TY - JOUR A1 - Nolze, Gert T1 - Characterization of the fcc/bcc orientation relationship by EBSD using pole figures and variants N2 - The orientation relationship (OR) between fcc and bcc lattices are described by crystallographic fundamentals using the example of Kurdjumov-Sachs (K-S) and Nishiyama-Wassermann (N-W). Complete pole figures containing all variants will be used to distinguish even between slightly different ORs. EBSD on iron meteorites and duplex steel has been used to analyse a large number of crystal orientations with regard to a high statistical significance and a high probability to capture all variants in a single measurement. It is shown that the use of fixed OR models like K-S, N-W, Bain, Pitsch, or Greninger-Troiano does not satisfacturally reflect the observed experimental pole distributions. It is not convenient to use high-indexed lattice planes and directions to describe the small deviations from the given models. The Euler subspace representation offers a readily comprehensible tool to get an idea about the characteristic of the experimentally detected OR. KW - EBSD KW - Duplex steel KW - Iron meteorite KW - Pole figure KW - Orientation relationship PY - 2004 DO - https://doi.org/10.1515/ijmr-2004-0142 SN - 0044-3093 VL - 95 IS - 9 (85 Jahre DGM) SP - 744 EP - 755 PB - Hanser CY - München AN - OPUS4-13972 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Munz, Martin A1 - Sturm, Heinz T1 - Structure formation on the surface of indium phosphide irradiated by femtosecond laser pulses N2 - Laser-induced periodic surface structures (LIPSS; ripples) with different spatial characteristics have been observed after irradiation of single-crystalline indium phosphide (c-InP) with multiple linearly polarized femtosecond pulses (130 fs, 800 nm) in air. With an increasing number of pulses per spot, N, up to 100, a characteristic evolution of two different types of ripples has been observed, i.e., (i) the growth of a grating perpendicular to the polarization vector consisting of nearly wavelength-sized periodic lines and (ii), in a specific pulse number regime (N = 5-30), the additional formation of equally oriented ripples with a spatial period close to half of the laser wavelength. For pulse numbers higher than 50, the formation of micrometer-spaced grooves has been found, which are oriented perpendicular to the ripples. These topographical surface alterations are discussed in the frame of existing LIPSS theories. KW - Femtosecond laser irradiation KW - Indium phosphide KW - Microstructure KW - Laser induced periodic surface structures KW - LIPSS KW - SEM PY - 2005 DO - https://doi.org/10.1063/1.1827919 SN - 0021-8979 SN - 1089-7550 VL - 97 SP - 1 EP - 9 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-5992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulz, Eckhard A1 - Schulte, K. T1 - Fachausschuss "Gefüge und Eigenschaften von Polymerwerkstoffen" N2 - Die in zunehmenden Maße Mitte der 80er Jahre einsetzende Substitution von metallischen Materialien z. B. durch hochleistungsfähige polymere Werkstoffe und Verbundwerkstoffe wurde u. a. von der DGM zum Anlass genommen, ihre zukünftigen Aufgaben neu zu definieren und gleichzeitig mit der Gründung des Fachausschusses "Gefüge und Eigenschaften von Polymerwerkstoffen" dieser neuen Entwicklung in der Materialkunde auf dem Gebiet der Kunststoffe und ihrer Anwendungen Rechnung zu tragen. KW - Aufgaben KW - Ziele PY - 2004 DO - https://doi.org/10.1515/ijmr-2004-0141 SN - 0044-3093 VL - 95 IS - 9 (85 Jahre DGM) SP - 742 EP - 743 PB - Hanser CY - München AN - OPUS4-5988 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kannengießer, Thomas A1 - Kromm, Arne T1 - Formation of welding residual stresses in low transformation temperature (LTT) materials N2 - For the safety and cost efficiency of welded high-strength steel structures, precise knowledge of the level and distribution of welding- and cooling-specific stresses and residual stresses is essential, since they exert a decisive influence on strength, crack resistance, and finally on the bearable service load. This paper presents innovative filler materials, of which the phase transformation temperature was deliberately adjusted via the chemical composition. The transformation behaviour of these martensitic Low Transformation Temperature (LTT-) filler materials shows direct effects on the local residual stresses in the weld and the HAZ. These effects can purposefully be exploited to counteract the thermally induced shrinkage of the material and to produce significant compressive residual stresses in the weld. Comparative welding experiments were carried out on 690 MPa high-strength base materials using various LTT-filler materials. High energy synchrotron radiation was used for residual stress measurement. Particularly the use of high energy synchrotron radiation makes it possible to detect the residual stress condition fast without destruction of material. Thereby, residual stress depth gradients can be determined simultaneously without removing material. In steel, gradients of up to 150 µm can be resolved in such a way. Furthermore, the application of high energy radiation permits determination of residual stresses of any available residual austenite contents. Results show significant dependence of transformation temperatures on the resulting residual stress level and distribution. KW - Phase specific residual stresses KW - Phase transformation KW - Low transformation temperature filler wire KW - Energy dispersive diffraction KW - High strength steel PY - 2009 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-205909 DO - https://doi.org/10.1590/S0104-92242009000100009 SN - 0104-9224 SN - 1980-6973 VL - 14 IS - 1 SP - 74 EP - 81 PB - Associação Brasileira de Soldagem, ABS CY - Rio de Janeiro AN - OPUS4-20590 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kromm, Arne A1 - Kannengießer, Thomas T1 - In-situ-phase analysis using synchrotron radiation of low transformation temperature (LTT) welding material N2 - Cold cracking resistance is a relevant evaluation criterion for welded joints and affected by residual stresses which result from the welding procedure. Compressive residual stresses can thereby have a positive influence on preventing cracking. A unique possibility of generating compressive residual stresses already during the welding procedure is offered by the so-called Low Transformation Temperature (LTT) filler wires. Compared to conventional wires, these materials show decreased phase transformation temperatures which can work against the cooling-specific contraction. In consequence, distinct compressive residual stresses can be observed within the weld and adjacent areas. The strength of these fillers makes them potentially applicable to high-strength steel welding. Investigations were carried out to determine the phase transformation behaviour of different LTT-filler materials. Transformation temperatures were identified using Single Sensor Differential Thermal Analysis (SS-DTA). Additionally Synchrotron radiation was used to measure the transformation kinetics of all involved crystalline phases during heating and cooling of a simulated weld thermal cycle. KW - In-situ phase analysis KW - Energy dispersive diffraction KW - Phase transformation KW - Low Transformation Temperature filler wire PY - 2009 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-205922 DO - https://doi.org/10.1590/S0104-92242009000100010 SN - 0104-9224 SN - 1980-6973 VL - 14 IS - 1 SP - 82 EP - 88 PB - Associação Brasileira de Soldagem, ABS CY - Rio de Janeiro AN - OPUS4-20592 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mull, Birte A1 - Horn, Wolfgang A1 - Jann, Oliver T1 - Methode zur Bestimmung von flüchtigen Estern der Phthalsäure im Innenraum und in Emissionsmesskammern N2 - Die Analytik von Phthalaten (DMP bis DEHP) in der Luft ist mit thermischer Desorption unter Verwendung von Quarzwolle als Adsorbens erfolgreich realisierbar. Dies wurde durch eine Methodenvalidierung bestätigt. Es wurden sowohl Messungen im Innenraum als auch in Emissionskammern vorgenommen. In den Emissionskammermessungen wurden mögliche Senkeneffekte der Kammeroberfläche (Glas) untersucht. Unter Zuhilfenahme der idealen Abklingkurve wird bestätigt, dass diese Oberfläche eine Senke darstellt. PY - 2010 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-209870 UR - http://www.gefahrstoffe.de SN - 0949-8036 SN - 1436-4891 VL - 70 IS - 3 SP - 93 EP - 97 PB - VDI Fachmedien CY - Düsseldorf AN - OPUS4-20987 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schartel, Bernhard T1 - Phosphorus-based flame retardancy mechanisms - Old hat or a starting point for future development? N2 - Different kinds of additive and reactive flame retardants containing phosphorus are increasingly successful as halogen-free alternatives for various polymeric materials and applications. Phosphorus can act in the condensed phase by enhancing charring, yielding intumescence, or through inorganic glass formation; and in the gas phase through flame inhibition. Occurrence and efficiency depend, not only on the flame retardant itself, but also on its interaction with pyrolysing polymeric material and additives. Flame retardancy is sensitive to modification of the flame retardant, the use of synergists/adjuvants, and changes to the polymeric material. A detailed understanding facilitates the launch of tailored and targeted development. KW - Fire retardancy KW - Red phosphorus KW - Phosphate KW - Phosphonate KW - Phosphinate KW - Phosphine oxide KW - Flame inhibition KW - Charring KW - Intumescence PY - 2010 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-220368 DO - https://doi.org/10.3390/ma3104710 SN - 1996-1944 VL - 3 IS - 10 SP - 4710 EP - 4745 PB - MDPI CY - Basel AN - OPUS4-22036 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pawlowski, Kristin A1 - Schartel, Bernhard A1 - Fichera, Mario Augusto A1 - Jäger, Christian T1 - Flame retardancy mechanisms of bisphenol A bis(diphenyl phosphate) in combination with zinc borate in bisphenol A polycarbonate/Acrylonitrile-butadiene-styrene blends N2 - Bisphenol A polycarbonate/acrylonitrile–butadiene–styrene (PC/ABS) with and without bisphenol A bis(diphenyl phosphate) (BDP) and 5 wt.% zinc borate (Znb) were investigated. The pyrolysis was studied by thermogravimetry (TG), TG-FTIR and NMR, the fire behaviour with a cone calorimeter applying different heat fluxes, LOI and UL 94. Fire residues were examined with NMR. BDP affects the decomposition of PC/ABS and acts as a flame retardant in the gas and condensed phases. The addition of Znb results in an additional hydrolysis of PC. The fire behaviour is similar to PC/ABS, aside from a slightly increased LOI and a reduced peak heat release rate, both caused by borates improving the barrier properties of the char. In PC/ABS + BDP + Znb, the addition of Znb yields a borate network and amorphous phosphates. Znb also reacts with BDP to form alpha-zinc phosphate and borophosphates that suppress the original flame retardancy mechanisms of BDP. The inorganic–organic residue formed provides more effective flame retardancy, in particular at low irradiation in the cone calorimeter, and a clear synergy in LOI, whereas for more developed fires BDP + Znb become less effective than BDP in PC/ABS with respect to the total heat evolved. KW - Flame retardancy KW - PC/ABS KW - Aryl phosphate KW - Zinc borate KW - Flammability PY - 2010 DO - https://doi.org/10.1016/j.tca.2009.10.007 SN - 0040-6031 SN - 1872-762X VL - 498 IS - 1-2 SP - 92 EP - 99 PB - Elsevier CY - Amsterdam AN - OPUS4-20746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Perret, Birgit A1 - Schartel, Bernhard A1 - Stöß, K. A1 - Ciesielski, M. A1 - Diederichs, J. A1 - Döring, M. A1 - Krämer, J. A1 - Altstädt, V. T1 - A new halogen-free flame retardant based on 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide for epoxy resins and their carbon fiber composites for the automotive and aviation industries N2 - The pyrolysis and fire behavior of halogen-free flame-retarded DGEBA/DMC, RTM6 and their corresponding 60 vol.-% carbon fibers (CF) composites were investigated. A novel phosphorous compound (DOPI) was used. Its action is dependent on the epoxy matrix. DGEBA/DMC and DOPI decompose independently of each other. Only flame inhibition occurs in the gas phase. RTM6 shows flame inhibition and a condensed phase interaction increasing charring. Both mechanisms decrease with increasing irradiance, whereas in RTM6-CF charring is suppressed at low ones. RTM6+DOPI shows a higher LOI (34.2%) than DGEBA/DMC+DOPI and a V-0 classification in UL 94. Adding CF only enhances the LOI, DOPI+CF leads to a superposition in LOI for DGEBA/DMC-CF+DOPI (31.8%, V-0) and a synergism for RTM6-CF+DOPI (47.7%, V-0). KW - Composites KW - Flame retardancy KW - Glass transition KW - Pyrolysis KW - Thermosets PY - 2011 DO - https://doi.org/10.1002/mame.201000242 SN - 1438-7492 SN - 1439-2054 VL - 296 IS - 1 SP - 14 EP - 30 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-22957 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hartmann, A. A1 - Petrov, V. A1 - Buhl, J.-C. A1 - Rübner, Katrin A1 - Lindemann, Mathias T1 - Digestion reactions of paper sludge combustion ash in strong alkaline solutions at 60 °C N2 - Alkaline reactions of paper sludge combustion ash at low temperature (60 °C) were performed using a calcite-rich paper ash (PA 1) and a gehlenite-rich ash (PA 2). Strong alkaline conditions (8, 12, 16 M NaOH) were revealed at reaction times of 1–4 h and 12–24 h. Reactions were performed with pure ashes and in the presence of NaAlO2. The products were characterized by XRD, FTIR, SEM/EDX, gravimetry and chemical analysis. The conversion was found to proceed mainly in the period between 1 and 4 h. Portlandite and hydrogarnet were observed from PA 1 in 8 M NaOH. Onset of formation of Ca4Al2O6CO·311H2O beside Ca(OH)2 could be analyzed after reaction of PA 1 in 12 M and 16 M NaOH. Addition of NaAlO2 favored crystallization of hydrogarnet and Ca4-Al2O6CO·311H2O. For PA 2 gehlenite remained stable, but a high portlandite fraction was observed. Addition of NaAlO2 yielded hydrogarnet beside gehlenite in 8 M NaOH. Higher alkalinities favored crystallization of Ca4Al2O6-CO·311H2O and onset of dissolution of gehlenite. Finally transformation of Ca4Al2O6CO·311H2O into sodium aluminum silicate hydrate was observed. All results were discussed with regard to heavy metal distribution of the initial PA between the alkaline digestion solution and the products. In conclusion suitable applications of the products were proposed. KW - Paper sludge combustion ash KW - Alkaline digestion reaction KW - Portlandite KW - Katoite KW - Zeolite PY - 2016 DO - https://doi.org/10.1007/s10163-014-0320-4 SN - 1438-4957 SN - 1611-8227 VL - 18 IS - 1 SP - 132 EP - 145 PB - Springer CY - Tokyo AN - OPUS4-32827 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Kricheldorf, H.R. A1 - Scheliga, F. T1 - Cyclization and dispersity of poly(alkylene isophthalate)s N2 - Poly(alkylene isophthalate)s were prepared by different methods, either in solution or in bulk. The SEC measurements were evaluated in such a way that all oligomers were included. In solution (monomer conc. 0.1–0.7 mol/L) large fractions of rings were formed and high dispersities (up to 12) were obtained, which disagree with theoretical predictions. Polycondensations in bulk did neither generate cyclics by 'back-biting' nor by end-to-end cyclization, when the maximum temperature was limited to 210 °C. The dispersities of these perfectly linear polyesters were again higher than the theoretical values. Regardless of the synthetic method monomeric cycles were never observed. Furthermore, SEC measurements performed in tetrahydrofuran and in chloroform and SEC measurements performed in three different institutes were compared. Finally, SEC measurements of five samples were performed with universal calibration and a correction factor of 0.71 ± 0.02 was found for normal calibration with polystyrene. KW - Cyclization KW - Polycondensation KW - Polyesters KW - Size exclusion chromatography KW - Cyclics KW - Dispersity KW - SEC KW - Universal calibration KW - MALDI mass spectrometry PY - 2016 DO - https://doi.org/10.1002/pola.27892 SN - 0360-6376 SN - 0887-624X VL - 54 IS - 1 SP - 197 EP - 208 PB - Wiley CY - Hoboken, NJ AN - OPUS4-33731 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wäsche, Rolf A1 - Hartelt, Manfred A1 - Hodoroaba, Vasile-Dan T1 - Analysis of nanoscale wear particles from lubricated steel-steel contacts N2 - A new method for sampling wear particles directly from the lubricant reservoir has been developed and applied successfully for analyzing wear particles by high-resolution scanning electron microscopy in transmission mode having coupled energy-dispersive X-ray spectroscopy. The lubricated tribological testing was carried out with fully formulated as well as with non-formulated synthetic base oil. It was possible to analyze individual particles with dimensions as small as about 5–30 nm which are likely the 'primary' wear particles. A majority of the particles, however, are agglomerated and, thus, lead to the formation of larger agglomerates of up to a few micrometers. Chemical analysis led to the conclusion that most of the observed particles generated in formulated oil, especially the larger ones, are composed of the additives of the lubricant oil. In non-formulated base oil, the primary particles are of similar dimensions but contain only iron, chromium and oxygen, but most likely stem from the mating materials. This finding points to the fact that the main wear mechanism under lubricated conditions with fully formulated oil is more like a continuous shearing process rather than a catastrophic failure with the generation of larger primary particles. When the oil is non-formulated, however, several wear mechanisms act simultaneously and the wear rate is increased significantly. Generated larger primary particles are milled down to the nanoscale. When the oil is fully formulated, wear mainly takes places at the additive layer or tribofilm; thus, the steel surface is protected. KW - Particle KW - Wear particle analysis KW - Lubricated contact KW - Bearing steel KW - Nanoscale T-SEM KW - Nanoscale EDX analysis PY - 2015 DO - https://doi.org/10.1007/s11249-015-0534-1 SN - 1023-8883 SN - 1573-2711 VL - 58 IS - 3 SP - 49-1 - 49-10 PB - Springer Science Business Media B.V. CY - Dordrecht AN - OPUS4-33525 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pulz, Robert A1 - Rehmer, Birgit A1 - Schneider, G.A. A1 - Skrotzki, Birgit T1 - Thermal shock study on different advanced ceramics by laser irradiation in different media N2 - The thermal shock behavior of three commercial-advanced ceramics (SSiC, MgO–PSZ, Al2O3) is characterized in air and vacuum applying a laser thermal shock. The available testing system permits the reproducible setting of defined temperature profiles in thin disks and allows a heating-up thermal shock in various media. Due to the accurate determination of the time- and space-resolved temperature distribution, the local stress state can be calculated as a function of time. It is shown that the thermal shock strength is highest for SSiC and lowest in Al2O3 with MgO–PSZ in between. The approach presented in this work allows quantifying the stress state at failure in terms of tangential tensile stress. The investigated environment does not affect the thermal shock resistance under the studied experimental conditions. KW - Laser-thermal shock KW - Advanced ceramic KW - Stress distribution KW - Thermal shock stress KW - Weibull statistics PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/adem.201500162/full DO - https://doi.org/10.1002/adem.201500162 SN - 1438-1656 VL - 18 IS - 1 SP - 132 EP - 140 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-33456 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matzen, Melissa A1 - Kandola, B. A1 - Huth, Christian A1 - Schartel, Bernhard T1 - Influence of flame retardants on the melt dripping behaviour of thermoplastic polymers N2 - Melt flow and dripping of the pyrolysing polymer melt can be both a benefit and a detriment during a fire. In several small-scale fire tests addressing the ignition of a defined specimen with a small ignition source, well-adjusted melt flow and dripping are usually beneficial to pass the test. The presence of flame retardants often changes the melt viscosity crucially. The influence of certain flame retardants on the dripping behaviour of four commercial polymers, poly(butylene terephthalate) (PBT), polypropylene (PP), polypropylene modified with ethylene-propylene rubber (PP-EP) and polyamide 6 (PA 6), is analysed based on an experimental monitoring of the mass loss due to melt dripping, drop size and drop temperature as a function of the furnace temperature applied to a rod-shaped specimen. Investigating the thermal transition (DSC), thermal and thermo-oxidative decomposition, as well as the viscosity of the polymer and collected drops completes the investigation. Different mechanisms of the flame retardants are associated with their influence on the dripping behaviour in the UL 94 test. Reduction in decomposition temperature and changed viscosity play a major role. A flow limit in flame-retarded PBT, enhanced decomposition of flame-retarded PP and PP-EP and the promotion of dripping in PA 6 are the salient features discussed. KW - Fire retardant KW - Viscosity KW - Melt dripping KW - Reaction-to-small-flame KW - UL 94 PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-338941 DO - https://doi.org/10.3390/ma8095267 SN - 1996-1944 VL - 8 IS - 9 SP - 5621 EP - 5646 PB - MDPI CY - Basel AN - OPUS4-33894 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gallo, Emanuela A1 - Schartel, Bernhard A1 - Schmaucks, G. A1 - von der Ehe, Kerstin A1 - Böhning, Martin T1 - Effect of well dispersed amorphous silicon dioxide in flame retarded styrene butadiene rubber N2 - Spherically shaped amorphous silicon dioxide with broad size particle distribution was used in combination with aluminium trihydroxide (ATH) in styrene butadiene rubber composites. The pyrolysis, flammability, fire properties, flame spread and gas diffusion were investigated. The kind and amount of ATH, but in particular the fine silicon dioxide chosen as an additive, influenced the thermal decomposition and fire behaviour of styrene butadiene rubber composites. Gravimetric gas sorption measurements showed that the gas diffusion was systematically lower with silicon dioxide. The initial pyrolysis gas release was hindered, increasing the temperature at which decomposition begins as well as the ignition time in fire tests. During combustion, ATH and silicon dioxide accumulate on the surface of the specimen, forming a residual protective layer. A reduced peak heat release rate and fire spread were observed. The addition of a special kind of silicon dioxide is proposed to play a key role in optimising fire retardancy. KW - Flame retardancy KW - Styrene butadiene rubber KW - SBR KW - Silicon dioxide KW - Aluminium trihydroxide KW - ATH PY - 2013 DO - https://doi.org/10.1179/1743289812Y.0000000012 SN - 1465-8011 SN - 1743-2898 VL - 42 IS - 1 SP - 34 EP - 42 PB - IOM Communications CY - London, UK AN - OPUS4-27626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Herbst, Tristan A1 - Meng, Birgit T1 - Concept for a holistic sustainability assessment of the end-of-life phase of masonry N2 - In Germany, a quantity of more than 10 million metric tons of masonry rubble is generated per year. With regard to a sustainable closed substance cycle waste management, these rest masses have to be recovered if possible. The end-of-life (EOL) phase of masonry includes the planning steps of demolition, processing and application. The choice of the most sustainable solution raises questions regarding material technology, plant engineering, economic efficiency and ecological issues. For this purpose, a methodological concept for a holistic assessment of the EOL phase of masonry is developed within the scope of a doctoral thesis. For the assessment the Cost-Effectiveness Analysis (CEA) is adapted. The assessment concept enables a holistic comparison of different EOL scenarios for masonry while integrating all planning steps. It combines Material Flow Analysis (MFA), Life Cycle Analysis (LCA), Life Cycle Working Environment (LCWE), economic evaluation methods and material testing. In future, various scenarios can be evaluated with regard to the goals of the European and German waste management industry. KW - sustainability KW - end-of-life phase KW - masonry PY - 2016 DO - https://doi.org/10.1144/SP416.5 SN - 0375-6440 SN - 0305-8719 SN - 2041-4927 VL - 416 IS - 1 SP - 47 EP - 57 CY - London AN - OPUS4-33166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Breßler, Ingo A1 - Kohlbrecher, J. A1 - Thünemann, Andreas T1 - SASfit: a tool for small-angle scattering data analysis using a library of analytical expressions N2 - SASfit is one of the mature programs for small-angle scattering data analysis and has been available for many years. This article describes the basic data processing and analysis workflow along with recent developments in the SASfit program package (version 0.94.6). They include (i) advanced algorithms for reduction of oversampled data sets, (ii) improved confidence assessment in the optimized model parameters and (iii) a flexible plug-in system for custom user-provided models. A scattering function of a mass fractal model of branched polymers in solution is provided as an example for implementing a plug-in. The new SASfit release is available for major platforms such as Windows, Linux and MacOS. To facilitate usage, it includes comprehensive indexed documentation as well as a web-based wiki for peer collaboration and online videos demonstrating basic usage. The use of SASfit is illustrated by interpretation of the small-angle X-ray scattering curves of monomodal gold nanoparticles (NIST reference material 8011) and bimodal silica nanoparticles (EU reference material ERM-FD-102). KW - Small-angle X-ray scattering KW - Small-angle neutron scattering KW - Curve fitting KW - Nanotechnology KW - Nanoparticles KW - Polymers KW - SAXS PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-343348 DO - https://doi.org/10.1107/S1600576715016544 SN - 0021-8898 SN - 1600-5767 VL - 48 SP - 1587 EP - 1598 PB - Blackwell CY - Oxford AN - OPUS4-34334 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Breßler, Ingo A1 - Pauw, Brian Richard A1 - Thünemann, Andreas T1 - McSAS: software for the retrieval of model parameter distributions from scattering patterns N2 - A user-friendly open-source Monte Carlo regression package (McSAS) is presented, which structures the analysis of small-angle scattering (SAS) using uncorrelated shape-similar particles (or scattering contributions). The underdetermined problem is solvable, provided that sufficient external information is available. Based on this, the user picks a scatterer contribution model (or 'shape') from a comprehensive library and defines variation intervals of its model parameters. A multitude of scattering contribution models are included, including prolate and oblate nanoparticles, core-shell objects, several polymer models, and a model for densely packed spheres. Most importantly, the form-free Monte Carlo nature of McSAS means it is not necessary to provide further restrictions on the mathematical form of the parameter distribution; without prior knowledge, McSAS is able to extract complex multimodal or odd-shaped parameter distributions from SAS data. When provided with data on an absolute scale with reasonable uncertainty estimates, the software outputs model parameter distributions in absolute volume fraction, and provides the modes of the distribution (e.g. mean, variance etc.). In addition to facilitating the evaluation of (series of) SAS curves, McSAS also helps in assessing the significance of the results through the addition of uncertainty estimates to the result. The McSAS software can be integrated as part of an automated reduction and analysis procedure in laboratory instruments or at synchrotron beamlines. KW - Nanotechnology KW - Nanoparticles KW - Small-angle X-ray scattering KW - SAXS PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-334396 DO - https://doi.org/10.1107/S1600576715007347 SN - 0021-8898 SN - 1600-5767 VL - 48 IS - 3 SP - 962 EP - 969 PB - Blackwell CY - Oxford AN - OPUS4-33439 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bruno, Giovanni A1 - Sevostianov, I. A1 - Cabeza, Sandra A1 - Mishurova, Tatiana T1 - Average phase stress concentrations in multiphase metal matrix composites under compressive loading N2 - We develop a model to predict average over individual phases stress concentrations in a multiphase metal matrix composite under compressive loading. The model accounts for matrix plasticity through variation of the shear modulus with applied stress and for frac- ture of filler through change in the shape of the particles. Three micromechanical models are compared –non interaction approximation, Mori–Tanaka–Benveniste (MTB) scheme, and Maxwell scheme. Comparison with the experimental measurements of Cabeza et al. (2016) shows that Maxwell scheme generally predicts the stress concentration with satis- factory accuracy. Results of MTB scheme vary depending on the loading case and ignoring of the interaction leads to substantial overestimation of the stresses. KW - Average phase stress concentrations KW - metal matrix composite KW - multiphase composite PY - 2016 DO - https://doi.org/10.1016/j.ijengsci.2016.06.004 SN - 0020-7225 VL - 106 SP - 245 EP - 261 PB - Elsevier Ltd. AN - OPUS4-37738 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lühr, T. A1 - Winkelmann, Aimo A1 - Nolze, Gert A1 - Krull, D. A1 - Westphal, C. T1 - Direct Atom Imaging by Chemical-Sensitive Holography N2 - In order to understand the physical and chemical properties of advanced materials, functional molecular adsorbates, and protein structures, a detailed knowledge of the atomic arrangement is essential. Up to now, if subsurface structures are under investigation, only indirect methods revealed reliable results of the atoms’ spatial arrangement. An alternative and direct method is three-dimensional imaging by means of holography. Holography was in fact proposed for electron waves, because of the electrons’ short wavelength at easily accessible energies. Further, electron waves are ideal structure probes on an atomic length scale, because electrons have a high scattering probability even for light elements. However, holographic reconstructions of electron diffraction patterns have in the past contained severe image artifacts and were limited to at most a few tens of atoms. Here, we present a general reconstruction algorithm that leads to high-quality atomic images showing thousands of atoms. Additionally, we show that different elements can be identified by electron holography for the example of FeS₂ . KW - holography KW - electron diffraction KW - atomic imaging KW - photoemission KW - electron backscattering PY - 2016 DO - https://doi.org/10.1021/acs.nanolett.6b00524 VL - 16 IS - 5 SP - 3195 EP - 3201 PB - American Chemical Society AN - OPUS4-37739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haith, M. I. A1 - Ewert, Uwe A1 - Hohendorf, Stefan A1 - Bellon, Carsten A1 - Deresch, Andreas A1 - Huthwaite, P. A1 - Lowe, M. J. S. A1 - Zscherpel, Uwe T1 - Modelling based radiography for NDE of subsea pipelines N2 - This work presents the use of limited experimental measurements to develop a set of calibrated Simulation parameters that can then be used for reliable simulation of subsea pipeline inspections. The modelling software aRTist is used as the simulation tool, and the calibration is through comparison with experimental images of a well characterised sample in a water tank. Image Quality parameters such as signal-to-noise ratio, contrast and basic spatial resolution are compared with the aim of matching simulated values to experimental results. Currently the model is partially calibrated, with signal-to-noise ratio successfully matched while differences are still found in contrast-to-noise ratio comparisons. This means that measurements depending on absolute intensity are not accurate enough in the simulation at this stage. However, the simulation is found to be accurate for wall thickness measurements in tangential images, which are not based on absolute intensity, with simulated and experimental cases producing similar results. T2 - 42nd Annual Review of Progress CY - Minneapolis, Minnesota, USA DA - 26.07.2015 KW - Modelling KW - Radiography KW - Pipeline inspection KW - Nondestructive evaluation PY - 2016 SN - 978-0-7354-1353-5 DO - https://doi.org/10.1063/1.4940575 SN - 0094-243X VL - 1706 SP - 110004-1 EP - 110004-8 PB - AIP Publishing AN - OPUS4-37553 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ewert, Uwe A1 - Martin Tschaikner, Martin A1 - Hohendorf, Stefan A1 - Bellon, Carsten A1 - Haith, M. I. A1 - Huthwaite, P. A1 - Lowe, M. J. S. T1 - Corrosion monitoring with tangential radiography and limited view computed tomography N2 - Accurate and reliable detection of subsea Pipeline corrosion is required in order to verify the integrity of the pipeline. A laboratory trial was conducted with a representative pipe sample. The accurate measurement of the wall thickness and corrosion was performed with high energy X-rays and a digital detector array. A 7.5 MV betatron was used to penetrate a stepped pipe and a welded test pipe of 3 m length and 327 mm outer diameter, with different artificial corrosion areas in the 24 mm thick steel wall. The radiographs were taken with a 40 x 40 cm² digital detector array, which was not large enough to cover the complete pipe diameter after magnification. A C-arm based geometry was tested to evaluate the potential for automated inspection in field. The primary goal was the accurate measurement of wall thickness conforming to the standard. The same geometry was used to explore the ability of a C-arm based scanner in asymmetric mode for computed tomography (CT) measurement, taking projections covering only two thirds of the pipe diameter. The technique was optimized with the modelling Software aRTist. A full volume of the pipe was reconstructed and the CT data set was used for reverse engineering, providing a CAD file for further aRTist simulations to explore the technique for subsea inspections. T2 - 42nd Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Minneapolis, Minnesota, USA DA - 26.07.2015 KW - Corrosion monitoring KW - Tangential radiography KW - Computed tomography PY - 2016 SN - 978-0-7354-1353-5 DO - https://doi.org/10.1063/1.4940574 SN - 0094-243X VL - 1706 SP - 110003-1 EP - 110003-8 PB - AIP Publishing AN - OPUS4-37555 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bach, S. A1 - Panthöfer, M. A1 - Bienert, Ralf A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska A1 - Tremel, W. T1 - Role of water during crystallization of amorphous cobalt phosphate nanoparticles N2 - The transformation of amorphous precursors into crystalline solids and the associated mechanisms are still poorly understood. We illuminate the formation and reactivity of an amorphous cobalt phosphate hydrate precursor and the role of water for its crystallization process. Amorphous cobalt phosphate hydrate nanoparticles (ACP) with diameters of ∼20 nm were prepared in the absence of additives from aqueous solutions at low concentrations and with short reaction times. To avoid the kinetically controlled transformation of metastable ACP into crystalline Co₃(PO₄)₂ × 8H₂O (CPO) its separation must be fast. The crystallinity of ACP could be controlled through the temperature during precipitation. A second amorphous phase (HT-ACP) containing less water and anhydrous Co₃(PO₄)₂ was formed at higher temperature by the release of coordinating water. ACP contains approximately five molecules of structural water per formula unit as determined by thermal analysis (TGA) and quantitative IR spectroscopy. The Co²+ coordination in ACP is tetrahedral, as shown by XANES/EXAFS spectroscopy, but octahedral in crystalline CPO. ACP is stable in the absence of water even at 500 °C. In the wet state, the transformation of ACP to CPO is triggered by the diffusion and incorporation of water into the structure. Quantitative in situ IR analysis allowed monitoring the crystallization kinetics of ACP in the presence of water. KW - Fluorapatite-gelatin nanocomposites KW - Calcium-carbonate KW - Zinc phosphate KW - Crystal-growth KW - Nucleation KW - Polymorphism PY - 2016 DO - https://doi.org/10.1021/acs.cgd.6b00208 SN - 1528-7483 SN - 1528-7505 VL - 16 IS - 8 SP - 4232 EP - 4239 PB - ACS Publications AN - OPUS4-37616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fritzsche, André A1 - Avilov, Vjaceslav A1 - Gumenyuk, Andrey A1 - Hilgenberg, Kai A1 - Rethmeier, Michael T1 - High power laser beam welding of thick-walled ferromagnetic steels with electromagnetic weld pool support N2 - The paper describes an experimental investigation of high power laser beam welding with an electromagnetic weld pool support for up to 20 mm thick plates made of duplex steel (AISI 2205) and mild steel (S235JR). The results of the welding tests show a successful application of this technology at ferromagnetic metals. Irregular sagging was suppressed successfully. An ac-power of less than 2 kW at oscillation frequencies between 800 Hz and 1.7 kHz is necessary for a full compasation of the hydrostatic pressure. Thus, it was demonstrated that the electromagnetic weld pool support is not only limited to non-ferromagnetic metals like austenitic steels. For future studies with duplex steel, the use of filler material has to take into account with regard to the balance of the mixed austenitic and ferritic phases. KW - Laser beam welding KW - Thick-walled steel KW - Ferromagnetic steel KW - Weld pool support PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-377593 DO - https://doi.org/10.1016/j.phpro.2016.08.038 SN - 1875-3892 VL - 83 SP - 362 EP - 372 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-37759 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hartmann, S. A1 - Shaporin, A. A1 - Hermann, S. A1 - Bonitz, J. A1 - Heggen, M. A1 - Meszmer, P. A1 - Sturm, Heinz A1 - Hölck, O. A1 - Blaudeck, T. A1 - Schulz, S. E. A1 - Mehner, J. A1 - Gessner, T. A1 - Wunderle, B. T1 - Towards nanoreliability of CNT-based sensor applications: Investigations of CNT-metal interfaces combining molecular dynamics simulations, advanced in situ experiments and analytics N2 - In this paper we present results of our recent efforts to understand the mechanical interface behaviour of single-walled carbon nanotubes (CNTs) embedded in metal matrices. We conducted experimental pull-out tests of CNTs embedded in Pd or Au and found Maximum forces in the range 10 - 102 nN. These values are in good agreement with forces obtained from molecular Dynamics simulations taking into account surface functional Groups (SFGs) covalently linked to the CNT material. The dominant failure mode in experiment is a CNT rupture, which can be explained with the presence of SFGs. To qualify the existence of SFGs on our used CNT material, we pursue investigations by means of fluorescence labeling of surface species in combination with Raman imaging. We also report of a tensile test system to perform pull-out tests inside a transmission electron microscope to obtain in situ images of CNT-metal interfaces under mechanical loads at the atomic scale. T2 - 2015 16th International Conference on Thermal, Mechanical and Multi-Physics Simulation and Experiments in Microelectronics and Microsystems CY - Budapest, Hungary DA - 20.4.2015 KW - Carbon nanotube CNT KW - Metal matrix KW - Pull-out test KW - Molecular dynamics simulation KW - Surface functional groups KW - Fluorescence labeling KW - Raman imaging KW - Tensile test inside a TEM PY - 2015 SN - 978-1-4799-9950-7 VL - 2015 SP - 1 EP - 8 PB - IEEE AN - OPUS4-37625 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bachmann, Marcel A1 - Gumenyuk, Andrey A1 - Rethmeier, Michael T1 - Welding with high-power lasers: trends and developments N2 - High-power laser beam welding became new stimuli within the last 10 years due to the availability of a new generation of high brightness multi kilowatt solid state lasers. In the welding research new approaches have been developed to establish reliable and praxis oriented welding processes meeting the demands of modern industrial applications during this time. The paper focuses on some of the current scientific and technological aspects in this research field like hybrid laser arc welding, simulation techniques, utilization of electromagnetic fields or reduced pressure environment for laser beam welding processes, which contributed to the further development of this technology or will play a crucial role in its further industrial implementation. T2 - 9th International Conference on Photonic Technologies - LANE 2016 CY - Fürth, Germany DA - 19.09.2016 KW - High-power Laserbeam Welding KW - Electromagnetic Force KW - Vacuum KW - Simulation PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-377280 DO - https://doi.org/10.1016/j.phpro.2016.08.003 VL - 83 SP - 15 EP - 25 PB - Elsevier B.V. CY - Berlin, Germany AN - OPUS4-37728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moser, Marko A1 - Schneider, Ralf A1 - Behnke, Thomas A1 - Schneider, Thomas A1 - Falkenhagen, Jana A1 - Resch-Genger, Ute T1 - Ellman’s and aldrithiol assay as versatile and complementary tools for the quantification of thiol groups and ligands on nanomaterials N2 - Simple, fast, and versatile methods for the quantification of thiol groups are of considerable interest not only for protein analysis but also for the characterization of the surface chemistry of nanomaterials stabilized with thiol ligands or bearing thiol groups for the subsequent (bio-) functionalization via maleimide−thiol chemistry. Here, we compare two simple colorimetric assays, the widely used Ellman’s assay performed at alkaline pH and the aldrithiol assay executed at acidic and neutral pH, with respect to their potential for the quantification of thiol groups and thiol ligands on different types of nanoparticles like polystyrene nanoparticles, semiconductor nanocrystals (SC NC), and noble metal particles, and we derive criteria for their use. In order to assess the underlying reaction mechanisms and to obtain stoichiometry factors mandatory for reliable thiol quantification, both methods were studied photometrically and with electrospray ionization time-of-flight mass spectrometry (ESI-TOF-MS), thereby demonstrating the influence of different thiols on the reaction mechanism. Our results underline the suitability of both methods for the quantification of directly accessible thiol groups or ligands on the surface of 2D- and 3D-supports, here exemplarily polystyrene nanoparticles. Moreover, we could derive strategies for the use of these simple assays for the determination of masked (i.e., not directly accessible) thiol groups like disulfides such as lipoic acid and thiol stabilizing ligands coordinatively bound to Cd and/or Hg surface atoms of II/VI and ternary SC NC and to gold and silver nanoparticles. KW - Nanoparticles KW - Ligands KW - Ellman KW - Aldrithiol KW - Quantification PY - 2016 DO - https://doi.org/10.1021/acs.analchem.6b01798 SN - 0003-2700 SN - 1520-6882 VL - 88 IS - 17 SP - 8624 EP - 8631 PB - ACS Publications CY - Washington AN - OPUS4-37561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abere, M. J. A1 - Zhong, M. A1 - Krüger, Jörg A1 - Bonse, Jörn T1 - Ultrafast laser-induced morphological transformations N2 - Ultrafast laser processing can be used to realize various morphological surface transformations, ranging from direct contour shaping to large-area-surface functionalization via the generation of “self-ordered” micro- and nanostructures as well as their hierarchical hybrids. Irradiation with high-intensity laser pulses excites materials into extreme conditions, which then return to equilibrium through these unique surface transformations. In combination with suitable top-down or bottom-up manufacturing strategies, such laser-tailored surface morphologies open up new avenues toward the control of optical, chemical, and mechanical surface properties, featuring various technical applications especially in the fields of photovoltaics, tribology, and medicine. This article reviews recent efforts in the fundamental understanding of the formation of laser-induced surface micro- and nanostructures and discusses some of their emerging capabilities. KW - Laser ablation KW - Laser-induced periodic surface structures (LIPSS) KW - Surface morphology KW - Oxidation KW - Tribology PY - 2016 DO - https://doi.org/10.1557/mrs.2016.271 SN - 0883-7694 SN - 1938-1425 VL - 41 IS - 12 SP - 969 EP - 974 PB - Cambride University Press AN - OPUS4-38637 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Naghib-zadeh, H. A1 - Oder, Gabriele A1 - Hesse, J. A1 - Reimann, T. A1 - Töpfer, J. A1 - Rabe, Torsten T1 - Effect of oxygen partial pressure on co-firing behavior and magnetic properties of LTCC modules with integrated NiCuZn ferrite layers N2 - Low-κ dielectric LTCC was developed, to realize successful co-firing with NiCuZn ferrite tapes. A critical high-temperature process in the production of highly integrated LTCC modules is the migration of silver from inner conductors into the LTCC glass phase. Intensive silver migration causes strong deformation of LTCC multilayers during firing in air. Silver migration into the LTCC glass phase depends on oxygen content of the sintering atmosphere and can be minimized by sintering in nitrogen atmosphere. However, partial decomposition of NiCuZn-ferrite and formation of cuprite was observed during sintering in nitrogen and, consequently, the permeability of the ferrite decreases. As shown by a combined XRD/thermogravimetric study the co-firing of LTCC modules with silver metallization and integrated ferrite layer demands precise adjustment of oxygen partial pressure. KW - Ferrite KW - Silver diffusion KW - Co-firing KW - LTCC PY - 2016 DO - https://doi.org/10.1007/s10832-016-0043-0 SN - 1385-3449 SN - 1573-8663 VL - 37 IS - 1-4 SP - 100 EP - 109 PB - Springer Science+Business Media CY - New York AN - OPUS4-38603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Höhm, S. A1 - Kirner, Sabrina V. A1 - Rosenfeld, A. A1 - Krüger, Jörg T1 - Laser-induced periodic surface structures — a scientific evergreen N2 - Laser-induced periodic surface structures (LIPSS, ripples) are a universal phenomenon and can be generated on almost any material upon irradiation with linearly polarized radiation. With the availability of ultrashort laser pulses, LIPSS have gained an increasing attraction during the past decade, since these structures can be generated in a simple single-step process, which allows a surface nanostructuring for tailoring optical, mechanical, and chemical surface properties. In this study, the current state in the field of LIPSS is reviewed. Their formation mechanisms are analyzed in ultrafast time-resolved scattering, diffraction, and polarization constrained double-pulse experiments. These experiments allow us to address the question whether the LIPSS are seeded via ultrafast energy deposition mechanisms acting during the absorption of optical radiation or via self-organization after the irradiation process. Relevant control parameters of LIPSS are identified, and technological applications featuring surface functionalization in the fields of optics, fluidics, medicine, and tribology are discussed. KW - Laser ablation KW - Nanostructures KW - Surface functionalization KW - Surface texture KW - Laser-induced periodic surface structures (LIPSS) PY - 2017 DO - https://doi.org/10.1109/JSTQE.2016.2614183 SN - 1077-260X SN - 1558-4542 VL - 23 IS - 3 SP - 9000615 PB - IEEE AN - OPUS4-38633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Batzdorf, Lisa A1 - Zientek, Nicolai A1 - Rump, Doreen A1 - Fischer, Franziska A1 - Maiwald, Michael A1 - Emmerling, Franziska T1 - Make and break - Facile synthesis of cocrystals and comprehensive dissolution studies N2 - Mechanochemistry is increasingly used as a ‘green alternative’ for synthesizing various materials including pharmaceutical cocrystals. Herein, we present the mechanochemical synthesis of three new cocrystals containing the API carbamazepine (cocrystals CBZ:Indometacin 1:1, CBZ:Benzamide 1:1, and CBZ:Nifedipine 1:1). The mechanochemical reaction was investigated in situ documenting a fast and complete reaction within one minute. Online NMR spectroscopy proved the direct influence of the dissolution behaviour of the coformers to the dissolution behaviour of the API carbamazepine. The dissolution behaviour of the organic cocrystals is compared to the behaviour of the pure drug indicating a general applicability of this approach for detailed cocrystal dissolution studies. KW - Cocrystals KW - Carbamazepine KW - Mechanochemistry KW - Powder diffraction KW - Online NMR spectroscopy PY - 2017 DO - https://doi.org/10.1016/j.molstruc.2016.11.063 SN - 0022-2860 SN - 1872-8014 VL - 1133 SP - 18 EP - 23 AN - OPUS4-38664 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fuhrmann, A. A1 - Göstl, R. A1 - Wendt, R. A1 - Kötteritzsch, J. A1 - Hager, M. D. A1 - Schubert, U. S. A1 - Brademann-Jock, Kerstin A1 - Thünemann, Andreas A1 - Nöchel, U. A1 - Behl, M. A1 - Hecht, S. T1 - Conditional repair by locally switching the thermal healing capability of dynamic covalent polymers with light N2 - Healable materials could play an important role in reducing the environmental footprint of our modern technological society through extending the life cycles of consumer products and constructions. However, as most healing processes are carried out by heat alone, the ability to heal damage generally kills the parent material’s thermal and mechanical properties. Here we present a dynamic covalent polymer network whose thermal healing ability can be switched ‘on’ and ‘off’ on demand by light, thereby providing local control over repair while retaining the advantageous macroscopic properties of static polymer networks. We employ a photoswitchable furan-based crosslinker, which reacts with short and mobile maleimidesubstituted poly(lauryl methacrylate) chains forming strong covalent bonds while simultaneously allowing the reversible, spatiotemporally resolved control over thermally induced de- and re-crosslinking. We reason that our system can be adapted to more complex materials and has the potential to impact applications in responsive coatings, photolithography and microfabrication. KW - Small-angle X-ray scattering KW - SAXS KW - Polymer PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-386689 DO - https://doi.org/10.1038/ncomms13623 SN - 2041-1723 VL - 7 SP - Article 13623, 1 EP - 7 PB - NATURE PUBLISHING GROUP CY - MACMILLAN BUILDING, 4 CRINAN ST, LONDON N1 9XW, ENGLAND AN - OPUS4-38668 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stegemann, Robert A1 - Cabeza, Sandra A1 - Lyamkin, V. A1 - Bruno, Giovanni A1 - Pittner, Andreas A1 - Wimpory, Robert A1 - Boin, M. A1 - Kreutzbruck, Marc T1 - Residual stress characterization of steel TIG welds by neutron diffraction and by residual magnetic stray field mappings N2 - The residual stress distribution of tungsten inert gas welded S235JRC+C plates was determined by means of neutron diffraction(ND). Large longitudinal residual stresses with maxima around 600 MPa were found. With these results as reference, the evaluation of residual stress with high spatial resolution GMR (giant magneto resistance) sensors was discussed. The experiments performed indicate a correlation between changes in residual stresses (ND) and the normal component of local residual magnetic stray fields (GMR). Spatial variations in the magnetic field strength perpendicular to the welds are in the order of the magnetic field of the earth. KW - GMR KW - Magnetic stray field KW - Neutron diffraction KW - Residual stress KW - TIG-welding PY - 2017 DO - https://doi.org/10.1016/j.jmmm.2016.11.102 SN - 0304-8853 SN - 1873-4766 VL - 426 SP - 580 EP - 587 PB - Elsevier CY - Amsterdam AN - OPUS4-38678 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 - Blaker, J. J. A1 - Anthony, David B. A1 - Tang, G. A1 - Shamsuddin, S.-R. A1 - Kalinka, Gerhard A1 - Wienrich, Malte A1 - Abdolvand, Amin A1 - Shaffer, M. S. P. A1 - Bismarck, A. T1 - Property and shape modulation of carbon fibers using lasers N2 - An exciting challenge is to create unduloid-reinforcing fibers with tailored dimensions to produce synthetic composites with improved toughness and increased ductility. Continuous carbon fibers, the state-of-the-art reinforcement for structural composites, were modified via controlled laser irradiation to result in expanded outwardly tapered regions, as well as fibers with Q-tip (cotton-bud) end shapes. A pulsed laser treatment was used to introduce damage at the single carbon fiber level, creating expanded regions at predetermined points along the lengths of continuous carbon fibers, while maintaining much of their stiffness. The range of produced shapes was quantified and correlated to single fiber tensile properties. Mapped Raman spectroscopy was used to elucidate the local compositional and structural changes. Irradiation conditions were adjusted to create a swollen weakened region, such that fiber failure occurred in the laser treated Region producing two fiber ends with outwardly tapered ends. Loading the tapered fibers allows for viscoelastic energy dissipation during fiber pull-out by enhanced friction as the fibers plough through a matrix. In these tapered fibers, diameters were locally increased up to 53%, forming outward taper angles of up to 1.8°. The tensile strength and strain to failure of the modified fibers were significantly reduced, by 75% and 55%, respectively, ensuring localization of the break in the expanded region; however, the fiber stiffness was only reduced by 17%. Using harsher irradiation conditions, carbon fibers were completely cut, resulting in cottonbud fiber end shapes. Single fiber pull-out tests performed using these fibers revealed a 6.75-fold increase in work of pull-out compared to pristine carbon fibers. Controlled laser irradiation is a route to modify the shape of continuous carbon fibers along their lengths, as well as to cut them into controlled lengths leaving tapered or cotton-bud shapes. KW - Composite KW - Irradiation KW - Pull-out tests KW - Pulsed laser treatment KW - Single carbon fibers PY - 2016 DO - https://doi.org/10.1021/acsami.6b05228 SN - 1944-8244 SN - 1944-8252 VL - 8 IS - 25 SP - 16351 EP - 16358 PB - ACS Publications CY - 1155 Sixteenth Street, NW, Washington, DC 20036, USA AN - OPUS4-37699 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dabah, Eitan A1 - Pfretzschner, Beate A1 - Schaupp, Thomas A1 - Kardjilov, N. A1 - Manke, I. A1 - Boin, M. A1 - Woracek, R. A1 - Griesche, Axel T1 - Time-resolved Bragg-edge neutron radiography for observing martensitic phase transformation from austenitized super martensitic steel N2 - Neutron Bragg-edge imaging was applied for the visualization of a γ-Austenite to α'-martensite phase transformation. In the present study, a super martensitic stainless steel sample was heated until complete austenitization and was subsequently cooled down to room temperature. The martensitic phase Transformation started at Ms = 190 °C. Using a monochromatic neutron beam with λ = 0.390 nm, the transmitted intensity was significantly reduced during cooling below Ms, since the emerging martensitic phase has a higher attenuation coefficient than the austenitic phase at this wavelength. The phase Transformation process was visualized by filming the transmission images from a scintillator screen with a CCD camera with a temporal resolution of 30 s and a spatial resolution of 100 µm. KW - Neutron imaging KW - Bragg-edge imaging KW - Phase transformation PY - 2017 DO - https://doi.org/10.1007/s10853-016-0642-9 SN - 0022-2461 SN - 1573-4803 VL - 52 IS - 6 SP - 3490 EP - 3496 AN - OPUS4-38574 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Franziska A1 - Greiser, Sebastian A1 - Peifer, Dietmar A1 - Jäger, Christian A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Mechanochemically Induced Conversion of Crystalline Benzamide Polymorphs by Seeding N2 - Benzamide has been known for its polymorphism for almost 200 years.Three polymorphic forms are described. To date,itwas only possible to crystallizeametastable form in amixture together with the thermodynamically most stable form I. Acomplete transformation of form Iinto the metastable form III by mechanochemical treatment has been achieved. Catalytic amounts of nicotinamide seeds were used to activate the conversion by mechanochemical seeding. NMR experiments indicated that the nicotinamide molecules were incorporated statistically in the crystal lattice of benzamide form III during the conversion. The transformation pathway was evaluated using in situ powder X-ray diffraction. KW - Nicotinamide KW - Benzamide KW - In situ reactions KW - Mechanochemistry KW - Polymorphs PY - 2016 DO - https://doi.org/10.1002/anie.201607358 VL - 128 IS - 46 SP - 14493 EP - 14497 PB - WILEY-VCH CY - Weinheim AN - OPUS4-38472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gers-Panther, C.F. A1 - Fischer, H. A1 - Nordmann, J. A1 - Seiler, T. A1 - Behnke, Thomas A1 - Würth, Christian A1 - Frank, W. A1 - Resch-Genger, Ute A1 - Müller, T.J.J. T1 - Four- and Five-Component Syntheses and Photophysical Properties of Emission Solvatochromic 3‑Aminovinylquinoxalines N2 - 3-Aminovinylquinoxalines are readily accessible from (hetero)aryl glyoxylic acids or heterocyclic π-nucleophiles by consecutive four- and fivecomponent syntheses in the sense of an activation-alkynylation-cyclocondensation-addition sequence or glyoxylation-alkynylation-cyclocondensation-addition sequence in good yields. The title compounds are highly fluorescent with pronounced emission solvatochromicity and protochromic fluorescence quenching. Time-resolved fluorescence spectroscopy furnishes radiative and nonradiative fluorescence decay rates in various solvent polarities. The electronic structure is corroborated by DFT and TD-DFT calculations rationalizing the observed spectroscopic effects. KW - Dye KW - Syntheseis KW - Spectroscopy PY - 2016 DO - https://doi.org/10.1021/acs.joc.6b02581 SN - 0022-3263 VL - 82 SP - 567 EP - 578 PB - ACS Publications AN - OPUS4-39211 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pasternak, H. A1 - Launert, B. A1 - Kannengießer, Thomas A1 - Rhode, Michael T1 - Advanced residual stress assessment of plate girders through welding simulation N2 - This article provides an impression on potentials in applying nowadays welding simulation tools in construction design. This is carried out exemplary on plate girders from two structural steel grades. The calculated residual stresses are compared with measurements by sectioning method. It has been repeatedly stated that present Eurocode models fail to approximate the residual stresses. Especially for high strength steel (HSS) only limited information is available on realistic occurring residual stresses in typical I-girders. The investigations are aimed to give further guidance on these values. A few proposals on advanced models are discussed. T2 - MBST 2016 - Modern Building Materials, Structures and Techniques CY - Vilnius, Litunia DA - 26.05.2016 KW - Residual stresses KW - Plate girders KW - I-shape sections KW - High-strength steel KW - Welding simulation PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-392177 UR - http://www.sciencedirect.com/science/article/pii/S1877705817305192 DO - https://doi.org/10.1016/j.proeng.2017.02.013 SN - 1877-7058 IS - 172 SP - 23 EP - 30 PB - Elsevier CY - Amsterdam, Niederlande AN - OPUS4-39217 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scheuerlein, C. A1 - Uhlemann, Patrick A1 - Finn, Monika A1 - Lackner, F. A1 - Savary, F. T1 - Mechanical properties of the HL-LHC 11 T Nb3Sn magnet constituent materials N2 - A test campaign was launched to determine the mechanical properties of the High Luminosity-Large HadronCollider (HL-LHC) 11 T Nb3Sn magnet components. The results can be used to accurately represent the mechanical properties in finite elementmodels that predict the stress and strain distribution in these magnets. Particular attention is paid to anisotropic mechanical behavior of the different magnet materials. Static and dynamic test methods have been applied for determining elastic materials’ behavior, and highly accurate Young’s moduli are obtained with the nondestructive dynamic methods resonance and impulse excitation at ambient temperature and during in situ heat cycles. KW - Superconducting magnets KW - Young’s modulus KW - Resonance testing KW - Stress-strain behavior PY - 2017 DO - https://doi.org/10.1109/TASC.2016.2638046 SN - 1051-8223 SN - 1558-2515 VL - 27 IS - 4 SP - 1 EP - 7 PB - IEEE AN - OPUS4-39219 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Lange, Axel A1 - Bruno, Giovanni T1 - Microstructure Characterization of Ceramics via 2D and 3D X-Ray Refraction Techniques N2 - 3D imaging techniques are very fashionable nowadays, and allow enormous progress in understanding ceramic microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this feature article, we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. While the techniques are limited by the X-ray absorption of the material under investigation, we demonstrate showcases of ceramics and composite materials, where understanding of process parameter influence or simply of microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography. KW - X-ray refraction KW - Porosity KW - Specific surface KW - Crack detection KW - Composites PY - 2017 DO - https://doi.org/10.1016/j.jeurceramsoc.2016.12.031 SN - 0955-2219 SN - 1873-619X VL - 37 IS - 5 SP - 1879 EP - 1889 PB - Elsevier CY - Amsterdam AN - OPUS4-39094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epping, Ruben A1 - Panne, Ulrich A1 - Falkenhagen, Jana T1 - Critical conditions for liquid chromatography of statistical copolymers: Functionality type and composition distribution characterization by UP-LCCC/ESI-MS N2 - Statistical ethylene oxide (EO) and propylene oxide (PO) copolymers of different monomer compositions and different average molar masses additionally containing two kinds of end groups (FTD) were investigated by ultra high pressure liquid chromatography under critical conditions (UP-LCCC) combined with electrospray ionization time-of flight mass spectrometry (ESI-TOFMS). Theoretical predictions of the existence of a critical adsorption point (CPA) for statistical copolymers with a given chemical and sequence distribution1 could be studied and confirmed. A fundamentally new approach to determine these critical conditions in a copolymer, alongside the inevitable chemical composition distribution (CCD), with mass spectrometric detection, is described. The shift of the critical eluent composition with the monomer composition of the polymers was determined. Due to the broad molar mass distribution (MMD) and the presumed existence of different end group functionalities as well as monomer sequence distribution (MSD), Gradient separation only by CCD was not possible. Therefore, isocratic separation conditions at the CPA of definite CCD fractions were developed. Although the various present distributions partly superimposed the separation process, the goal of separation by end group functionality was still achieved on the basis of the additional dimension of ESI-TOF-MS. The existence of HO-H besides the desired allylO-H end group functionalities was confirmed and their amount estimated. Furthermore, indications for a MSD were found by UPLC/MS/MS measurements. This approach offers for the first time the possibility to obtain a fingerprint of a broad distributed statistical copolymer including MMD, FTD, CCD, and MSD. KW - Polymer KW - Liquid chromatography at critical conditions KW - ESI-TOF-MS PY - 2017 DO - https://doi.org/10.1021/acs.analchem.6b04064 SN - 0003-2700 SN - 1520-6882 VL - 89 IS - 3 SP - 1778 EP - 1786 AN - OPUS4-39240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Wilke, Manuel A1 - Fischer, Franziska A1 - Röllig, Mathias A1 - Maierhofer, Christiane A1 - Emmerling, Franziska T1 - Warming up for mechanosynthesis – temperature development in ball mills during synthesis N2 - We present a first direct measurement of the temperature during milling combined with in situ Raman spectroscopy monitoring. The data reveal a low temperature increase due to the mechanical impact and clear temperature increases as a consequence of the reaction heat. Based on the data, temperature rises as postulated in the magma plasma and hot spot theory can be excluded for soft matter milling syntheses. KW - Thermography KW - Milling KW - Mechanochemistry KW - Soft matter PY - 2017 DO - https://doi.org/10.1039/c6cc08950j SN - 1364-548X SN - 1359-7345 SN - 0009-241X VL - 53 IS - 10 SP - 1664 EP - 1667 AN - OPUS4-39251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madkour, Sherif A1 - Szymoniak, Paulina A1 - Heídari, M. A1 - von Klitzing, R. A1 - Schönhals, Andreas T1 - Unveiling the dynamics of self-assembled layers of thin films of poly(vinyl methyl ether) (PVME) by nanosized relaxation spectroscopy N2 - A combination of nanosized dielectric relaxation (BDS) and thermal spectroscopy (SHS) was utilized to characterize the dynamics of thin films of Poly(vinyl methyl ether) (PVME) (thicknesses: 7 nm – 160 nm). For the BDS measurements, a recently designed nano-structured electrode system is employed. A thin film is spin-coated on an ultra-flat highly conductive silicon wafer serving as the bottom electrode. As top electrode, a highly conductive wafer with non-conducting nanostructured SiO2 nano-spacers with heights of 35 nm or 70 nm is assembled on the bottom electrode. This procedure results in thin supported films with a free polymer/air interface. The BDS measurements show two relaxation processes, which are analyzed unambiguously for thicknesses smaller than 50 nm. The relaxation rates of both processes have different temperature dependencies. One process coincidences in its position and temperature dependence with the glassy dynamics of bulk PVME and is ascribed to the dynamic glass transition of a bulk-like layer in the middle of the film. The relaxation rates were found to be thickness independent as confirmed by SHS. Unexpectedly, the relaxation rates of the second process obey an Arrhenius-like temperature dependence. This process was not observed by SHS and was related to the constrained fluctuations in a layer, which is irreversibly adsorbed at the substrate with a heterogeneous structure. Its molecular fluctuations undergo a confinement effect resulting in the localization of the segmental dynamics. To our knowledge, this is the first report on the molecular dynamics of an adsorbed layer in thin films. KW - Broadband dielectric spectroscopy KW - AC-nanochip calorimetry KW - Nanostructured capacitors KW - Thin films PY - 2017 UR - http://pubs.acs.org/doi/pdf/10.1021/acsami.6b14404 DO - https://doi.org/10.1021/acsami.6b14404 SN - 1944-8244 VL - 9 IS - 8 SP - 7535 EP - 7546 PB - ACS Publications CY - Washington DC AN - OPUS4-39291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dittrich, Matthias A1 - Meixner, Matthias A1 - Schumacher, Gerhard T1 - Texture formation in amorphous Al86Ni6Y4.5La1.5Co2 splats by thermal and mechanical treatment N2 - The crystallization behavior of amorphous Al86Ni6Y4.5La1.5Co2 splats was analyzed by differential scanning calorimetry (DSC) and X-ray diffraction (XRD). Rietveld refinement was used to analyze the preferred orientation of fcc aluminum nanocrystals in the residual amorphous matrix after annealing. Fiber textures in [200] and [220] directions were found after heating to 360 C. The influence of cold rolling on the preferred crystal orientation was studied as a function of the thickness reduction of the specimen. It was found that cold rolling significantly increases the (220) texture, while the (200) texture remains unchanged. Based on the experimental results the formation of (220) and (200) texture during the crystallization of the amorphous splats was ascribed to two different processes, internal stresses induced during splat formation or cold-rolling. KW - Aluminum alloy KW - Metallic glass KW - Al-TM-RE KW - Crystallization KW - Cold rolling KW - Texture PY - 2016 DO - https://doi.org/10.1016/j.intermet.2016.04.008 SN - 0966-9795 SN - 1879-0216 VL - 74 SP - 46 EP - 52 PB - ELSEVIER AN - OPUS4-39268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stegemann, Robert A1 - Cabeza, Sandra A1 - Pelkner, Matthias A1 - Lyamkin, Viktor A1 - Sonntag, Nadja A1 - Bruno, Giovanni A1 - Skrotzki, Birgit A1 - Kreutzbruck, Marc T1 - Evaluation of high spatial resolution imaging of magnetic stray fields for early damage detection N2 - The paper discusses the evaluation of elastic and plastic strain states in two low-carbon steels of the same steel group with high spatial resolution GMR (giant magneto resistance) sensors. The residual stress distributions of tungsten inert gas welded plates were determined by means of neutron diffraction as a reference. The normal component of local residual magnetic stray fields arise in the vicinity of the positions of maximum stress. The experiments performed on flat tensile specimen indicate that the boundaries of plastic deformations are a source of stray fields. The spatial variations of magnetic stray fields for both the weld and the tensile samples are in the order of the earths magnetic field. T2 - 43rd Annual Review of Progress in Quantitative Nondestructive Evaluation, Volume 36 CY - Atlanta, Georgia, USA DA - 17.07.2016 KW - Plastic deformation KW - GMR KW - Neutron diffraction KW - Residual stress KW - Microstructure KW - Low carbon steel KW - TIG weld PY - 2017 SN - 978-0-7354-1474-7 DO - https://doi.org/10.1063/1.4974688 SN - 0094-243X VL - 1806 IS - 1 SP - Article UNSP 110010-1 EP - 10 PB - AIP Publishing CY - Melville, NY 11747 AN - OPUS4-39279 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Seuthe, T. A1 - Mermillod-Blondin, A. A1 - Grehn, M. A1 - Bonse, Jörn A1 - Wondraczek, L. A1 - Eberstein, M. T1 - Structural relaxation phenomena in silicate glasses modifed by irradiation with femtosecond laser pulses N2 - Structural relaxation phenomena in binary and multicomponent lithium silicate glasses were studied upon irradiation with femtosecond (fs) laser pulses (800 nm central wavelength, 130 fs pulse duration) and subsequent thermal annealing experiments. Depending on the annealing temperature, micro-Raman spectroscopy analyses evidenced different relaxation behaviours, associated to bridging and non-bridging oxygen structures present in the glass network. The results indicate that the mobility of lithium ions is an important factor during the glass modification with fs-laser pulses. Quantitative phase contrast imaging (spatial light interference microscopy) revealed that these fs-laser induced structural modifications are closely related to local changes in the refractive index of the material. The results establish a promising strategy for tailoring fs-laser sensitivity of glasses through structural mobility. KW - Femtosecond laser KW - Silicate glasses KW - Raman spectroscopy KW - Structural relaxation KW - Refractive index PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-393045 DO - https://doi.org/10.1038/srep43815 SN - 2045-2322 VL - 7 SP - 43815, 1 EP - 43815, 10 PB - Nature Publishing Group CY - London, UK AN - OPUS4-39304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonse, Jörn A1 - Kirner, Sabrina V. A1 - Höhm, S. A1 - Epperlein, Nadja A1 - Spaltmann, Dirk A1 - Rosenfeld, A. A1 - Krüger, Jörg T1 - Applications of laser-induced periodic surface structures (LIPSS) N2 - Laser-induced periodic surface structures (LIPSS, ripples) are a universal phenomenon that can be observed on almost any material after the irradiation by linearly polarized laser beams, particularly when using ultrashort laser pulses with durations in the picosecond to femtosecond range. During the past few years significantly increasing research activities have been reported in the field of LIPSS, since their generation in a single-step process provides a simple way of nanostructuring and surface functionalization towards the control of optical, mechanical or chemical properties. In this contribution current applications of LIPSS are reviewed, including the colorization of technical surfaces, the control of surface wetting, the tailoring of surface colonization by bacterial biofilms, and the improvement of the tribological performance of nanostructured metal surfaces. T2 - SPIE Photonics West Conference, Laser-based Micro- and Nanoprocessing XI CY - San Francisco, USA DA - 27.01.2017 KW - Laser-induced periodic surface structures (LIPSS) KW - Laser processing KW - Surface functionalization KW - Application PY - 2017 SN - 978-1-5106-0625-8 SN - 978-1-5106-0626-5 DO - https://doi.org/10.1117/12.2250919 SN - 0277-786X SN - 1996-756X VL - 10092 SP - Article UNSP 100920N, 100920N-1 EP - 100920N-9 PB - SPIE CY - Bellingham, USA AN - OPUS4-39305 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 - Sötebier, Carina A. A1 - Weidner, Steffen A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Bettmer, J. T1 - Separation and quantification of silver nanoparticles and silver ions using reversed phase high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry in combination with isotope dilution analysis N2 - A reversed phase high performance liquid chromatography coupled to an inductively coupled Plasma mass spectrometer (HPLC–ICP-MS) approach in combination with isotope dilution analysis (IDA) for the separation and parallel quantification of nanostructured and ionic silver (Ag) is presented. The main Focus of this work was the determination of the ionic Ag concentration. For a sufficient stabilization of the Ions without dissolving the nanoparticles (NPs), the eluent had to be initially optimized. The determined Ag ion concentration was in a good agreement with results obtained using ultrafiltration. Further, the mechanism of the NP separation in the HPLC column was investigated. Typical size exclusion effects were found by comparing results from columns with different pore sizes. Since the recovery rates decreased with increasing Ag NP size and large Ag NPs did not elute from the column, additional interactions of the particles with the stationary phase were assumed. Our results reveal that the presented method is not only applicable to Ag NPs, but also to gold and polystyrene NPs. Finally, IDA-HPLC-ICP-MS experiments in single particle mode were performed to determine the particle cut-off size. The comparison with conventional spICP-MS experiments resulted in a similar diameter and particle size distribution. KW - ICP-MS KW - Silver nanoparticles KW - Speciation KW - High performance liquid chromatography KW - Isotope dilution analysis PY - 2016 DO - https://doi.org/10.1016/j.chroma.2016.09.028 SN - 0021-9673 VL - 1468 SP - 102 EP - 108 AN - OPUS4-37652 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -