TY - JOUR A1 - Maier, W. A1 - Arlt, Tobias A1 - Wannek, C. A1 - Manke, I. A1 - Riesemeier, Heinrich A1 - Krüger, P. A1 - Scholta, J. A1 - Lehnert, W. A1 - Banhart, J. A1 - Stolten, D. T1 - In-situ synchrotron X-ray radiography on high temperature polymer electrolyte fuel cells N2 - In contrast to classical low temperature polymer electrolyte fuel cells (LT-PEFCs), the membrane conductivity in high temperature polymer electrolyte fuel cells (HT-PEFCs) (operating temperature ~ 160 °C) is based on proton transport within phosphorus-oxygen acids at different levels of hydration, orthophosphoric acid (H3PO4) being the simplest example. We present for the first time in-situ synchrotron X-ray radiography measurements applied to a HT-PEFC to gain insight into the local composition of the membrane electrode assembly (MEA) under dynamic operating conditions. Transmission changes during the radiographic measurements exhibit a clear influence of the formation of product water on the membrane composition. KW - HT-PEFC KW - Synchrotron x-ray radiography KW - Membrane electrode assembly (MEA) KW - Phosphoric acid PY - 2010 DO - https://doi.org/10.1016/j.elecom.2010.08.002 SN - 1388-2481 VL - 12 IS - 10 SP - 1436 EP - 1438 PB - Elsevier CY - Amsterdam AN - OPUS4-23962 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schulz, Eduard A1 - Erhard, Anton A1 - Heinrich, W. A1 - Mohr, F. T1 - Nachqualifikation einer Wasserreibbremse mit Ultraschall N2 - Neu entwickelte Gasturbinen werden im Prüffeld mit wechselnden Belastungen beaufschlagt. Dazu wird die Gasturbine mit einer Wasserreibbremse gekoppelt, mit der eine definierte Last erzeugt werden kann. Ursprünglich war die Wasserreibbremse für eine bestimmte Leistung, die den früheren Leistungen der Gasturbine entsprach, ausgelegt worden. Die erste Prüfung fand im Jahr 1975 statt. Da neuere Gasturbinen wesentlich höhere Leistungen erbringen und die vorhandene Wasserreibbremse weiterhin eingesetzt werden sollte, musste eine Nachqualifizierung vorgenommen werden. Das Ziel war die Absicherung auf eine mögliche Sprödbruchgefahr. Zunächst wurde eine Studie zur Prüfbarkeit erstellt. An speziellen Testkörpern wurden im Ultraschallabor der BAM Vorversuche zur Machbarkeit, zur Empfindlichkeitsein-stellung und zur Vorbereitung der Prüfung durchgeführt. Dazu wurden spezielle Gruppenstrahlerprüfköpfe gefertigt und ein an die komplizierte Geometrie der Bremsscheiben angepasster Manipulator gebaut. Ferner wurde, um die Prüfzeiten zu reduzieren, die Software zur Datenerfassung und zur Auswertung angepasst. Im Werk Berlin der Siemens AG wurde in Zusammenarbeit mit der Siemens AG Erlangen eine Ultraschallprüfung mit der Gruppenstahlertechnik der Wasserreibbremse durchgeführt. Überprüft wurde das gesamte Volumen auf axial, radial und tangential beanspruchte Fehler in den Bereichen der Welle und der Bremsscheibe.Die Überprüfung ergab keine relevanten Fehler, so dass die Wasserreibbremse weiterhin eingesetzt werden kann. T2 - Jahrestagung Zerstörungsfreie Materialprüfung 2000 CY - Innsbruck, Österreich DA - 2000-05-29 PY - 2000 UR - http://www.ndt.net/abstract/dgzfp00/data/79.htm SN - 3-931381-32-3 VL - 73 IS - 2 SP - 1(?) EP - 7(?) PB - DGZfP CY - Berlin AN - OPUS4-940 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinrich, F. A1 - Schmidt, C. A1 - Löffler, E. A1 - Menzel, Michael A1 - Grünert, W. T1 - Fe-ZSM-5 Catalysts for the Selective Reduction of NO by Isobutane - The Problem of the Active Sites N2 - Relations between the structure of Fe–ZSM-5 catalysts prepared by interaction of FeCl3 with H–ZSM-5 and their catalytic behavior in the SCR of NO by isobutane were investigated by combining results of catalytic studies (1000 ppm NO, 1000 ppm isobutane, and 2% O2 in He, 30,000 h-1) and of physicochemical characterization (XRD, EXAFS, Mössbauer spectroscopy, TPR, IR, XPS). By variation of the preparation conditions (method of FeCl3 introduction—chemical vapor deposition or solid-state ion exchange, washing intensity, calcination regime) and of the matrix (H–ZSM-5 with normal and high defect density), Fe–ZSM-5 materials with strongly varying properties (aggregation degree of the Fe phase, acidity) were obtained. Significant discrepancies between conclusions derived from EXAFS, TPR, and Mössbauer spectroscopy were ascribed to a preference of Mössbauer spectroscopy for the detection of aggregated phases and a high defectivity of Fe oxide clusters formed upon calcination. The critical step for the preparation of a highly disperse Fe phase is extensive washing after Fe introduction. The catalytic behavior of overexchanged Fe–ZSM-5 materials prepared by interaction of FeCl3 with H–ZSM-5 of normal defect density was not influenced by aggregation of a significant part of the Fe phase. The comparison of their catalytic properties with those of a Fe2O3/H–ZSM-5 mechanical mixture and of catalysts prepared by aqueous ion exchange or by CVD of FeCl3 into H–ZSM-5 of high defect density implies that the particular activity of overexchanged Fe–ZSM-5 arises from minority sites. In these, the Fe ions are probably isolated. Other Fe sites of low nuclearity appear to add to the activity. The poor SCR performance (at a given ability for isobutane activation) of Fe–ZSM-5 prepared with a defective ZSM-5 matrix may indicate that the Fe sites which provi de the particular activity of overexchanged Fe–ZSM-5 require the cooperation of acidic sites. KW - deNOx KW - Hydrocarbons KW - Isobutane KW - Fe-ZSM-5 KW - EXAFS KW - Mössbauer spectroscopy KW - Temperature-programmed reduction PY - 2002 DO - https://doi.org/10.1006/jcat.2002.3775 SN - 0021-9517 SN - 1090-2694 VL - 212 SP - 157 EP - 172 PB - Acad. Press CY - San Diego, Calif. AN - OPUS4-2258 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Bernd R. A1 - Görner, Wolf A1 - Hentschel, Manfred P. A1 - Riesemeier, Heinrich A1 - Krumrey, M. A1 - Ulm, G. A1 - Diete, W. A1 - Klein, U. A1 - Frahm, R. T1 - BAMlin - the first hard X-ray beamline at BESSY II N2 - The first hard X-ray beamline at BESSY II will be 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. The two devices can be used separately or in-line. Main applications of monochromatic radiation with photon energies up to 50 keV are X-ray fluorescence analysis, micro-computed tomography, X-ray topography, detector calibration and reflectometry. Calculable undispersed radiation up to 200 keV will be available for radiometric applications. KW - Double-Multilayer-Monochromator with meridional bender KW - Double-Crystal-Monochromator with sagittal bender KW - X-ray fluorescence analysis KW - Micro-computed tomography KW - X-ray topography KW - Detector calibration KW - Reflectometry PY - 2001 DO - https://doi.org/10.1016/S0168-9002(01)00466-1 SN - 0168-9002 SN - 0167-5087 VL - 467-468 IS - 1 SP - 703 EP - 706 PB - North-Holland CY - Amsterdam AN - OPUS4-1171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Treimer, W. A1 - Feye–Treimer, U. A1 - Radke, C. A1 - Hilger, A. A1 - Neumann, O. A1 - Manke, I. A1 - Haibel, A. A1 - Rack, A. A1 - Riesemeier, Heinrich T1 - Investigations of mamma biopsies by means of µ-tomography PY - 2005 UR - http://www.helmholtz-berlin.de/media/media/oea/web/pr_webseite/druckschriften/berichte/bessy/annualreport2004.pdf#page=452 SN - 0179-4159 SP - 452 EP - 453 PB - Berliner Elektronenspeicherring-Gesellschaft für Synchrotronstrahlung CY - Berlin AN - OPUS4-7383 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rienitz, O. A1 - Jährling, R. A1 - Schiel, D. A1 - Matschat, Ralf A1 - Kipphardt, Heinrich A1 - Gernand, W. A1 - Oeter, D. T1 - Rückführung in der Elementanalytik PY - 2005 SN - 0030-834X VL - 115 IS - 4 SP - 295 EP - 299 PB - Wirtschaftsverl. NW CY - Bremerhaven AN - OPUS4-12056 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, G. A1 - Nellesen, J. A1 - Anar, N. B. A1 - Ehrig, Karsten A1 - Riesemeier, Heinrich A1 - Tillmann, W. T1 - 3D analysis of micro-deformation in VHCF-loaded nodular cast iron by µCT N2 - The impact of very high cycle fatigue (VHCF) load conditions on the microstructure of specimens consisting of nodular cast iron is analyzed by means of micro-computed tomography (µCT) utilizing both monochromatic synchrotron radiation and polychromatic X-ray tube radiation. Using 3D µCT, the microstructure in the region of the smallest cross-sections of shouldered round specimens is imaged in different stages of the VHCF loading. By digital image correlation (DIC) of these tomograms strain fields are analyzed three-dimensionally. Strain levels in the range of a few percent were detected. It is proven that a localization of strain allows to predict the site of the crack which precedes and induces the macroscopic failure of the specimens. KW - VHCF (very high cycle fatigue) KW - µCT KW - Micro-computed tomography KW - Strain analysis KW - Nodular cast iron PY - 2013 DO - https://doi.org/10.1016/j.msea.2013.04.057 SN - 0921-5093 SN - 1873-4936 VL - 577 SP - 202 EP - 209 PB - Elsevier CY - Amsterdam AN - OPUS4-28533 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Boehm, Rainer A1 - Brackrock, Daniel A1 - Kitze, Jessica A1 - Brekow, Gerhard A1 - Kreutzbruck, Marc A1 - Heinrich, W. T1 - Ultraschalluntersuchungen an einem Turbinenradscheibentestkörper mit Sägezahn-Arrays N2 - - Besondere Anforderungen der Prüfaufgabe - Elektronischer Scan für Tandemtechnik bzw. Pitch - Catch Technik - Der ebene Winkelprüfkopf, ein besonderer Gruppenstrahler (PA) - Charakterisierung des Prüfkopfes, Verifikation durch Messung - Messungen am Turbinenradscheibentestkörper T2 - DGZfP-Jahrestagung 2011 CY - Bremen, Germany DA - 30.05.2011 KW - Ultraschallprüftechnik KW - Phased array KW - Prüfkopfentwicklung KW - Turbinenradscheiben PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-252085 SN - 978-3-940283-33-7 IS - DGZfP-BB 127 (Di.1.A.3) SP - 1 EP - 21 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) AN - OPUS4-25208 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koenen, Heinrich A1 - Ide, Karl-Heinz A1 - Haupt, W. T1 - Über die Prüfung explosiver Stoffe - IV. Ermittlung der Schlagempfindlichkeit explosivr Stoffe von fester, flüssiger und gelantinöser Beschaffenheit - On the Testing of Explosive Matters - Sur l'examen de matières explosives - Sobre el ensayo de materias explosivas PY - 1958 SN - 0014-505X SN - 0014-5068 VL - 46 IS - 8 SP - 178 EP - 179 PB - Barth CY - Neustadt, Weinstr. AN - OPUS4-7783 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koenen, Heinrich A1 - Ide, Karl-Heinz A1 - Haupt, W. T1 - Über die Prüfung explosiver Stoffe - IV. Ermittlung der Schlagempfindlichkeit explosivr Stoffe von fester, flüssiger und gelantinöser Beschaffenheit - On the Testing of Explosive Matters - Sur l'examen de matières explosives - Sobre el ensayo de materias explosivas - Fortsetzung PY - 1958 SN - 0014-505X SN - 0014-5068 VL - 46 IS - 9 SP - 202 EP - 214 PB - Barth CY - Neustadt, Weinstr. AN - OPUS4-7784 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koenen, Heinrich A1 - Ide, Karl-Heinz A1 - Haupt, W. T1 - Über die Prüfung explosiver Stoffe - IV. Ermittlung der Schlagempfindlichkeit explosivr Stoffe von fester, flüssiger und gelantinöser Beschaffenheit - On the Testing of Explosive Matters - Sur l'examen de matières explosives - Sobre el ensayo de materias explosivas - Fortsetzung PY - 1958 SN - 0014-505X SN - 0014-5068 VL - 46 IS - 10 SP - 223 EP - 235 PB - Barth CY - Neustadt, Weinstr. AN - OPUS4-7785 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tonn, W. A1 - Günther, Heinrich T1 - Beitrag zur Gebrauchsprüfung von Zinn-Bleiloten PY - 1936 IS - 28 SP - 117 EP - 119 PB - Springer CY - Berlin AN - OPUS4-16891 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kipphardt, Heinrich A1 - Matschat, Ralf A1 - Rienitz, O. A1 - Schiel, D. A1 - Gernand, W. A1 - Oeter, D. T1 - Traceability system for elemental analysis N2 - A complete metrological traceability system for measurement results of chemical analysis was set up. Core components are pure substances (national standards) characterised at the highest metrological level, primary solutions prepared from these pure substances and secondary solutions deduced from the primary solutions and intended for sale. The relative uncertainty of the element mass fraction of the primary substances and solutions is < 0.01 and < 0.05%, respectively. For the certification of transfer solutions and for stability testing, a precision measurement method for element contents has been developed by means of optical emission spectrometry (ICP OES) by which uncertainties between 0.1 and 0.05% can be achieved. The dissemination to field laboratories is effected with the aid of a calibration laboratory of the German Calibration Service (DKD) which certifies the element content of the secondary solutions with an uncertainty <= 0.3%. Calibration with these solutions enables the user to establish traceability of his measurement results to the International System of Units (SI). Currently, the system comprises Cu, Fe, Bi, Ga, Si, Na, K, Sn, W, and Pb. KW - Elemental analysis KW - Traceability KW - Elemental calibration solutions KW - Pure substances KW - Precision measurement of elements PY - 2006 DO - https://doi.org/10.1007/s00769-005-0084-6 SN - 0949-1775 SN - 1432-0517 VL - 10 IS - 11 SP - 633 EP - 639 PB - Springer CY - Berlin AN - OPUS4-12199 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mooshofer, H. A1 - Boehm, Rainer A1 - Heinrich, W. A1 - Fendt, K. A1 - Goldammer, M. A1 - Kolk, K. A1 - Vrana, J. T1 - Amplitudenbasierte Fehlergrößenbewertung mit SAFT: Auf dem Weg von der bildlichen Darstellung zum Messverfahren N2 - Die Größenbewertung von Anzeigen und die Bestimmung der Nachweisgrenze spielen bei der Ultraschallprüfung eine zentrale Rolle: Sie stellen sicher, dass kritische Ungänzen erfasst und bruchmechanisch behandelt werden können. Bei SAFT wurde bisher die Größe von Ungänzen dadurch bestimmt, dass die räumliche Anzeigenausdehnung im Rekonstruktionsergebnis ausgewertet wird, d.h. die Anzahl von Voxel über die sich eine Anzeige erstreckt. Auf diese Weise lassen sich jedoch nur Defektanzeigen bewerten, die größer oder gleich der Wellenlänge sind. Bei kleinen Defekten versagt diese Methode, d.h. es ist keine Größenbewertung möglich. Außerdem bietet diese Methode keine Aussage über die Nachweisgrenze des Verfahrens. Ein Hauptvorteil von SAFT gegenüber der konventionellen Ultraschallprüfung ist aber gerade die Verbesserung der Nachweisgrenze, denn SAFT steigert das Signal-Rausch-Verhältnis (SNR) gegenüber dem Gefügerauschen und reduziert statistisches Rauschen. Um diesen Hauptvorteil nutzen (und quantifizieren) zu können, wird für SAFT eine Methode zur Nachweisgrenzenbestimmung und zur Größenbewertung der Anzeigen kleiner Ungänzen benötigt. Neben ihrer räumlichen Ausdehnung lassen sich Anzeigen im SAFT-Ergebnis auch durch ihre Amplitude charakterisieren, wenn die Prüfkopfeigenschaften und die geometrischen Verhältnisse beim Scan berücksichtigt werden. Genauer gesagt durch die Amplitudensumme, in die - neben der Echoamplitude - auch die winkelabhängige Streucharakteristik eingeht. Im Folgenden wird dargelegt, dass sich die Amplitudensumme zur Nachweisgrenzenbestimmung und zur Größenbewertung kleiner Ungänzen eignet. Es wird der Zusammenhang zwischen der Amplitudensumme und der Größe von Ungänzen dargestellt, und es wird gezeigt, dass auch die Anzeigenposition und die Form des Prüfobjektes eine Rolle spielen können. Auf dieser Basis wird eine Methode zur Größenbestimmung kleiner Anzeigen im SAFT-Ergebnis entwickelt. Damit lässt sich das SAFT-Ergebnis als Ersatzfehlergröße darstellen, so wie das bei konventioneller Ultraschallprüfung z.B. mit Hilfe von AVG-Diagrammen erfolgt. Durch die Vervollständigung um die Größenbewertung ist SAFT nicht mehr nur ein bildgebendes Verfahren, sondern es kann vielmehr als vollwertiges Messverfahren dienen. T2 - DGZfP-Jahrestagung 2017 CY - Koblenz, Germany DA - 22.05.2017 KW - Synthetic aperture focussing technique (SAFT) KW - Defektgrößenbewertung KW - Gewichtete Amplitudensumme KW - Kleine Reflektoren PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-411571 SN - 978-3-940283-85-6 VL - 162 SP - 1 EP - 9 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-41157 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gonzales-Gago, C. A1 - Smid, P. A1 - Hofmann, T. A1 - Venzago, C. A1 - Hoffmann, V. A1 - Gruner, W. A1 - Pfeifer, Jens A1 - Richter, Silke A1 - Kipphardt, Heinrich T1 - Investigations of matrix independent calibration approaches in fast flow glow discharge mass spectrometry N2 - The performance of glow discharge mass spectrometry (GD-MS) is investigated for the accurate quantification of metallic impurities and oxygen in solid samples using the fast flow source GD-MS instrument ELEMENT GD. Different quantification approaches based on relative and absolute sensitivity factors are evaluated for the determination of metallic impurities using three sample matrixes (Al, Cu and Zn). The effect of the discharge conditions (voltage, current, discharge gas pressure/flow) on the sensitivity is investigated and the parameters are optimized to favour matrix independent calibrations. Improved standard relative sensitivity factors (StdRSFs) are calculated under optimal conditions based on multi-matrix calibrations. The sputtering rate corrected calibration is also presented as a multi-matrix calibration approach. The capabilities of GD-MS for oxygen determination are also investigated using a set of new conductive samples containing oxygen with mass fractions in the percent range in three different matrices (Al, Mg and Cu) produced by a sintering process. Poor limits of detection (in the order of g/kg) were obtained as consequence of the reduced sensitivity of oxygen in GD-MS and high oxygen background signal intensity as well as its variations. The absolute sensitivity procedure is shown as a matrix-independent approach, which provides quantitative values consistent with those obtained by carrier gas hot extraction (CGHE). KW - Fast flow GD KW - GDMS KW - Calibration KW - Matrix independent calibration PY - 2019 DO - https://doi.org/10.1039/c9ja00023b SN - 1364-5544 SN - 0267-9477 VL - 34 IS - 6 SP - 1109 EP - 1125 PB - Royal Society of Chemistry CY - London AN - OPUS4-47842 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - van der Hout, J. W. A1 - van der Veen, A. M. H. A1 - Ziel, P. R. A1 - Kipphardt, Heinrich A1 - Tuma, Dirk A1 - Maiwald, Michael A1 - Fernández, T. E. A1 - Gómez, C. A1 - Cieciora, D. A1 - Ochman, G. A1 - Dias, F. A1 - Silvino, V. A1 - Macé, T. A1 - Sutour, C. A1 - Marioni, F. A1 - Ackermann, A. A1 - Niederhauser, B. A1 - Fükő, J. A1 - Büki, T. A1 - Szilágyi, Z. N. A1 - Tarhan, T. A1 - Engin, E. T1 - International Comparison Euramet.QM-K111 – Propane in Nitrogen N2 - This key comparison aims to assess the core capabilities of the participants in gas analysis. Such competences include, among others, the capabilities to prepare Primary Standard gas Mixtures (PSMs), perform the necessary purity analysis on the materials used in the gas mixture preparation, the verification of the composition of newly prepared PSMs against existing ones, and the capability of calibrating the composition of a gas mixture. According to the Strategy for Key Comparisons of the Gas Analysis Working Group, this key comparison is classified as an RMO track A key comparison. The artefacts were binary mixtures of propane in nitrogen at a nominal amount-of-substance fraction level of 1000 μmol/mol. The values and uncertainties from the gravimetric gas mixture preparation were used as key comparison reference values (KCRVs). Each transfer standard had its own KCRV. The results are generally good. All results are within ± 1 % of the KCRV. KW - EURAMET.QM-K111 KW - Propane in nitrogen PY - 2017 DO - https://doi.org/10.1088/0026-1394/54/1A/08020 SN - 0026-1394 VL - 54 IS - Technical Supplement SP - 08020, 1 EP - 34 PB - IOP Science AN - OPUS4-44471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Anja A1 - Heinrich, Thomas A1 - Tougaard, S. A1 - Werner, W. S. M. A1 - Hronek, M. A1 - Kunz, Valentin A1 - Radnik, Jörg A1 - Stockmann, Jörg M. A1 - Hodoroaba, Vasile-Dan A1 - Benemann, Sigrid A1 - Nirmalananthan-Budau, Nithiya A1 - Geißler, Daniel A1 - Sparnacci, K. A1 - Unger, Wolfgang T1 - Determining the thickness and completeness of the shell of polymer core-shell nanoparticles by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and transmission scanning electron microscopy N2 - Core–shell nanoparticles (CSNPs) have become indispensable in various industrial applications. However, their real internal structure usually deviates from an ideal core–shell structure. To control how the particles perform with regard to their specific applications, characterization techniques are required that can distinguish an ideal from a nonideal morphology. In this work, we investigated poly(tetrafluoroethylene)–poly(methyl methacrylate) (PTFE–PMMA) and poly(tetrafluoroethylene)–polystyrene (PTFE–PS) polymer CSNPs with a constant core diameter (45 nm) but varying shell thicknesses (4–50 nm). As confirmed by transmission scanning electron microscopy (T-SEM), the shell completely covers the core for the PTFE–PMMA nanoparticles, while the encapsulation of the core by the shell material is incomplete for the PTFE–PS nanoparticles. X-ray photoelectron spectroscopy (XPS) was applied to determine the shell thickness of the nanoparticles. The software SESSA v2.0 was used to analyze the intensities of the elastic peaks, and the QUASES software package was employed to evaluate the shape of the inelastic background in the XPS survey spectra. For the first time, nanoparticle shell thicknesses are presented, which are exclusively based on the analysis of the XPS inelastic background. Furthermore, principal component analysis (PCA)-assisted time-of-flight secondary-ion mass spectrometry (ToF-SIMS) of the PTFE–PS nanoparticle sample set revealed a systematic variation among the samples and, thus, confirmed the incomplete encapsulation of the core by the shell material. As opposed to that, no variation is observed in the PCA score plots of the PTFE–PMMA nanoparticle sample set. Consequently, the complete coverage of the core by the shell material is proved by ToF-SIMS with a certainty that cannot be achieved by XPS and T-SEM. KW - XPS KW - T-SEM KW - ToF-SIMS KW - Core-shell nanoparticles PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-499165 DO - https://doi.org/10.1021/acs.jpcc.9b09258 VL - 123 IS - 49 SP - 29765 EP - 29775 PB - American Chemical Society CY - Washington, DC AN - OPUS4-49916 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Müller, Anja A1 - Heinrich, Thomas A1 - Tougaard, S. A1 - Werner, W. S. M. A1 - Hronek, M. A1 - Kunz, Valentin A1 - Radnik, Jörg A1 - Stockmann, Jörg M. A1 - Hodoroaba, Vasile-Dan A1 - Benemann, Sigrid A1 - Nirmalananthan-Budau, Nithiya A1 - Geißler, Daniel A1 - Sparnacci, K. A1 - Unger, Wolfgang T1 - Correction to "Determining the thickness and completeness of the shell of polymer core-shell nanoparticles by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and transmission scanning electron microscopy" N2 - This is a corrigendum to the original article "Determining the thickness and completeness of the shell of polymer core-shell nanoparticles by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and transmission scanning electron microscopy" that was published in "The journal of physical chemistry C", vol. 123 (2019), no. 49 pp. 29765-29775. PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505451 DO - https://doi.org/10.1021/acs.jpcc.0c00027 SN - 1932-7447 SN - 1932-7455 VL - 124 IS - 6 SP - 3923 PB - American Chemical Society CY - Washington, DC AN - OPUS4-50545 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 - 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 -