TY - GEN A1 - Frisch, A. A1 - Merchel, Silke A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Vogl, Jochen ED - Röhrs, S. T1 - Synchrotron-XRF und PIXE Untersuchungen an bronzezeitlichen Fussringen T2 - Jahrestagung 2003 im Ethnologischen Museum Berlin-Dahlem CY - Berlin, Deutschland DA - 2003-03-12 PY - 2003 SN - 3-00-014223-1 SN - 0949-4057 SP - 101 EP - 103 CY - [Frankfurt am Main] AN - OPUS4-2355 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Berger, Achim A1 - Ecker, Klaus A1 - Görner, Wolf A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Segebade, Christian T1 - Strahlenverfahren in Kombination - ein Werkzeug für Analyse und Zertifizierung von Feststoffen T2 - 12. Jahrescolloquium "Analyse von Feststoffen unterschiedlicher Materialien aus Industrie und Umwelt" CY - Berlin, Deutschland DA - 2002-11-19 PY - 2002 SP - 1(?) AN - OPUS4-2025 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Berger, Achim A1 - Görner, Wolf A1 - Merchel, Silke A1 - Procop, Mathias A1 - Radtke, Martin A1 - Riesemeier, Heinrich T1 - SY-XRF in certification of a reference material at the BAMline PY - 2003 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2002.pdf#page=311 SN - 0179-4159 SP - 311 EP - 312 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-2492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reiche, I. A1 - Berger, Achim A1 - Görner, Wolf A1 - Merchel, Silke A1 - Radtke, Martin A1 - Riederer, J. A1 - Riesemeier, Heinrich T1 - Silberstiftzeichnungen - Zerstörungsfreie Spurenanalyse mit Synchrotronstrahlung T2 - 10. IADA-Kongress (Internationale Arbeitsgemeinschaft der Archiv-, Bibliotheks- und Graphikrestauratoren) CY - Göttingen, Deutschland DA - 2003-09-21 PY - 2003 SN - 1563-2628 VL - 4 PB - Foto Text Verl. CY - Stuttgart AN - OPUS4-2663 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lahiri, D. A1 - Sharma, S.M. A1 - Verma, A.K. A1 - Vishwanadh, B. A1 - Dey, G.K. A1 - Schumacher, G. A1 - Scherb, T. A1 - Riesemeier, Heinrich A1 - Reinholz, Uwe A1 - Radtke, Martin A1 - Banerjee, S. T1 - Investigation of short-range structural order in Zr69.5Cu12Ni11Al7.5 and Zr41.5Ti41.5Ni17 glasses, using X-ray absorption spectroscopy and ab initio molecular dynamics simulations N2 - Short-range order has been investigated in Zr69.5Cu12Ni11Al7.5 and Zr41.5Ti41.5Ni17 metallic glasses using X-ray absorption spectroscopy and ab initio molecular dynamics simulations. While both of these alloys are good glass formers, there is a difference in their glass-forming abilities (Zr41.5Ti41.5Ni17 > Zr69.5Cu12Ni11Al7.5). This difference is explained by inciting the relative importance of strong chemical order, icosahedral content, cluster symmetry and configuration diversity. KW - Multi-component alloy KW - Glass-forming ability KW - XAFS KW - Local structure KW - AIMD simulation PY - 2014 DO - https://doi.org/10.1107/S1600577514017792 SN - 0909-0495 SN - 1600-5775 VL - 21 IS - 6 SP - 1296 EP - 1304 PB - Blackwell Publishing CY - Oxford AN - OPUS4-31837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reiche, I. A1 - Berger, Achim A1 - Duval, A. A1 - Görner, Wolf A1 - Guicharnaud, H. A1 - Merchel, Silke A1 - Radtke, Martin A1 - Riederer, J. A1 - Riesemeier, Heinrich A1 - Roth, M. ED - Marabelli, M. ED - Tabaso, M. T1 - Spatially resolved SR-XRF analyses of complex drawings of the Holbein family T2 - 8th International Conference on "Non-Destructive Investigations and Microanalysis for the Diagnostics and Conservation of the Cultural and Environmental Heritage" CY - Lecce, Italy DA - 2005-05-15 KW - X-ray spectrometry KW - XRF KW - Röntgenfluoreszenzanalyse KW - RFA KW - Silverpoint drawing KW - Silberstiftzeichnung PY - 2005 SP - 7 pages PB - Italian Society of Non Destructive Testing CY - Lecce AN - OPUS4-7677 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reiche, I. A1 - Berger, Achim A1 - Görner, Wolf A1 - Merchel, Silke A1 - Radtke, Martin A1 - Riederer, J. A1 - Riesemeier, Heinrich A1 - Roth, M. T1 - Following the traces of Albrecht Dürer: analysis of silverpoint drawings by spatially resolved synchrotron-induced X-ray fluorescence analysis N2 - Spatially resolved X-ray fluorescence analysis using synchrotron radiation (SR-XRF) at the wavelength shifter beamline, BAMline, at BESSY was used to investigate Renaissance silverpoint drawings as it is extremely sensitive, non-destructive and can be carried out in air using an excitation spot in the hundred micrometer range. This paper deals with first results of the study of silverpoint drawings of Albrecht Dürer (1471–1528) belonging to the sketchbook that Albrecht Dürer used during a travel to the Netherlands in 1520/21. These results are compared to a PIXE study performed on drawings from the same sketchbook. The minor element composition of the silverpoint used for the drawings in the sketchbook was (10.6 ± 3.5) wt.% of Cu and traces of Zn. Mercury was found in the marks but does not belong to the initial composition of the silverpoint as it is attributed to an alteration phenomenon. One drawing of the sketchbook represents an exception. It consists of silver marks containing an additional minor element, Zn, in the marks and was, therefore, created with another silverpoint, probably at a different time than the other drawings. KW - Synchrotron KW - SR-XRF analysis KW - Drawing KW - Silverpoint KW - Albrecht Dürer PY - 2004 DO - https://doi.org/10.1016/j.nimb.2004.03.081 SN - 0168-583X SN - 1872-9584 VL - 226 IS - 1-2 SP - 83 EP - 91 PB - Elsevier CY - Amsterdam AN - OPUS4-4574 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Berger, Achim A1 - Calligaro, T. A1 - Duval, A. A1 - Görner, Wolf A1 - Guerra, M.-F. A1 - Merchel, Silke A1 - Radtke, Martin A1 - Reiche, I. A1 - Riesemeier, Heinrich A1 - Roth, M. T1 - Study of Ag and Au based historical and archaeological objects by high energy Sy-XRF KW - Synchrotron KW - XRF analysis KW - Drawings KW - Archaeometry KW - Gold KW - Röntgenfluoreszenzanalyse KW - RFA KW - Zeichnungen KW - Archäometrie KW - Albrecht Dürer KW - gold PY - 2004 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2003.pdf#page=544 SN - 0179-4159 SP - 544 EP - 546 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-3507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riesemeier, Heinrich T1 - Schwefelbestimmung in Kraftstoffen mittels SYRFA T2 - DGZfP-Jahrestagung 2003: Zerstörungsfreie Materialprüfung - ZfP in Anwendung, Entwicklung und Forschung CY - Mainz, Germany DA - 2003-05-26 PY - 2003 AN - OPUS4-3855 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Reiche, I. A1 - Berger, Achim A1 - Bevers, H. A1 - Dupuis, G. A1 - Duval, A. A1 - Görner, Wolf A1 - Guicharnaud, H. A1 - Merchel, Silke A1 - Radtke, Martin A1 - Riederer, J. A1 - Riesemeier, Heinrich A1 - Roth, M. T1 - Spatially resolved SR-XRF analyses of complex drawings by the Holbein family and silverpoint drawings by Rembrandt KW - X-ray spectrometry KW - XRF KW - Röntgenfluoreszenzanalyse KW - RFA KW - Silverpoint drawing KW - Silberstiftzeichnung PY - 2005 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2004.pdf#page=491 SN - 0179-4159 SP - 491 EP - 493 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-7380 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Armbruster, B. A1 - Eilbracht, H. A1 - Grüger, A. A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Reiche, I. T1 - The Vikings in Berlin: SR-XRF analyses of the Hiddensee gold jewellery PY - 2005 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/infos/bessy/highlights2004.pdf#page=32 SN - 1611-6127 SP - 32 EP - 33 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-7386 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riesemeier, Heinrich A1 - Ecker, Klaus A1 - Görner, Wolf A1 - Müller, Bernd R. A1 - Radtke, Martin A1 - Krumrey, M. T1 - Layout and first XRF Applications of the BAMline at BESSY II+ N2 - The first hard x-ray beamline at BESSY II has been installed by BAM and PTB at a superconducting 7 T wavelength shifter. The main optical elements of the beamline are a double-multilayer monochromator and a double-crystal monochromator. Depending on the application, the two devices are used separately or in-line. The main applications of the monochromatic radiation with photon energies up to 60 keV are x-ray fluorescence analysis, micro computed tomography, x-ray topography, detector calibration and reflectometry. Calculable undispersed radiation up to 200 keV is available for radiometric applications. KW - BAMline KW - XRF PY - 2005 DO - https://doi.org/10.1002/xrs.750 SN - 0049-8246 VL - 34 IS - 2 SP - 160 EP - 163 PB - Wiley CY - Chichester AN - OPUS4-11929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Wilde, L. A1 - Radnik, J. A1 - Schneider, M. A1 - Herein, D. A1 - Riesemeier, Heinrich A1 - Radtke, Martin T1 - In situ TEY cell for XAS measurements at the BAMline PY - 2004 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2003.pdf#page=283 SN - 0179-4159 SP - 283 EP - 285 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-3508 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reiche, I. A1 - Berger, Achim A1 - Duval, A. A1 - Görner, Wolf A1 - Merchel, Silke A1 - Radtke, Martin A1 - Riederer, J. A1 - Riesemeier, Heinrich T1 - Metallstiftzeichnungen Albrecht Dürers KW - Synchrotron KW - XRF analysis KW - Drawings KW - Archaeometry KW - Röntgenfluoreszenzanalyse (RFA) KW - Zeichnungen KW - Archäometrie KW - Albrecht Dürer PY - 2004 SN - 1563-2628 VL - 5 IS - 2 SP - 30 EP - 38 PB - Foto Text Verl. CY - Stuttgart AN - OPUS4-3570 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riesemeier, Heinrich T1 - Layout and first applications of the BAMline at BESSY II T2 - EDXRS 2002 - European Conference on Energy Dispersive X-Ray Spectrometry CY - Berlin, Germany DA - 2002-06-16 PY - 2002 AN - OPUS4-3003 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 - GEN A1 - Eichelbaum, M. A1 - Rademann, K. A1 - Müller, Ralf A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Görner, Wolf T1 - Vom Atom zum Nanodraht: Kontrolliertes Wachstum von Edelmetall-Nanokristalliten in Kalk-Natron-Silikatglas T2 - 79. Glastechnische Tagung CY - Würzburg, Deutschland DA - 2005-05-23 KW - Glas KW - Metallnanocluster KW - Optische Eigenschaften PY - 2005 SN - 3-921089-43-3 SP - 15 Seiten PB - Deutsche Glastechnische Gesellschaft CY - Offenbach AN - OPUS4-7558 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reiche, I. A1 - Radtke, Martin A1 - Berger, Achim A1 - Görner, Wolf A1 - Merchel, Silke A1 - Riesemeier, Heinrich A1 - Bevers, H. T1 - Spatially resolved synchrotron radiation induced X-ray fluorescence analyses of rare Rembrandt silverpoint drawings N2 - New analyses of a series of very rare silverpoint drawings that were executed by Rembrandt Harmensz. van Rijn (1606–1669) which are kept today in the Kupferstichkabinett (Museum of Prints and Drawings) of the State Museums of Berlin are reported here. Analysis of these drawings requires particular attention because the study has to be fully non-destructive and extremely sensitive. The metal alloy on the paper does not exceed some hundreds of µg/cm². Therefore, synchrotron radiation induced X-ray fluorescence (SR-XRF) is – together with external micro-proton-induced X-ray emission – the only well-suited method for the analyses of metalpoint drawings. In some primary work, about 25 German and Flemish metalpoint drawings were investigated using spatially resolved SR-XRF analysis at the BAMline at BESSY. This study enlarges the existing French–German database of metalpoint drawings dating from the 15th and 16th centuries, as these Rembrandt drawings originate from the 17th century where this graphical technique was even rarer and already obsolete. It also illustrates how SR-XRF analysis can reinforce art historical assumptions on the dating of drawings and their connection. KW - X-ray spectrometry KW - XRF KW - Röntgenfluoreszenzanalyse KW - RFA KW - Silverpoint drawing KW - Silberstiftzeichnung PY - 2006 DO - https://doi.org/10.1007/s00339-006-3505-4 SN - 0947-8396 VL - 83 IS - 2 SP - 169 EP - 173 PB - Springer CY - Berlin AN - OPUS4-12532 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Reiche, I. A1 - Berger, Achim A1 - Duval, A. A1 - Görner, Wolf A1 - Guicharnaud, H. A1 - Merchel, Silke A1 - Radtke, Martin A1 - Riederer, J. A1 - Riesemeier, Heinrich A1 - Roth, M. ED - Denker, A. ED - Adriaens, A. ED - Dowsett, M. ED - Giumlia-Mair, A. T1 - Synchrotron radiation and protons on the traces of famous artists - Non-destructive analyses of silverpoint drawings by Albrecht Dürer KW - X-ray spectrometry KW - XRF KW - Röntgenfluoreszenzanalyse KW - RFA KW - Silverpoint drawing KW - Silberstiftzeichnung PY - 2006 SN - 3-8167-7178-5 SP - 91 EP - 101 PB - Fraunhofer-IRB-Verl. CY - Stuttgart AN - OPUS4-14190 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Görner, Wolf A1 - Eichelbaum, Maik A1 - Matschat, Ralf A1 - Rademann, K. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich T1 - Non-destructive investigation of composition, chemical properties and structure of materials by synchrotron radiation PY - 2006 SN - 0007-1137 VL - 48 IS - 9 SP - 540 EP - 544 PB - British Institute of Non-Destructive Testing CY - Northampton AN - OPUS4-14186 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guerra, M. F. A1 - Calligaro, T. A1 - Radtke, Martin A1 - Reiche, I. A1 - Riesemeier, Heinrich T1 - Fingerprinting ancient gold by measuring Pt with spatially resolved high energy Sy-XRF N2 - Trace elements of ancient gold such as Pt, give fundamental information on the circulation of the metal in the past. In the case of objects from the cultural heritage, the determination of trace elements requires non-destructive point analysis in general. These conditions and the need of good detection limits restrain the number of applicable analytical techniques. After the development of a PIXE set-up with a selective Cu or Zn filter of 75 µm and of a PIXE-XRF set-up using a primary target of As, we tested the possibilities of spatially resolved Sy-XRF to determine Pt in gold alloys. With a Zn filter, PIXE showed a detection limit of 1000 ppm in gold while PIXE-XRF lowers this detection limit down to 80 ppm. This last value being constrained by the resonant Raman effect produced on gold. In order to improve the detection limit of Pt keeping the non-destructiveness and access to point analysis, we developed an analytical protocol for XRF with synchrotron radiation at BESSY II, using the BAMline set-up. The L-lines of Pt were excited by a beam of energy above and below 11.564 keV and measured using a Si(Li) detector with a 50 µm Cu filter. A µ-beam of 100–250 µm2 was used according to the size of the sample. The determination of the Pt content in the samples was carried out by Monte-Carlo simulation and subtraction of Au and Pt spectra obtained on pure standards. The limit of detection for Pt of 20 ppm was determined by using certified standards. The detection limits of a small set of other characteristic elements of gold were also measured using an incident energy of 33 keV. KW - PIXE-XRF KW - Sy-XRF KW - Pt KW - Ancient gold KW - Fingerprinting PY - 2005 DO - https://doi.org/10.1016/j.nimb.2005.06.150 SN - 0168-583X SN - 1872-9584 VL - 240 IS - 1-2 SP - 505 EP - 511 PB - Elsevier CY - Amsterdam AN - OPUS4-14236 LA - eng 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 - Scharf, Oliver A1 - Ihle, S. A1 - Ordavo, I. A1 - Arkadiev, V. A1 - Bjeoumikhov, A. A1 - Bjeoumikhova, S. A1 - Buzanich, Günter A1 - Gubzhokov, R. A1 - Günther, A. A1 - Hartmann, R. A1 - Kühbacher, M. A1 - Lang, M. A1 - Langhoff, N. A1 - Liebel, A. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Soltau, H. A1 - Strüder, L. A1 - Thünemann, Andreas A1 - Wedell, R. T1 - Compact pnCCD-based X-ray camera with high spatial and energy resolution: a color X-ray camera N2 - For many applications there is a requirement for nondestructive analytical investigation of the elemental distribution in a sample. With the improvement of X-ray optics and spectroscopic X-ray imagers, full field X-ray fluorescence (FF-XRF) methods are feasible. A new device for high-resolution X-ray imaging, an energy and spatial resolving X-ray camera, is presented. The basic idea behind this so-called 'color X-ray camera' (CXC) is to combine an energy dispersive array detector for X-rays, in this case a pnCCD, with polycapillary optics. Imaging is achieved using multiframe recording of the energy and the point of impact of single photons. The camera was tested using a laboratory 30 µm microfocus X-ray tube and synchrotron radiation from BESSY II at the BAMline facility. These experiments demonstrate the suitability of the camera for X-ray fluorescence analytics. The camera simultaneously records 69696 spectra with an energy resolution of 152 eV for manganese Kα with a spatial resolution of 50 µm over an imaging area of 12.7 × 12.7 mm². It is sensitive to photons in the energy region between 3 and 40 keV, limited by a 50 µm beryllium window, and the sensitive thickness of 450 µm of the chip. Online preview of the sample is possible as the software updates the sums of the counts for certain energy channel ranges during the measurement and displays 2-D false-color maps as well as spectra of selected regions. The complete data cube of 264 × 264 spectra is saved for further qualitative and quantitative processing. KW - Color X-ray camera KW - X-ray fluorescence KW - pnCCD KW - Polycapillary optic KW - Synchrotron radiation PY - 2011 DO - https://doi.org/10.1021/ac102811p SN - 0003-2700 SN - 1520-6882 VL - 83 IS - 7 SP - 2532 EP - 2538 PB - American Chemical Society CY - Washington, DC AN - OPUS4-23948 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guerra, M. F. A1 - Radtke, Martin A1 - Reiche, I. A1 - Riesemeier, Heinrich A1 - Strub, Erik T1 - Analysis of trace elements in gold alloys by SR-XRF at high energy at the BAMline N2 - Measuring in a non-destructive way the characteristic trace elements of the metal allows following the circulation of gold in the past. The aim of this work is to probe the possibilities of X-ray fluorescence with high energy synchrotron radiation (SR-XRF) at the BAMline at BESSY II to determine the concentration of Pt in ancient gold alloys. A HP-Ge detector was used to measure the Pt K-lines excited with an incident energy of 79.5 keV. Data processing was done by subtraction of a Pt free gold standard spectrum from the spectrum of the sample. Depending on the sample composition, the MDL ranges between 40 and 90 ppm. The first results obtained for a small set of gold alloys of different thickness, size and composition showed that high energy SR-XRF is a significant method for the non-destructive determination of Pt in gold. KW - SR-XRF KW - Gold KW - Provenancing KW - Trace elements PY - 2008 DO - https://doi.org/10.1016/j.nimb.2008.03.008 SN - 0168-583X SN - 1872-9584 VL - 266 IS - 10 SP - 2334 EP - 2338 PB - Elsevier CY - Amsterdam AN - OPUS4-17735 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riesemeier, Heinrich T1 - Materials research at the 7T-Wave Length Shifter, WLS-1 at BESSY: Instrumentation and selected results T2 - Seminar, ANKA CY - Karlsruhe, Germany DA - 2008-03-03 PY - 2008 AN - OPUS4-17898 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mandel, K. A1 - Szczerba, Wojciech A1 - Thünemann, Andreas A1 - Riesemeier, Heinrich A1 - Girod, Matthias A1 - Sextl, G. T1 - Nitric acid-stabilized superparamagnetic iron oxide nanoparticles studied with X-rays N2 - Agglomerated superparamagnetic iron oxide nanoparticles can easily and in large scale be precipitated from iron salt solutions. Although the process is well known, it is ambiguously either assumed that magnetite or maghemite is obtained. The first part of our study clarifies this question using X-ray absorption spectroscopy. For further processing of the nanoparticles, i.e., for giving them a surface functionality or incorporating them into composites, it is important to break the agglomerates and individualize the particles at first. This can effectively be done with nitric acid treatment. The influence of this process on the particles chemistry and structure was analyzed in great detail using X-ray diffraction, X-ray absorption, and smallangle X-ray scattering. In contrast to our expectation, no oxidation from magnetite (Fe3O4) to maghemite (γ- Fe2O3) was found; the formal valence of the particles in any case is magnetite (Fe3O4). Instead, an increase in the particles' surface disorder was discovered from X-ray absorption analyses and high-resolution transmission electron microscopy. The acid treatment roughens and distorts the surface of the nanoparticles which is connected with an increased spin disorder. KW - XANES KW - EXAFS KW - SAXS KW - Coprecipitation KW - Iron oxide spectra KW - Ferrofluid PY - 2012 DO - https://doi.org/10.1007/s11051-012-1066-3 SN - 1388-0764 SN - 1572-896X VL - 14 IS - 8 SP - 1 EP - 9 PB - Kluwer CY - Dordrecht AN - OPUS4-26357 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szczerba, Wojciech A1 - Schott, M. A1 - Riesemeier, Heinrich A1 - Thünemann, Andreas A1 - Kurth, D.G. T1 - Thermally induced structural rearrangement of the Fe(II) coordination geometry in metallo-supramolecular polyelectrolytes N2 - Rigid rod-type metallo-supramolecular coordination polyelectrolytes with Fe(II) centres (Fe-MEPEs) are produced via the self-assembly of the ditopic ligand 1,4-bis(2,2':6',2''-terpyridine-4'-yl)benzene (tpy-ph-tpy) and Fe(II) acetate. Fe-MEPEs exhibit remarkable electrochromic properties; they change colour from blue to transparent when an electric potential is applied. This electrochemical process is generally reversible. The blue colour in the ground state is a result of a metal-to-ligand charge transfer at the Fe(II) centre ion in a quasi-octahedral geometry. When annealed at temperatures above 100 °C, the blue colour turns into green and the formerly reversible electrochromic properties are lost, even after cooling down to room temperature. The thermally induced changes in the Fe(II) coordination sphere are investigated in situ during annealing of a solid Fe-MEPE using X-ray absorption fine structure (XAFS) spectroscopy. The study reveals that the thermally induced transition is not accompanied by a redox process at the Fe(II) centre. From the detailed analysis of the XAFS spectra, the changes are attributed to structural changes in the coordination sphere of the Fe(II) site. In the low temperature state, the Fe(II) ion rests in a quasi-octahedral coordination environment surrounded by six nitrogen atoms of the pyridine rings. The axial Fe–N bond length is 1.94 Å, while the equatorial bond length amounts to 1.98 Å. In the high temperature state, the FeN6-site exhibits a distortion with the axial Fe–N bonds being shortened to 1.88 Å and the equatorial Fe–N bonds being elongated to 2.01 Å. KW - Metallo-supramolecular polyelectrolytes KW - Electrochromism KW - XANES KW - EXAFS KW - Local structure KW - Thermal stability PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-317331 DO - https://doi.org/10.1039/c4cp01187b SN - 1463-9076 SN - 1463-9084 VL - 16 IS - 36 SP - 19694 EP - 19701 PB - The Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-31733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szczerba, Wojciech A1 - Riesemeier, Heinrich A1 - Thünemann, Andreas T1 - Bond length cntraction in gold nanoparticles N2 - The structure of nanoparticles typically differs from its bulk counterpart. Predominantly, the structures of gold nanoparticles have been under exceedingly intense discussion since the discovery of their high catalytic activity. We found an increasing bond length contraction with decreasing particle size for citrate-stabilized gold nanoparticles in aqueous solution as determined by in situ extended X-ray absorption fine structure (EXAFS) spectroscopy. Particle sizes and size distributions were determined by small-angle X-ray scattering. The analysis of the obtained EXAFS spectra employing ab initio calculations reveals that the Au–Au bond length undergoes a contraction of 2 pm for nanoparticles with a radius of 2.9 nm. NIST reference material RM 8011 gold nanoparticles with a radius of 4.4 nm exhibit a smaller contraction of approximately 1 pm. Finally, gold atoms in RM 8013 particles with a radius of 25.7 nm show distances of 288 pm— identical to the distance in gold foil—and exhibits bulk-like properties. The observed bond length contraction of gold nanoparticles in solution is significantly smaller than previously reported for gold nanoparticle deposited on surfaces, which is up to 15 pm. This indicates that the bond length contraction effect of 'free' and 'surfaceimmobilized' nanoparticles differ fundamentally. Such difference could be essential for the understanding of nanoparticle-supported catalysis. KW - Small-angle X-ray scattering KW - SAXS KW - EXAFS KW - XAFS KW - Nanoparticle KW - Gold PY - 2010 DO - https://doi.org/10.1007/s00216-010-4200-z SN - 1618-2642 SN - 1618-2650 VL - 398 IS - 5 SP - 1967 EP - 1972 PB - Springer CY - Berlin AN - OPUS4-22173 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 - 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 - 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 - Brieger, C. A1 - Melke, J. A1 - van der Bosch, N. A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - de Oliveira Guilherme Buzanich, Ana A1 - Krishna Kayarkatte, M. A1 - Schoeckel, A. A1 - Roth, C. T1 - A combined in-situ XAS-DRIFTS study unraveling adsorbate induced changes on the Pt nanoparticle structure N2 - The adsorption behavior of Platinum nanoparticles was studied for the as-received catalyst (under inert gas), under hydrogen and CO atmosphere using our newly designed in-situ cell. X-ray Absorption Spectroscopy (XAS) and Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS) experiments were performed simultaneously with high data quality. Structural information and the type of adsorbate could be revealed via Extended X-ray Absorption Fine Structure (EXAFS) analysis, Dl X-ray Absorption Near Edge Structure analysis (Dl XANES) and in-situ DRIFTS. The as-received catalyst showed sub-surface oxygen and O(n-fold). Under CO atmosphere only CO(atop) was found. Reversible adsorbate induced changes of the Pt nanoparticle structure were derived from changes in the PtAPt coordination number and the corresponding bond distance. Under reducing conditions (H2, CO) a significant increase in both values occurred. Temperature dependent desorption of CO revealed a gradual shift from PtACO to PtAO. Reoxidation was clearly assigned to strong metal support interaction from the SiO2 support. KW - X-ray absorption spectroscopy KW - DRIFTS KW - XANES KW - CO adsorption KW - Platinum KW - Strong metal support interaction KW - Silica support KW - Adsorbates KW - Infrared spectroscopy PY - 2016 DO - https://doi.org/10.1016/j.jcat.2016.03.034 IS - 339 SP - 57 EP - 67 PB - Elsevier Inc. CY - Philadelphia, Pennsylvania, USA AN - OPUS4-35815 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 - 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 - Nusser, K. A1 - Mosbauer, T. A1 - Schneider, G. J. A1 - Brandt, K. A1 - Weidemann, Gerd A1 - Goebbels, Jürgen A1 - Riesemeier, Heinrich A1 - Göritz, D. T1 - Silica dispersion in styrene butadiene rubber composites studied by synchrotron tomography N2 - By means of synchrotron X-ray computed tomography, model composites consisting of silica and styrene–butadiene rubber were studied with a very high spatial resolution. By our analysis technique we were able to determine the nano- and micro dispersion from the experimental results by our numerical analysis. These results are discussed with respect to crucial advantages of the generically 3-dimensional tomography technique as compared to 2-dimensional methods. Our quantitative analysis of the 3d images demonstrates that in the case of our model composites the filler dispersion is good, independent on the filler concentration. Our new 3-dimensional results evidence that considering only 2-d pictures may lead to ambiguities that can lead to wrong conclusions. KW - X-ray tomography KW - Silica KW - Styrene butadiene rubber KW - Dispersion PY - 2012 DO - https://doi.org/10.1016/j.jnoncrysol.2011.10.009 SN - 0022-3093 VL - 358 IS - 3 SP - 557 EP - 563 PB - North-Holland Publ. Co. CY - Amsterdam AN - OPUS4-26105 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 - JOUR A1 - Polte, Jörg A1 - Emmerling, Franziska A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Thünemann, Andreas T1 - Real-time monitoring of copolymer stabilized growing gold nanoparticles N2 - A great challenge in the production of nanoparticles with defined sizes and properties is to control their growth in situ. We developed a dedicated combined small-angle X-ray scattering (SAXS) and X-ray absorption spectroscopy (XAS) setup to monitor nanoparticle formation in solution. The capabilities of simultaneously deriving particle sizes and oxidation states of atoms/ions are illustrated for the formation of spherical gold nanoparticles by the reduction of hydrogen tetrachloroaureate (HAuCl4). Particles with initial radii of 4.60 ± 0.10 nm and final radii of 5.67 ± 0.10 nm were produced in a levitated droplet with a volume of 4 µL. An ethylene oxide/propylene oxide triblock copolymer PEO-PPO-PEO (Pluronic F-127) functions as reducing agent and colloidal stabilizer. XANES shows in situ how the gold was reduced in the droplet from Au(III) to Au(0), and simultaneously SAXS recorded the size distribution of the formed nanoparticles. It is shown that the final particle number is reached quickly. Thereafter, only the particles’ sizes increase. Comparison of XANES and SAXS shows that the quantity of Au(0) is higher than the quantity of gold located in the nanoparticles while the particles are growing. Finally, all the Au(0) is found in the nanoparticles. We tentatively attribute this finding to the pseudo crown ether effect of the polymer surfactant that kinetically stabilizes gold atoms when formed from gold ions within their protecting cavity. A simple “burst” mechanism for the gold nanoparticle formation is the consequence. The possibility of an inhomogeneous particles structure with an enhanced density near the particle surface is discussed. PY - 2010 DO - https://doi.org/10.1021/la903829q SN - 0743-7463 SN - 1520-5827 VL - 26 IS - 8 SP - 5889 EP - 5894 PB - American Chemical Society CY - Washington, DC AN - OPUS4-21223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paris, O. A1 - Li, C. A1 - Siegel, S. A1 - Weseloh, G. A1 - Emmerling, Franziska A1 - Riesemeier, Heinrich A1 - Erko, A. A1 - Fratzl, P. T1 - A new experimental station for simultaneous X-ray microbeam scanning for small- and wide-angle scattering and fluorescence at BESSY II N2 - A new instrument for simultaneous microbeam small- and wide-angle X-ray scattering and X-ray fluorescence (SAXS/WAXS/XRF) is presented. The instrument is installed at the microfocus beamline at BESSY II and provides a beam of 10 µm size with a flux of about 109 photons s-1. A SAXS resolution up to 500 Å d-spacing and a range of scattering vectors of almost three orders of magnitude are reached by using a large-area high-resolution CCD-based detector for simultaneous SAXS/WAXS. The instrument is particularly suited for scanning SAXS/WAXS/XRF experiments on hierarchically structured biological tissues. The necessary infrastructure, such as a cryo-stream facility and an on-site preparation laboratory for biological specimens, are available. KW - Scanning SAXS KW - Scanning WAXS KW - Microbeam KW - Synchrotron radiation PY - 2007 SN - 0021-8898 SN - 1600-5767 VL - 40 IS - Supplement SP - s466 EP - s470 PB - Blackwell CY - Oxford AN - OPUS4-15049 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Polte, Jörg A1 - Kraehnert, R. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Thünemann, Andreas A1 - Emmerling, Franziska T1 - New insights of the nucleation and growth process of gold nanoparticles via in situ coupling of SAXS and XANES N2 - Although metallic nanoparticles play an important role in the area of nanotechnology, a coherent mechanistic explanation for the evolution of the particles during their chemical synthesis has not yet been provided in many cases. To gain a profound understanding of the growth mechanism of colloidal nanoparticles, new approaches using Small Angle X-Ray Scattering (SAXS) combined with X-ray absorption near-edge structure (XANES) are presented. This combination allows for insights into two prominent syntheses routes of gold nanoparticles (GNP): The 'slow' reaction using sodium citrate (30-90 min) as a reducing agent and the 'fast' reaction employing NaBH4 (within few seconds). In the first case data derived with the coupled XANES and SAXS suggests a four-step particle formation mechanism. For the second system a time resolution in the order of 100-200 ms was achieved by coupling a common laboratory SAXS instrument with a microstructured mixer, which allows data acquisition in a continuous-flow mode. The results indicate a coalescence driven growth process. Based on the capabilities to deduce the size, number and polydispersity of the particles, the results of both methods enable the development of mechanistic schemes explaining the different phases of particle formation and growth, thus providing a basis for improved control over the synthesis processes. KW - SAXS KW - XANES KW - Nanoparticle formation PY - 2010 DO - https://doi.org/10.1088/1742-6596/247/1/012051 SN - 1742-6588 SN - 1742-6596 VL - 247 IS - 1 SP - 012051-1 - 012051-10 PB - IOP Publ. CY - Bristol, UK AN - OPUS4-22684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -