TY - JOUR A1 - Kraehnert, R. A1 - Ortel, Erik A1 - Paul, B. A1 - Eckhardt, B. A1 - Kanis, M. A1 - Liu, R. A1 - Antoniou, A. T1 - Electrochemically dealloyed platinum with hierarchical pore structure as highly active catalytic coating N2 - Micro structured reactors are attractive candidates for further process intensification in heterogeneous catalysis. However, they require catalytic coatings with significantly improved space-time yields compared to traditional supported catalysts. We report the facile synthesis of homogeneous nanocrystalline Pt coatings with hierarchical pore structure by electrochemical dealloying of amorphous sputter-deposited platinum silicide layers. Thickness, porosity and surface composition of the catalysts can be controlled by the dealloying procedure. XPS analysis indicates that the catalyst surface is primarily composed of metallic Pt. Catalytic tests in gas-phase hydrogenation of butadiene reveal the typical activity, selectivity and activation energy of nanocrystalline platinum. However, space time yields are about 13 to 200 times higher than values reported for Pt-based catalysts in literature. The highly open metallic pore structure prevents heat and mass transport limitations allowing for very fast reactions and reasonable stability at elevated temperatures. KW - Pt catalysts KW - Pt–Si layers KW - Scanning Electron Microscopy (SEM) KW - Transmission Electron Microscopy (TEM) KW - pore structure KW - electrochemical dealloying PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-351393 DO - https://doi.org/10.1039/C4CY00851K SN - 2044-4753 SN - 2044-4761 VL - 5 IS - 1 SP - 206 EP - 216 PB - RSC Publ. CY - Cambridge AN - OPUS4-35139 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hemmann, Felix A1 - Agirrezabal-Telleria, Iker A1 - Jäger, Christian A1 - Kemnitz, E. T1 - Quantification of acidic sites of nanoscopic hydroxylated magnesium fluorides by FTIR and 15N MAS NMR spectroscopy N2 - Lewis and Brønsted sites were quantified in a series of weak acidic hydroxylated magnesium fluorides by Fourier transform infrared spectroscopy (FTIR) and solid state nuclear magnetic resonance spectroscopy (NMR) with pyridine as probe molecule. Molar extinction coefficients, which are necessary for quantitative FTIR measurements, were calculated by an easy approach. It utilizes the fact that both signals, used for the quantification by FTIR, are caused by the same deformation vibration mode of pyridine. Comparison of quantitative FTIR experiments and quantification by NMR shows that concentrations of acidic sites determined by FTIR spectroscopy have to be interpreted with caution. Furthermore, it is shown that the transfer of molar extinction coefficients from one catalyst to another may lead to wrong results. Molar extinction coefficients and concentrations of acidic sites determined by FTIR spectroscopy are affected by grinding and probably the particle size of the sample. High temperature during FTIR experiments has further impact on the quantification results. KW - Acidity KW - Fluoride catalyst KW - Infrared spectroscopy KW - Adsorption of pyridine KW - Molar extinction coefficient determination PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-351448 DO - https://doi.org/10.1039/C5RA15116C SN - 2046-2069 VL - 5 IS - 109 SP - 89659 EP - 89668 PB - RSC Publishing CY - London AN - OPUS4-35144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nguyen, Thi Yen A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Direct evidence of polyamorphism in paracetamol N2 - While polymorphism is a common phenomenon in the crystallization processes of organic compounds, polyamorphism has gained importance only recently. Using sophisticated sample environments and applying in situ scattering methods and vibrational spectroscopy, the complete crystallization process of organic compounds from solution can be traced and characterized. Diffuse scattering from amorphous intermediates can be investigated by analyzing the atomic pair distribution function (PDF) to gain further insights into molecular pre-orientation. The crystallization behavior of paracetamol was studied exemplarily under defined, surface-free conditions. Based on the choice of the solvent, the formation of different polymorphs is promoted. The thermodynamically stable form I and the metastable orthorhombic form II could be isolated in pure form directly from solution. For both polymorphs, the crystallization from solution proceeds via a distinct amorphous precursor phase. PDF analyses of these different amorphous states indicate a specific pre-orientation of the analyte molecules introduced by the solvent. The resulting crystalline polymorph is already imprinted in these proto-crystalline precursors. Direct experimental evidence for the polyamorphism of paracetamol is provided. PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-351366 DO - https://doi.org/10.1039/C5CE01583A SN - 1466-8033 VL - 17 IS - 47 SP - 9029 EP - 9036 PB - Royal Society of Chemistry CY - London, UK AN - OPUS4-35136 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten A1 - Gollwitzer, Christian A1 - Fratzscher, Daniel A1 - Ewert, Uwe A1 - Jaenisch, Gerd-Rüdiger T1 - Simulation of complex scan paths for 3D reconstruction N2 - X-ray computed tomography (CT) is a volumetric (3D) Imaging diagnostic method, well established in the medical field, and in industrial NDE as well. Developments in industrial CT aim to extent the applicability to complex structures, which do not allow the access of all directions. This are e.g. limited view, data and angle CT applications. New reconstruction algorithms are required on one side, and the accuracy has to be improved on the other side. Numerical Simulation can support such developments by providing well defined data sets for the testing of reconstruction algorithms. This approach of virtual CT is realized within the radiographic simulator aRTist, developed by BAM. The poster shows the possibilities of this tool to consider complex scan paths. Simulated data sets have been reconstructed by an versatile backprojection algorithm. T2 - International symposium on digital industrial radiology and computed tomography CY - Berlin, Germany DA - 20.06.2011 KW - Radiographie KW - Computer-Simulation KW - 3D-Rekonstruktion PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-243928 SN - 978-3-940283-34-4 IS - DGZfP-BB 128 (Poster 17) SP - 1 EP - 4 PB - Deutsche Gesellschaft für zerstörungsfreie Prüfung e.V. (DGZfP) AN - OPUS4-24392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abbott, A. P. A1 - Abolibda, T. Z. A1 - Davis, S.J. A1 - Emmerling, Franziska A1 - Lourdin, D. A1 - Leroy, E. A1 - Wise, W. R. T1 - Glycol based plasticisers for salt modified starch N2 - Starch is one of the most common and easily obtained natural polymers, making it attractive as a potential bio-based alternative to synthetic polymers. This study shows that a simple quaternary ammonium salt combined with urea or glycols forms effective modifiers that produce flexible plastics with good mechanical properties that are comparable to some polyolefin plastics. The processing conditions are shown to significantly affect the structure of the polymer which has a concomitant effect upon the mechanical and physical properties of the resulting plastic. Using a glycerol based modifier results in a totally sustainable and biodegradable material which can be injection moulded. KW - biodegradable material KW - flexible plastics KW - injection moulded PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-351426 DO - https://doi.org/10.1039/C4RA06220E SN - 2046-2069 VL - 4 IS - 76 SP - 40421 EP - 40427 PB - RSC Publishing CY - London AN - OPUS4-35142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gollwitzer, Christian A1 - Bellon, Carsten A1 - Deresch, Andreas A1 - Ewert, Uwe A1 - Jaenisch, Gerd-Rüdiger T1 - On POD estimations with radiographic simulator aRTist N2 - The computer simulation of radiography is applicable for different purposes in NDT such as for the qualification of NDT systems, the optimization of system parameters, feasibility analysis, model-based data interpretation, education and training of NDT/NDE personnel, and others. Within the framework of the European project PICASSO simulators will be adapted to support reliability assessments of NDT tasks. The radiographic simulator aRTist developed by BAM is well suited for this task. It combines analytical modelling of the RT inspection process with the CAD-orientated object description applicable to various industrial sectors such as power generation, aerospace, railways and others. The analytic model includes the description of the radiation source, the interaction of Radiation with the material of the part, and the detection process with special focus to DIR. To support reliability estimations the simulation tool is completed by a tool for probability of detection (POD) estimation. It consists of a user interface for planning automatic simulation runs with varying parameters, specifically defect variations. Further, an automatic image analysis procedure is included to evaluate the defect visibility and calculate the POD therefrom. T2 - International symposium on digital industrial radiology and computed tomography CY - Berlin, Germany DA - 20.06.2011 KW - Radiographie KW - Computersimulation KW - Probability of detection PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-245092 SN - 978-3-940283-34-4 IS - DGZfP-BB 128 (Tu.2.3) SP - 1 EP - 8 PB - Deutsche Gesellschaft für zerstörungsfreie Prüfung e.V. (DGZfP) AN - OPUS4-24509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sötebier, Carina A. A1 - Kutscher, D. J. A1 - Rottmann, L. A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Bettmer, J. T1 - Combination of single particle ICP-QMS and isotope dilution analysis for the determination of size, particle number and number size distribution of silver nanoparticles N2 - Single particle ICP-MS (spICP-MS) has gained great influence in the analysis of engineered nanoparticles (NPs) due to its simplicity, speed and ability to obtain a particle number size distribution. Despite its many advantages, the method is hampered by matrix effects affecting the sensitivity of the instruments. Consequently, over- or underestimated particle sizes might be obtained. To overcome these challenges, we present in this work the detection of both Ag isotopes with a quadrupole mass spectrometer for the application of isotopic dilution analysis (IDA) in combination with spICP-MS. Here, the isotopes are measured sequentially using the conventional spICP-MS integration time of 10 ms. Citrate stabilized Ag NPs of a spherical shape with the nominal diameters of 30, 40, 50 and 80 nm have been investigated. The experimental concept of adding ¹⁰⁹Ag+ solutions to the NP suspensions resulted in the NP Spikes being only visible in the ¹⁰⁷Ag trace. Therefore, a maximum of 45% of the particles was detected compared to that by conventional spICP-MS. A modified mass flow equation was applied to determine the particle sizes, particle size distributions and particle number concentrations of various Ag NPs. The addition of different spike concentrations between 0.5 and 4 mg L⁻¹ ¹⁰⁹Ag resulted in similar particle diameters, suggesting that the calculated diameter might be independent of the spike concentration. This would have the advantage that no size information would be needed before the analysis. By analyzing Ag NP suspensions in a simulated seawater matrix, we demonstrate its significant influence on the particle size determination using conventional spICP-MS. A lower transport efficiency of 6.1% was found in the matrix compared to 7.3% without the matrix. In our approach, the addition of the Matrix influenced the NP intensity stronger than the spike signal, resulting in slightly smaller diameters using IDA–spICP-MS with the matrix compared to the results without the matrix. On the other hand, the IDA–spICP-MS approach with the matrix can result in equivalent results for the particle sizes compared with conventional spICP-MS using suspensions without the matrix. Due to the lower instrument sensitivity in the matrix, a diameter of 30 nm was found to be close to the detection limit of the instrument. KW - Ag nanoparticles KW - Single particle ICP-MS KW - Matrix influence KW - Isotope dilution analysis PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-376490 DO - https://doi.org/10.1039/c6ja00137h SN - 0267-9477 VL - 31 IS - 10 SP - 2045 EP - 2052 AN - OPUS4-37649 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neubert, Sebastian A1 - Pittner, Andreas A1 - Rethmeier, Michael T1 - Experimental determination of TRIP parameter K for mild- and high strength low alloy steels and a super martensitic filler material N2 - A combined experimental numerical approach is applied to determine the transformation induced plasticity (TRIP)-parameter K for different strength low-alloy steels of grade S355J2+N and S960QL as well as the super martensitic filler CN13-4-IG containing 13 wt% chromium and 4 wt% nickel. The thermo-physical analyses were conducted using a Gleeble® 3500 facility. The thermal histories of the specimens to be tested were extracted from corresponding simulations of a real gas metal arc weldment. In contrast to common TRIP-experiments which are based on complex specimens a simple flat specimen was utilized together with an engineering evaluation method. The evaluation method was validated with literature values for the TRIP-parameter. It could be shown that the proposed approach enables a correct description of the TRIP behavior. KW - Transformation induced plasticity (TRIP) KW - Phase transformation KW - High-strength low-alloy steel KW - Super martensitic filler material KW - Thermo physical simulation KW - Gleeble experiments PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-367297 DO - https://doi.org/10.1186/s40064-016-2474-0 VL - 5 IS - 575 SP - Paper 754, 1 EP - 16 PB - SpringerPlus AN - OPUS4-36729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tölle, Florian A1 - Gumenyuk, Andrey A1 - Gebhardt, Moritz Oliver A1 - Rethmeier, Michael T1 - Post-weld residual stress mitigation by scanning of a defocused laser beam N2 - High welding residual stresses can cause service life reducing consequences. Even though many processes have been developed to reduce these stresses, they are only applicable for wider welds and simple component geometries or are cost-intensive, respectively. The presented method uses a defocused beam after welding for heating the material regions on both sides of the weld. In this way, the welding stresses are decreased without contacting the surfaces using the available equipment. Different process parameters could be used depending on the component geometry and the laser power. The mechanism and the influence of the process parameters were investigated by FEM-simulation and experiments on S355J2+N steel and showed a stress reduction of about 73%. T2 - Lasers in Manufacturing 2011 - Proceedings of the Sixth International WLT Conference on Lasers in Manufacturing CY - Munich, Germany DA - 23.05.2011 KW - Residual stresses KW - Stress reduction KW - High energy beam welding KW - Post-weld heat treatment KW - Laser scanner optics PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-238482 DO - https://doi.org/10.1016/j.phpro.2011.03.052 SN - 1875-3892 VL - 12 IS - 1 SP - 410 EP - 418 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-23848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Osterloh, Kurt A1 - Bellon, Carsten A1 - Hohendorf, Stefan A1 - Kolkoori, Sanjeevareddy A1 - Wrobel, Norma A1 - Nusser, A. A1 - Freitag, M. A1 - Bücherl, T. A1 - Bar, D. A1 - Mor, I. A1 - Tamin, N. A1 - Weiss-Babai, R. A1 - Bromberger, B. A1 - Dangendorf, V. A1 - Tittelmeier, K. T1 - Computed tomography with X-rays and fast neutrons for restoration of wooden artwork N2 - The objects of this investigation were sculptures taken from a ca. three hundred years old baroque epitaph of a church in Tonning, a town in Northern Germany. Around 1900 it was found in a disastrous state heavily damaged by wood-worm. At that time, the whole artwork was treated with the tar extract carbolineum as a remedy. Nowadays, this substance has been identified as carcinogenic, and its presence can be perceived by its stench and visually at certain spots on the surface where it has penetrated the covering paint. A gold-painted sculpture of a massive wooden skull was interrogated with X-rays and fast neutrons to investigate the internal distribution of the carbolineum. The X-ray tomography, with its excellent spatial resolution revealed galleries left over from the worm infestation in the outer areas and cracks in the central region. The golden color coating appeared as a thick and dense layer. In comparison the tomography with fast neutrons, though being of lower resolution and yet unresolved artefacts revealed sections of slightly different densities in the bulk of the wood. These differences we attribute to the differences in the distribution of the impregnant in the wood, visible due to its higher hydrogen content making it less transparent for neutrons. T2 - WCNR-10 - 10th World conference on neutron radiography CY - Grindelwald, Switzerland DA - 05.10.2014 KW - Computed tomography KW - Neutron radiology KW - Conservation of wooden artwork PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-323050 DO - https://doi.org/10.1016/j.phpro.2015.07.066 SN - 1875-3892 VL - 69 SP - 472 EP - 477 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-32305 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -