The chip has a read-out rate of 400 Hz. PY - 2011 DO - https://doi.org/10.1039/c1ja10069f SN - 0267-9477 SN - 1364-5544 VL - 26 SP - 1986 EP - 1989 PB - Royal Society of Chemistry CY - London AN - OPUS4-24386 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 - CONF A1 - Radtke, Martin T1 - Shading Effects in SR-TXRF: Calcullations and Experimental Visualization using a Color X-ray Camera T2 - Denver X-ray Conference CY - BIG SKY RESORT, BIG SKY, MONTANA, USA DA - 2014-07-28 PY - 2014 AN - OPUS4-32386 LA - deu 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 - GEN A1 - Hahn, Oliver A1 - Denker, A. A1 - Merchel, S. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Wolff, T. ED - Armbruster, B. ED - Eilbracht, H. ED - Hahn, Oliver ED - Heinrich-Tamaska, O. T1 - Zerstörungsfreie Analyse von Metallartefakten - Eine Fallstudie N2 - Die naturwissenschaftliche Analyse historischer Materialen ermöglicht die Beantwortung kulturhistorischer Fragestellungen, die mit kunsthistorischen oder archäologischen Ansätzen allein nicht zu leisten sind. In dieser Studie wurden sechs römische Münzen mit unterschiedlich stark ausgeprägten Korrosionsschichten an unbehandelten und polierten Stellen mit vier zerstörungsfreien analytischen Methoden untersucht: Hoch- und Niederenergie Protonen Induzierter Röntgenemission (HE-/PIXE), Synchrotronstrahlungsinduzierte-Röntgenfluoreszenzanalyse (SY-RFA) und Mikro-Röntgenfluoreszenzanalyse (Mikro-RFA) mit einem mobilen Gerät. Aufgrund von Unterschieden in den Messbedingungen und dem Einfluss der Patina-Schichten auf diese ergaben sich nur für wenige Elemente Übereinstimmungen in den quantitativen Daten. Zur Validierung zukünftiger Messkampagnen mit verschiedenen Methoden sind daher Vergleichstudien unerlässlich. N2 - Investigations of physical properties and chemical composition of ancient materials generate important data for answering culture-historical questions that cannot be solved by art historical and archaeological methods alone. This contribution reports on the analysis of six Roman coins, with different degrees of corrosion layers in parts that were not handled or polished, using four non-destructive methods: low-energy particle-induced X-ray emission (PIXE, 2 MeV), high-energy PIXE (68 MeV), μ-X-ray fluorescence (XRF) spectrometry with a portable device and synchrotron-radiation induced XRF. Because of differences in the conditions needed for measurement and the influence of the layers of patina on these measurements, there were few elements where the quantitative data were in agreement. Thus comparative analyses are essential to validate future measurement projects using different methods. KW - Zerstörungsfreie Prüfung KW - Protoneninduzierte Röntgenemission KW - Röntgenfluoreszenzanalyse KW - Non-destructive testing KW - Particle-induced X-ray emission KW - X-ray fluorescence analysis PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-385702 SN - 978-3-9816751-5-3 VL - Berlin studies of the ancient world, Band 35 SP - 117 EP - 137 PB - Edition Topoi CY - Berlin AN - OPUS4-38570 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nowak, S.H. A1 - Bjeoumikhov, A. A1 - Von Borany, J. A1 - Buchriegler, J. A1 - Munnik, F. A1 - Petric, M. A1 - Radtke, Martin A1 - Renno, A.D. A1 - Reinholz, Uwe A1 - Scharf, O. A1 - Wedell, R. T1 - Sub-pixel resolution with a color X-ray camera N2 - The color X-ray camera SLcam® is a full-field, single photon detector providing scanning-free, energy and spatially resolved X-ray imaging. Spatial resolution is achieved with the use of polycapillary optics guiding X-ray photons from small regions on a sample to distinct energy dispersive pixels on a charged-coupled device detector. Applying sub-pixel resolution, signals from individual capillary channels can be distinguished. Therefore, the SLcam® spatial resolution, which is normally limited to the pixel size of the charge-coupled device, can be improved to the size of individual polycapillary channels. In this work a new approach to a sub-pixel resolution algorithm comprising photon events also from the pixel centers is proposed. The details of the employed numerical method and several sub-pixel resolution examples are presented and discussed. KW - Color X-ray camera KW - Sub pixel analysis PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-334948 DO - https://doi.org/10.1039/c5ja00028a SN - 0267-9477 SN - 1364-5544 SP - 1890 EP - 1897 PB - Royal Society of Chemistry CY - London AN - OPUS4-33494 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hachmöller, O. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Aichler, M. A1 - Radtke, Martin A1 - Dietrich, D. A1 - Schwamborn, K. A1 - Lutz, L. A1 - Werner, M. A1 - Sperling, M. A1 - Walch, A. A1 - Karst, U. T1 - Elemental bioimaging and speciation analysis for the investigation of Wilsons disease using μXRF and XANES N2 - A liver biopsy specimen from a Wilson’s disease (WD) patient was analyzed by means of micro-X-ray fluorescence (mXRF) spectroscopy to determine the elemental distribution. First, bench-top mXRF was utilized for a coarse scan of the sample under laboratory conditions. The resulting distribution maps of copper and iron enabled the determination of a region of interest (ROI) for further analysis. In order to obtain more detailed elemental information, this ROI was analyzed by synchrotron radiation (SR)-based mXRF with a beam size of 4 mm offering a resolution at the cellular level. Distribution maps of additional elements to copper and iron like zinc and manganese were obtained due to a higher sensitivity of SR-mXRF. In addition to this, X-ray absorption near edge structure spectroscopy (XANES) was performed to identify the oxidation states of copper in WD. This speciation analysis indicated a mixture of copper(I) and copper(II) within the WD liver tissue. KW - progressive hepatolenticular degeneration KW - mXRF Micro-X-ray fluorescence spectroscopy KW - XANES X-ray absorption near edge structure spectroscopy PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-360811 DO - https://doi.org/10.1039/C6MT00001K SN - 1756-5901 SN - 1756-591X PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-36081 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Ecker, K. H. A1 - Wätjen, U. A1 - Berger, Achim A1 - Grötzschel, R. A1 - Persson, L. A1 - Pritzkow, W. A1 - Radtke, Martin A1 - Riebe, Gundel A1 - Riesemeier, Heinrich A1 - Vogl, Jochen T1 - Certification of antimony implanted in silicon wafer with a silicon dioxide diffusion barrier - IRMM-302 and BAM-L001 N2 - This Report describes the certification of the reference material antimony implanted in Si/SiO2 intended to be used for calibration of surface and near surface analytical methods. It describes the preparation, homogeneity measurements and the analytical work performed for the certification of both Areal density of antimony Atoms (retained dose) and the isotope amount Ratio as well as giving considerations on the stability of the material. KW - Isotope ratio KW - Areal density KW - Surface analysis PY - 2002 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355752 SP - 1 EP - 40 PB - Institute for Reference Materials and Measurements CY - Geel, Belgium AN - OPUS4-35575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guerra, M. F. A1 - Fischer, M. A1 - Radtke, Martin A1 - Reinholz, Uwe T1 - Inca figurines from the Ethnologisches Museum in Berlin: an analytical study of some typical and atypical productions N2 - Fourteen hollow and one cast anthropomorphic and zoomorphic figurines produced in Incan times for ritual offerings from the Ethnologisches Museum in Berlin were selected to investigate the technologies and alloys used for their fabrication with portable optical microscopy and non-destructive XRF elemental analysis. This group of gold and silver figurines includes typical specimens of the Inca production, such as the four silver figurines from the Island Coati in Lake Titicaca and the two gold figurines from Pachacamac, as well as specimens that are seldom present in collections, which makes them atypical. In addition to the tall figurines with atypical hair or standing pose, one bicolour figurine half silver, half gold) and another with coloured inlays were included in this study for comparison. The large majority of the silver specimens are made from very high quality alloys and the gold figurines are made from alloys containing low copper contents and silver ranging from 30wt% to 52wt%. KW - Gold KW - pXRF KW - Inca PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-436015 DO - https://doi.org/10.4000/bifea.8232 SN - 0303-7495 VL - 46 IS - 1 SP - 221 EP - 251 PB - Institut Français d'Études Andines AN - OPUS4-43601 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 - de O. Primo, J. A1 - Horsth, D.F. A1 - de S. Correa, J. A1 - Das, A. A1 - Bittencourt, C. A1 - Umek, P. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Yusenko, Kirill A1 - Zanetta, C. A1 - Anaissi, F.J. T1 - Synthesis and Characterization of Ag/ZnO Nanoparticles for Bacteria Disinfection in Water N2 - n this study, two green synthesis routes were used for the synthesis of Ag/ZnO nanoparticles, using cassava starch as a simple and low-cost effective fuel and Aloe vera as a reducing and stabilizing agent. The Ag/ZnO nanoparticles were characterized and used for bacterial dis- infection of lake water contaminated with Escherichia coli (E. coli). Characterization indicated the formation of a face-centered cubic structure of metallic silver nanoparticles with no insertion of Ag into the ZnO hexagonal wurtzite structure. Physicochemical and bacteriological analyses described in “Standard Methods for the Examination of Water and Wastewater” were used to evaluate the efficiency of the treatment. In comparison to pure ZnO, the synthesized Ag/ZnO nanoparticles showed high efficiencies against Escherichia coli (E. coli) and general coliforms present in the lake water. These pathogens were absent after treatment using Ag/ZnO nanoparticles. The results indicate that Ag/ZnO nanoparticles synthesized via green chemistry are a promising candidate for the treatment of wastewaters contaminated by bacteria, due to their facile preparation, low-cost synthesis,and disinfection efficiency. KW - Synchrotron KW - BAMline PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562440 DO - https://doi.org/10.3390/nano12101764 SN - 2079-4991 VL - 12 IS - 10 SP - 1 EP - 18 PB - MDPI CY - Basel AN - OPUS4-56244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Margreiter, R. A1 - Baumann, J. A1 - Mantouvalou, I. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Strub, E. T1 - Investigations on fire-gilding N2 - Fire-gilding is a historic technique for the application of golden layers on a number of different base materials utilizing a gold amalgam. This technique leaves a significant amount of Hg in the golden layer, giving archeometrists a reliable indicator to identify firegildings. Recent findings on presumably fire-gilded objects have shown in several cases significantly lower Hg content than previously studied objects. This prompted a synchrotron-based X-ray fluorescence investigation into the Hg distribution along the material–gilding interface, as well as a series of measurements regarding the Hg content development in fire-gilded samples during artificial aging. This work presents findings on laboratory-prepared fire-gildings, indicating an Hg enrichment at the interface of firegilded silver samples. Notably, such an enrichment is missing in fire-gilded copper samples. Further, it is confirmed that fire-gilded layers typically do not undercut an Hg bulk content of 5%. In this light, it seems improbable that ancient samples that contain <5% Hg are fire-gilded. The results presented in this study might lead to a non-destructive method to identify the Hg enrichment at the interface. This might be obtained by a combination of different non-destructive measurements and might also work unambiguously in samples in which the gold top layer is altered. KW - BAMline KW - X-Ray Fluorescence KW - Gilding KW - Depth profile KW - Archaeometry PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552885 DO - https://doi.org/10.1111/arcm.12797 SN - 0003-813X SP - 1 EP - 14 PB - Wiley online library AN - OPUS4-55288 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 - Dobosy, Péter A1 - Nguyen, Hoang Thi Phuong A1 - Záray, Gyula A1 - Streli, Christina A1 - Ingerle, Dieter A1 - Ziegler, Philipp A1 - Radtke, Martin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Endrédi, Anett A1 - Fodor, Ferenc T1 - Effect of iodine species on biofortification of iodine in cabbage plants cultivated in hydroponic cultures N2 - Iodine is an essential trace element in the human diet because it is involved in the synthesis of thyroid hormones. Iodine deficiency affects over 2.2 billion people worldwide, making it a significant challenge to find plant-based sources of iodine that meet the recommended daily intake of this trace element. In this study, cabbage plants were cultivated in a hydroponic system containing iodine at concentrations ranging from 0.01 to 1.0 mg/L in the form of potassium iodide or potassium iodate. During the experiments, plant physiological parameters, biomass production, and concentration changes of iodine and selected microelements in different plant parts were investigated. In addition, the oxidation state of the accumulated iodine in root samples was determined. Results showed that iodine addition had no effect on photosynthetic efficiency and chlorophyll content. Iodide treatment did not considerably stimulate biomass production but iodate treatment increased it at concentrations less than 0.5 mg/L. Increasing iodine concentrations in the nutrient solutions increased iodine content in all plant parts; however, the iodide treatment was 2–7 times more efficient than the iodate treatment. It was concluded, that iodide addition was more favourable on the target element accumulation, however, it should be highlighted that application of this chemical form in nutrient solution decreased the concetrations of selected micoelement concentration comparing with the control plants. It was established that iodate was reduced to iodide during its uptake in cabbage roots, which means that independently from the oxidation number of iodine (+ 5, − 1) applied in the nutrient solutions, the reduced form of target element was transported to the aerial and edible tissues. KW - BAMline KW - XANES KW - Synchrotron KW - Lodine PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608330 DO - https://doi.org/10.1038/s41598-024-66575-z VL - 14 IS - 1 SP - 1 EP - 12 PB - Springer Science and Business Media LLC AN - OPUS4-60833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Huang, Junhao A1 - Klahn, Marcus A1 - Tian, Xinxin A1 - Bartling, Stephan A1 - Zimina, Anna A1 - Radtke, Martin A1 - Rockstroh, Nils A1 - Naliwajko, Pawel A1 - Steinfeldt, Norbert A1 - Peppel, Tim A1 - Grunwaldt, Jan‐Dierk A1 - Logsdail, Andrew J. A1 - Jiao, Haijun A1 - Strunk, Jennifer T1 - Fundamental Structural and Electronic Understanding of Palladium Catalysts on Nitride and Oxide Supports N2 - The nature of the support can fundamentally affect the function of a heterogeneous catalyst. For the novel type of isolated metal atom catalysts, sometimes referred to as single‐atom catalysts, systematic correlations are still rare. Here, we report a general finding that Pd on nitride supports (non‐metal and metal nitride) features a higher oxidation state compared to that on oxide supports (non‐metal and metal oxide). Through thorough oxidation state investigations by X‐ray absorption spectroscopy (XAS), X‐ray photoelectron spectroscopy (XPS), CO‐DRIFTS, and density functional theory (DFT) coupled with Bader charge analysis, it is found that Pd atoms prefer to interact with surface hydroxyl group to form a Pd(OH)x species on oxide supports, while on nitride supports, Pd atoms incorporate into the surface structure in the form of Pd−N bonds. Moreover, a correlation was built between the formal oxidation state and computational Bader charge, based on the periodic trend in electronegativity. KW - BAmline KW - XANES KW - Catalyst PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608341 DO - https://doi.org/10.1002/anie.202400174 SN - 1433-7851 VL - 63 IS - 20 SP - 1 EP - 9 PB - Wiley AN - OPUS4-60834 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Förste, F. A1 - Bauer, L. A1 - Streeck, C. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Kadow, D. A1 - Keil, C. A1 - Mantouvalou, I. T1 - Quantitative Analysis and 2D/3D Elemental Imaging of Cocoa Beans Using X‑ray Fluorescence Techniques N2 - As an important raw material for the confectionery industry, the cocoa bean (Theobroma cacao L.) has to meet certain legal requirements in terms of food safety and maximum contaminant levels in order to enter the cocoa market. Understanding the enrichment and distribution of essential minerals but also toxic metals is of utmost importance for improving the nutritional quality of this economically important raw food material. We present three X-ray fluorescence (XRF) techniques for elemental bio-imaging of intact cocoa beans and one additional XRF technique for quantitative analysis of cocoa pellets. The interrelation of all the methods presented gives a detailed picture of the content and 3D-resolved distribution of elements in complete cocoa beans for the first time. KW - BAMline KW - Synchrotron KW - XRF KW - CXC KW - Cocoa PY - 2023 DO - https://doi.org/10.1021/acs.analchem.2c05370 VL - 95 SP - 5627 EP - 5635 PB - ACS Publications AN - OPUS4-57832 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 - INPR A1 - Nowak, S. H. A1 - Petric, M. A1 - Buchriegler, J. A1 - Bjeoumikhov, A. A1 - Bjeoumikhova, Z. A1 - von Borany, J. A1 - Munnik, F. A1 - Radtke, Martin A1 - Renno, A. D. A1 - Reinholz, Uwe A1 - Scharf, O. A1 - Tilgner, J. A1 - Wedell, R. T1 - Road to micron resolution with a color X-ray camera - Polycapillary optics characterization N2 - In a color X-ray camera spatial resolution is achieved by means of a polycapillary optic conducting X-ray photons from small regions on a sample to distinct energy dispersive pixels on a CCD matrix. At present, the resolution limit of color X-ray camera systems can go down to several microns and is mainly restricted by Pixel dimensions. The recent development of an efficient subpixel resolution algorithm allows a release from pixel size, limiting the resolution only to the quality of theoptics. In this work polycapillary properties that influence the spatial resolution are systematized and assessed both theoretically and experimentally. It is demonstrated that with the current technological Level reaching one micron resolution is challenging, but possible. KW - Color X-ray camera KW - Polycapillary optics PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-404404 DO - https://doi.org/10.48550/arXiv.1705.08939 SN - 2331-8422 SP - 1 EP - 11 PB - Cornell University CY - Ithaca, NY AN - OPUS4-40440 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 - Radtke, Martin A1 - Buzanich, Günter A1 - Curado, Jessica A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Scharf, O. T1 - Slicing - a new method for non destructive 3D elemental sensitive characterization of materials N2 - Recent advances in synchrotron sources and detector technology have led to substantial improvements in spatial resolution and detection limits for X-ray fluorescence analysis (XRF). However, the non-destructive three-dimensional elemental sensitive characterization of samples remains a challenge. We demonstrate the use of the so-called 'Color X-ray Camera' (CXC) for 3D measurements for the first time. The excitation of the sample is realized with a thin sheet-beam. The stepwise movement of the sample allows getting the elemental distribution for each layer with one measurement. These layers can be combined to a full 3D dataset for each element afterwards. Since the information is collected layer by layer, there is no need to apply reconstruction techniques, which quite often are the reason for artifacts in the results achieved by computed tomography (CT). The field of applications is wide, as the 3D elemental distribution of a material contains clues to processes inside the samples from a variety of origins. The technique is of special interest and well suited for biological specimens, because their light matrix minimizes restricting absorption effects. Measurement examples of a hornet and the teeth of a Sorex araneus are shown. KW - SR-microXRF KW - 3D KW - CXC PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-324330 DO - https://doi.org/10.1039/c4ja00085d SN - 0267-9477 SN - 1364-5544 VL - 29 IS - 8 SP - 1339 EP - 1344 PB - Royal Society of Chemistry CY - London AN - OPUS4-32433 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 - CONF A1 - Radtke, Martin A1 - Fittschen, U. E. A. T1 - Shading Effects in SR-TXRF: Calculations and Experimental Visualization using a Color X-ray Camera T2 - Denver X-ray Conference CY - BIG SKY RESORT, BIG SKY, MONTANA, USA DA - 2014-07-28 PY - 2014 AN - OPUS4-32371 LA - deu 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 - Radtke, Martin A1 - Rakotondrajoa, A. T1 - Machine learning based quantification of synchrotron radiation-induced X-ray fluorescence measurements - a case study N2 - In this work, we describe the use of artificial neural networks for the quantification of X-ray fluorescence measurements. The training data were generated using Monte Carlo simulation, which avoided the use of adapted reference materials. The extension of the available data set by means of an ANN to generate additional data was demonstrated. Particular emphasis was put on the comparability of simulated and experimental data and how the influence of deviations can be reduced. The search for the optimal hyperparameter, manual and automatic, is also described. For the presented case, we were able to train a network with a mean absolute error of 0.1 weight percent for the synthetic data and 0.7 weight percent for a set of experimental data obtained with certified reference materials. KW - Machine learning KW - BAMline KW - XRF KW - Synchrotron KW - Neural network PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519008 DO - https://doi.org/10.1088/2632-2153/abc9fb SP - 1 EP - 16 PB - IOP Publishing AN - OPUS4-51900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Emmerling, Franziska ED - de Oliveira Guilherme Buzanich, Ana ED - Strange, R. W. T1 - Time- and spatial-resolved XAFS spectroscopy in a single shot: new analytical possibilities for in situ material characterization N2 - A new concept that comprises both time- and lateral-resolved X-ray absorption fine-structure information simultaneously in a single shot is presented. This uncomplicated set-up was tested at the BAMline at BESSY-II (Berlin, Germany). The primary broadband beam was generated by a double multilayer monochromator. The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by either an energy-sensitive area detector, the so-called color X-ray camera, or by an area-sensitive detector based on a CCD camera, in θ–2θ geometry. The first tests were performed with thin metal foils and some iron oxide mixtures. A time resolution of lower than 1 s together with a spatial resolution in one dimension of at least 50 mm is achieved. KW - Single-shot XAFS KW - Time resolution PY - 2016 UR - http://scripts.iucr.org/cgi-bin/paper?S1600577516003969 DO - https://doi.org/10.1107/S1600577516003969 SN - 1600-5775 VL - 23 SP - 769 EP - 776 PB - International Union of Crystallography CY - Liverpool, UK AN - OPUS4-35903 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Cakir, Cafer Tufan A1 - Radtke, Martin A1 - Haider, M. Bilal A1 - Emmerling, Franziska A1 - F. M. Oliveira, P. A1 - Michalchuk, Adam T1 - Dispersive x-ray absorption spectroscopy for time-resolved in situ monitoring of mechanochemical reactions N2 - X-ray absorption spectroscopy (XAS) provides a unique, atom-specific tool to probe the electronic structure of solids. By surmounting long-held limitations of powder-based XAS using a dynamically averaged powder in a Resonant Acoustic Mixer (RAM), we demonstrate how time-resolved in situ (TRIS) XAS provides unprecedented detail of mechanochemical synthesis. The use of a custom-designed dispersive XAS (DXAS) setup allows us to increase the time resolution over existing fluorescence measurements from ∼15 min to 2 s for a complete absorption spectrum. Hence, we here establish TRIS-XAS as a viable method for studying mechanochemical reactions and sampling reaction kinetics. The generality of our approach is demonstrated through RAM-induced (i) bottom-up Au nanoparticle mechanosynthesis and (ii) the synthesis of a prototypical metal organic framework, ZIF-8. Moreover, we demonstrate that our approach also works with the addition of a stainless steel milling ball, opening the door to using TRIS-DXAS for following conventional ball milling reactions. We expect that our TRIS-DXAS approach will become an essential part of the mechanochemical tool box. KW - In situ studies KW - Dipsersive XAS KW - Mechanochemistry KW - Time-resolved PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567659 DO - https://doi.org/10.1063/5.0130673 SN - 1089-7690 VL - 157 IS - 21 SP - 1 EP - 12 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-56765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Emmerling, Franziska ED - Rogge, Andreas ED - Meng, Birgit T1 - Exploring new materials for Green Intelligent Building - How can our BAMline help? N2 - In the scope of exploring and characterizing new materials related to Green Intelligent Building (GIB), we will provide an overview of the X-ray spectroscopy and diffraction analytical methods available at the BAMline /1/. and Myspot beamlines. These are two universal beamlines at the Berlin Synchrotron BESSY-II, where BAM has access and supervision role. Overarching electronic and structural properties at different time and length scales, such measurements enable a real-time characterization of materials properties. We will show-case in situ and ex situ deterioration and hydration studies on cement-based constructure materials. T2 - 11. Jahrestagung des DAfStb mit 63. Forschungskolloquium der BAM Green Intelligent Building CY - Berlin, Germany DA - 16.10.2024 KW - BAMline KW - Scope of exploring KW - Green intelligent building PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612882 SN - 978-3-9818564-7-7 SP - 30 EP - 36 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-61288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peters, Stefan A1 - Kunkel, Benny A1 - Cakir, Cafer Tufan A1 - Kabelitz, Anke A1 - Witte, Steffen A1 - Bernstein, Thomas A1 - Bartling, Stephan A1 - Radtke, Martin A1 - Emmerling, Franziska A1 - Abdel-Mageed, Ali Mohamed A1 - Wohlrab, Sebastian A1 - de Oliveira Guilherme Buzanich, Ana T1 - Time-, space- and energy-resolved in situ characterization of catalysts by X-ray absorption spectroscopy N2 - A novel setup for dispersive X-ray absorption spectroscopy (XAS) with simultaneous resolution of space, time and energy for in situ characterization of solid materials is demonstrated. KW - Dispersive XAS KW - Catalysis KW - In situ KW - Structure analysis PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584924 DO - https://doi.org/10.1039/d3cc03277a SN - 1359-7345 SP - 1 EP - 4 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cakir, Cafer Tufan A1 - Bogoclu, Can A1 - Emmerling, Franziska A1 - Streli, Christina A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin T1 - Machine learning for efficient grazing-exit x-ray absorption near edge structure spectroscopy analysis: Bayesian optimization approach N2 - In materials science, traditional techniques for analyzing layered structures are essential for obtaining information about local structure, electronic properties and chemical states. While valuable, these methods often require high vacuum environments and have limited depth profiling capabilities. The grazing exit x-ray absorption near-edge structure (GE-XANES) technique addresses these limitations by providing depth-resolved insight at ambient conditions, facilitating in situ material analysis without special sample preparation. However, GE-XANES is limited by long data acquisition times, which hinders its practicality for various applications. To overcome this, we have incorporated Bayesian optimization (BO) into the GE-XANES data acquisition process. This innovative approach potentially reduces measurement time by a factor of 50. We have used a standard GE-XANES experiment, which serve as reference, to validate the effectiveness and accuracy of the BO-informed experimental setup. Our results show that this optimized approach maintains data quality while significantly improving efficiency, making GE-XANES more accessible to a wider range of materials science applications. KW - Machine Learning KW - GE-XANES KW - Bayesian Optimization PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-603955 DO - https://doi.org/10.1088/2632-2153/ad4253 VL - 5 IS - 2 SP - 1 EP - 12 PB - IOP Publishing AN - OPUS4-60395 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Senges, Gene A1 - de Oliveira Guilherme Buzanich, Ana A1 - Lindič, Tilen A1 - Gully, Tyler A. A1 - Winter, Marlon A1 - Radtke, Martin A1 - Röder, Bettina A1 - Steinhauer, Simon A1 - Paulus, Beate A1 - Emmerling, Franziska A1 - Riedel, Sebastian T1 - Unravelling highly oxidized nickel centers in the anodic black film formed during the Simons process by in situ X-ray absorption near edge structure spectroscopy N2 - The electrofluorination after Simons has been used for the last century to produce everyday life materials. An in situ XANES investigation of the controversially debated black film apparent in the Simons process revealed high-valent nickel centers. KW - Synchrotron KW - BAMline KW - XANES PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608366 DO - https://doi.org/10.1039/d3sc06081k SN - 2041-6520 VL - 15 IS - 12 SP - 4504 EP - 4509 PB - Royal Society of Chemistry (RSC) AN - OPUS4-60836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kabelitz, Anke A1 - de Oliveira Guilherme Buzanich, Ana A1 - Joester, Maike A1 - Reinholz, Uwe A1 - Radtke, Martin A1 - Bienert, Ralf A1 - Schulz, K. A1 - Schmack, R. A1 - Kraehnert, R. A1 - Emmerling, Franziska T1 - Time-resolved in situ studies on the formation mechanism of iron oxide nanoparticles using combined fast-XANES and SAXS N2 - The reaction of iron chlorides with an alkaline reagent is one of the most prominent methods for the synthesis of iron oxide nanoparticles. We studied the particle formation mechanism using triethanolamine as reactant and stabilizing agent. In situ fast-X-ray absorption near edge spectroscopy and small-angle X-ray scattering provide information on the oxidation state and the structural information at the same time. In situ data were complemented by ex situ transmission electron microscopy, wide-angle X-ray scattering and Raman analysis of the formed nanoparticles. The formation of maghemite nanoparticles (γ-Fe2O3) from ferric and ferrous chloride was investigated. Prior to the formation of these nanoparticles, the formation and conversion of intermediate phases (akaganeite, iron(II, III) hydroxides) was observed which undergoes a morphological and structural collapse. The thus formed small magnetite nanoparticles (Fe3O4) grow further and convert to maghemite with increasing reaction time. KW - oxidation state KW - structural information KW - maghemite PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-351376 DO - https://doi.org/10.1039/C5CE01585E SN - 1466-8033 VL - 17 IS - 44 SP - 8463 EP - 8470 CY - London, UK AN - OPUS4-35137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Emmerling, Franziska T1 - Time- & spatial-resolved X-ray absorption fine structure (XAFS) spectroscopy in a single-shot – new analytical possibilities for in situ material characterization N2 - A new concept that comprises both time- and lateral-resolved X-ray absorption fine-structure information simultaneously in a single shot is presented. This uncomplicated set-up was tested at the BAMline at BESSY-II (Berlin, Germany). The primary broadband beam was generated by a double multilayer monochromator. The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by either an energy-sensitive area detector, the so-called color X-ray camera, or by an area-sensitive detector based on a CCD camera, in θ-2θ geometry. The first tests were performed with thin metal foils and some iron oxide mixtures. A time resolution of lower than 1 s together with a spatial resolution in one dimension of at least 50 µm is achieved. KW - Time resolution KW - Single-shot XAFS PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-370892 DO - https://doi.org/10.1107/S1600577516003969 SN - 1600-5775 IS - 23 SP - 769 EP - 776 PB - International Union of Crystallography CY - Chester, UK AN - OPUS4-37089 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 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Yusenko, Kirill A1 - Stawski, Tomasz A1 - Kulow, Anicó A1 - Cakir, Cafer Tufan A1 - Röder, Bettina A1 - Naese, Christoph A1 - Britzke, Ralf A1 - Sintschuk, Michael A1 - Emmerling, Franziska T1 - BAMline - A real-life sample materials research beamline N2 - With increasing demand and environmental concerns, researchers are exploring new materials that can perform as well or better than traditional materials while reducing environmental impact. The BAMline, a real-life sample materials research beamline, provides unique insights into materials’ electronic and chemical structure at different time and length scales. The beamline specializes in x-ray absorption spectroscopy, x-ray fluorescence spectroscopy, and tomography experiments. This enables real-time optimization of material properties and performance for various applications, such as energy transfer, energy storage, catalysis, and corrosion resistance. This paper gives an overview of the analytical methods and sample environments of the BAMline, which cover non-destructive testing experiments in materials science, chemistry, biology, medicine, and cultural heritage. We also present our own synthesis methods, processes, and equipment developed specifically for the BAMline, and we give examples of synthesized materials and their potential applications. Finally, this article discusses the future perspectives of the BAMline and its potential for further advances in sustainable materials research. KW - Extended X-ray absorption fine structure KW - Energy storage KW - Environmental impacts KW - Nondestructive testing techniques KW - X-ray fluorescence spectroscopy KW - Corrosion KW - Near edge X-ray absorption fine structure spectroscopy KW - X-ray absorption spectroscopy PY - 2023 DO - https://doi.org/10.1063/5.0157194 VL - 158 IS - 24 SP - 1 EP - 22 PB - AIP Publishing AN - OPUS4-57824 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Emmerling, Franziska ED - de Oliveira Guilherme Buzanich, Ana T1 - Time- and spatial-resolved X-ray absorption fine structure (XAFS) spectroscopy in a single-shot: new analytical possibilities for in situ material characterization N2 - A new concept that comprises both time- and lateral-resolved X-ray absorption fine-structure information simultaneously in a single shot is presented. This uncomplicated set-up was tested at the BAMline at BESSY-II (Berlin, Germany). The primary broadband beam was generated by a double multilayer monochromator. The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by either an energy-sensitive area detector, the so-called color X-ray camera, or by an area-sensitive detector based on a CCD camera, in θ-2θ geometry. The first tests were performed with thin metal foils and some iron oxide mixtures. A time resolution of lower than 1 s together with a spatial resolution in one dimension of at least 50 µm is achieved. KW - Single-shot XAFS KW - Time resolution KW - Spatial resolution KW - Divergent XAFS PY - 2016 DO - https://doi.org/10.1107/S1600577516003969 SN - 1600-5775 VL - 23 SP - 769 EP - 776 PB - International Union of Crystallography AN - OPUS4-38370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Energy Resolved Imaging with Coded Apertures N2 - Our aim is to develop a simple and inexpensive method for full field X-ray fluorescence imaging.We combine an energydispersive array detector with a coded aperture to obtain high resolut ion images. To obtain the information from the recorded image a reconstruction step is necessary. The reconstruction methods we have developed, were tested on simulated data and then applied to experimental data. The first tests were carried out at the BAMline @BESSY II. This method enables the simultaneous detection of multiple elements,which is important e.g. in the field of catalysis. T2 - SRI 2021 CY - Online meeting DA - 28.3.2022 KW - Synchrotron KW - BAMline KW - Machine Learning KW - Coded Aperture PY - 2022 AN - OPUS4-56298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Insights into materials with hard x-rays: capabilities of the bamline N2 - This contribution provides an overview of the BAMline synchrotron radiation beamline, which specializes in hard X-ray spectroscopy techniques for materials research. The BAMline offers X-ray absorption spectroscopy (XAS), x-ray fluorescence spectroscopy (XRF), and tomography to study materials' electronic structure, chemical composition, and structure. Key capabilities include standard and dispersive XAS for electronic structure, micro-XRF for elemental mapping, coded aperture imaging, and depth-resolved grazing exit XAS. The BAMline enables in situ characterization during materials synthesis and functions for energy, catalysis, corrosion, biology, and cultural heritage applications. Ongoing developments like the implementation of machine learning techniques for experiment optimization and data analysis will be discussed. For instance, Bayesian optimization is being used to improve beamline alignment and scanning. An outlook to the future, where the BAMline will continue pioneering dynamic and multi-scale characterization, aided by advanced data science methods, to provide unique insights into materials research, will be given. T2 - μ-XRF at Elettra 2.0: challenges and opportunities CY - Trieste, Italy DA - 11.09.2023 KW - Synchrotron KW - XRF KW - XANES KW - Bayes PY - 2023 AN - OPUS4-58607 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 -