TY - JOUR A1 - Meschut, G. A1 - Janzen, V. A1 - Rethmeier, Michael A1 - Gumenyuk, Andrey A1 - Frei, J. T1 - Charakterisierung des Bruch- und Festigkeits verhaltens von widerstandspunktgeschweißten Aluminiumverbindungen N2 - Die Reduktion des Fahrzeuggewichts ist ein wesentlicher Ansatz zur Ver-ringerung des Energie- und Ressourcenverbrauchs und damit zur Senkung der CO2-Emissionen im Automobilbau. In der Karosserieentwicklung kann der vermehrte Einsatz von Aluminiumwerkstoffen einen bedeutenden Beitrag dazu leisten. Im preissensitiven Umfeld des Karosseriebaus etabliert sich das bei Stahlanwendungen genutzte Widerstandspunktschweißen zunehmend auch für Aluminiumverbindungen. Verfahrensbedingte Herausforderungen, wie verkürzte Elektrodenstandzeiten und mangelnde Kenntnis über den Einfluss von Imperfektionen auf die Festigkeit, begrenzen dennoch die Weiterverbreitung des Verfahrens und stellen die Prozessrobustheit insgesamt in Frage. Im Rahmen des hier vorgestellten Forschungsvorhabens wurden das Auftreten verschiedener Brucharten experimentell untersucht und Prognosefunktionen zur Abschätzung der Tragfähigkeit von Widerstandspunktschweißverbindungen unter verschiedenen Belastungsfällen erstellt. Anschließend wurde der Einfluss von Oberflächenrissen und Rissen in der Schweißlinse auf die Scherzugfestigkeit sowohl experimentell als auch simulativ analysiert. KW - Aluminium KW - Widerstandspressschweißen KW - Rissbildung KW - Festigkeit KW - Werkstofffragen PY - 2017 UR - http://www.schweissenundschneiden.de/article/charakterisierung-des-bruch-und-festigkeitsverhaltens-von-widerstandspunktgeschweissten-aluminiumverbindungen/ VL - 69 IS - 3 SP - 126 EP - 133 PB - DVS Media GmbH AN - OPUS4-39577 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dieck, S. A1 - Rosemann, Paul A1 - Kromm, Arne A1 - Halle, T. T1 - Reversed austenite for enhancing ductility of martensitic stainless steel N2 - The novel heat treatment concept, “quenching and partitioning” (Q&P) has been developed for high strength steels with enhanced formability. This heat treatment involves quenching of austenite to a temperature between martensite start and finish, to receive a several amount of retained austenite. During the subsequent annealing treatment, the so called partitioning, the retained austenite is stabilized due to carbon diffusion, which results in enhanced formability and strength regarding strain induced austenite to martensite transformation. In this study a Q&P heat treatment was applied to a Fe-0.45C-0.65Mn-0.34Si-13.95Cr stainless martensite. Thereby the initial quench end temperature and the partitioning time were varied to characterize their influence on microstructural evolution. The microstructural changes were analysed by dilatometer measurements, X-ray diffraction and scanning electron microscopy, including electron backscatter diffraction. Compression testing was made to examine the mechanical behaviour. It was found that an increasing partitioning time up to 30 min leads to an enhanced formability without loss in strength due to a higher amount of stabilized retained and reversed austenite as well as precipitation hardening. T2 - 19th Chemnitz Seminar on Materials Engineering – 19. Werkstofftechnisches Kolloquium CY - Chemnitz, Germany DA - 16.03.2017 KW - Quenching and partitioning KW - Martensitic stainless steels KW - Heat treatment KW - Transformation induced plasticity KW - High ductility PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-395328 DO - https://doi.org/10.1088/1757-899X/181/1/012034 SN - 1757-899X SN - 1757-8981 VL - 181 IS - Conference 1 SP - Article UNSP 012034, 1 EP - 8 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-39532 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottlieb, Cassian A1 - Millar, Steven A1 - Günther, Tobias A1 - Wilsch, Gerd T1 - Revealing hidden spectral information of chlorine and sulfur in data of a mobile Laser-induced Breakdown Spectroscopy system using chemometrics N2 - For the damage assessment of reinforced concrete structures the quantified ingress profiles of harmful species like chlorides, sulfates and alkali need to be determined. In order to provide on-site analysis of concrete a fast and reliable method is necessary. Low transition probabilities as well as the high ionization energies for chlorine and sulfur in the near-infrared range makes the detection of Cl I and S I in low concentrations a difficult task. For the on-site analysis a mobile LIBS-system (k = 1064 nm, Epulse ≤ 3 mJ, t = 1.5 ns) with an automated scanner has been developed at BAM. Weak chlorine and sulfur signal intensities do not allow classical univariate analysis for process data derived from the mobile system. In order to improve the analytical performance multivariate analysis like PLS-R will be presented in this work. A comparison to standard univariate analysis will be carried out and results covering important parameters like detection and quantification limits (LOD, LOQ) as well as processing variances will be discussed (Allegrini and Olivieri, 2014 [1]; Ostra et al., 2008 [2]). It will be shown that for the first time a low cost mobile system is capable of providing reproducible chlorine and sulfur analysis on concrete by using a low sensitive system in combination with multivariate evaluation. KW - LIBS KW - Chemometrics KW - Building materials PY - 2017 DO - https://doi.org/10.1016/j.sab.2017.04.001 SN - 0584-8547 VL - 132 SP - 43 EP - 49 PB - Elsevier B.V. AN - OPUS4-40066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Joester, Maike A1 - Seifert, Stephan A1 - Emmerling, Franziska A1 - Kneipp, Janina T1 - Physiological influence of silica on germinating pollen as shown by Raman spectroscopy N2 - The process of silicification in plants and the biochemical effects of silica in plant tissues are largely unknown. To study the molecular changes occurring in growing cells that are exposed to higher than normal concentration of silicic acid, Raman spectra of germinating pollen grains of three species (Pinus nigra, Picea omorika, and Camellia japonica) were analyzed in a multivariate classification approach that takes into account the variation of biochemical composition due to species, plant tissue structure, and germination condition. The results of principal component analyses of the Raman spectra indicate differences in the utilization of stored lipids, a changed mobilization of storage carbohydrates in the pollen grain bodies, and altered composition and/or structure of cellulose of the developing pollen tube cell walls. These biochemical changes vary in the different species. KW - Silica KW - Raman spectroscopy KW - Principal component analysis PY - 2017 DO - https://doi.org/10.1002/jbio.201600011 SN - 1864-063X SN - 1864-0648 VL - 10 IS - 4 SP - 542 EP - 552 AN - OPUS4-40090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weltschev, Margit T1 - Auswahl eines Kennwertes für den Vergleich des mechanischen Leistungsniveaus von Polyethylenformstoffen für Gefahrgutverpackungen T1 - Parameter selection for the comparison of the mechanical level of performance of polyethylene molding materials for packagings of dangerous goods N2 - Zum Vergleich der Polyethylenformstoffe für eine Bauart von Gefahrgutverpackungen und IBC wurden die Materialkennwerte: Schmelze-Massefließrate MFR, Dichte D, Kerbschlag-zähigkeit acN bei -30 °C, Spannungsrissbeständigkeit (bestimmt mit dem Full Notch Creep Test) und Beständigkeit gegen oxidativen Abbau Ox (bestimmt durch den prozentualen Anstieg des MFR in Salpetersäure) in der DIN EN 15507 – Verpackung – Verpackungen zur Beförderung gefährlicher Güter – Vergleichende Werkstoffprüfung von Polyethylensorten ausgewählt. Das Ziel der Untersuchungen war die Auswahl eines Kennwertes für die Bestimmung des mechanischen Leistungsniveaus von Polyethylenformstoffen, da unter Druck Verpackungen beulen oder knicken. Zur Auswahl standen drei Prüfverfahren: a) Bestimmung der Biegesteifigkeit S nach DIN 53 350 (Prinzip von Ohlsen). b) Bestimmung der Biegefestigkeit σfM und Biegedehnung ɛfM nach DIN EN ISO 178 c) Bestimmung der Druckkraft Fmax und Verformung dL bei Fmax nach DIN EN ISO 604. Die Prüfmethode zur Bestimmung der Biegesteifigkeit nach DIN 53 350 eignet sich zum Vergleich des mechanischen Leistungsniveaus der Formstoffe. Zur Verbesserung der Reproduzierbarkeit der Ergebnisse sollte der Skalierungsbereich der Prüfapparatur erweitert wer-den, um genauere Messergebnisse zu erzielen. Der Dreipunktbiegeversuch nach DIN EN ISO 178 eignet sich bei verformungsfähigen Kunststoffen, wie dem Polyethylen, zur Bestimmung der Biegefestigkeit σfM. Dieser Ver-such besitzt den Nachteil, dass am Ort des maximalen Biegemoments in der Randschicht, wo auch die maximale Biegespannung erzeugt wird, zusätzlich der Biegestempel angreift. Die Messergebnisse haben gezeigt, dass die Druckprüfung nach DIN EN ISO 604 sich sehr gut zur Bewertung des mechanischen Verhaltens der Polyethylenformstoffe unter Druckbelastung (Stapeldruckprüfung der Verpackungen) eignet. KW - Gefahrgutverpackung KW - Polyethylen KW - Biegesteifigkeit KW - Biegefestigkeit KW - Druckkraft PY - 2017 DO - https://doi.org/10.3139/120.111025 SN - 0025-5300 VL - 59 IS - 5 SP - 466 EP - 471 PB - Carl Hanser Verlag GmbH & Co.KG CY - München AN - OPUS4-40145 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rodrigues, A.C.P. A1 - Österle, Werner A1 - Gradt, Thomas A1 - Azevedo, César Roberto de Farias T1 - Impact of copper nanoparticles on tribofilm formation determined by pin-on-disc tests with powder supply: Addition of artificial third body consisting of Fe3O4, Cu and graphite N2 - Copper, magnetite and graphite particles were mixed in order to observe their impact on the coefficient of friction (CoF) during pin-on-disc tests and on the tribofilm formation after testing. Pure magnetite powder provided a value of CoF of 0.4. Magnetite-copper mixtures tested at 400 °C revealed lower CoF values (~0.4) than those at room temperature (~0.6). Magnetite-graphite and magnetite-graphite-copper mixtures presented lower CoF values (~0.3). All systems formed a magnetite-based tribofilm and patches of metallic copper were found on the tribosurfaces of the mixtures containing copper. Carbon layers and graphite nanoinclusions were observed in the graphite mixtures. The incorporation of zirconia particles, a by-product of ball milling mixing, prevented the selective transfer of graphite and copper to the tribosurfaces of some of the samples. KW - Brake pad materials KW - Sliding friction KW - Transfer layer KW - Surface analysis KW - Model friction tests PY - 2017 DO - https://doi.org/10.1016/j.triboint.2017.02.014 SN - 0301-679X VL - 110 SP - 103 EP - 112 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-40104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sproesser, G. A1 - Chang, Y.-J. A1 - Pittner, Andreas A1 - Finkbeiner, M. A1 - Rethmeier, Michael T1 - Environmental energy efficiency of single wire and tandem gas metal arc welding N2 - This paper investigates gas metal arc welding (GMAW) with respect to energy consumption and its associated environmental impacts. Different material transfer modes and power levels for single wire GMAW (SGMAW) and tandem GMAW (TGMAW) are evaluated by means of the indicator electrical deposition efficiency. Furthermore, the wall-plug efficiency of the equipment is measured in order to describe the total energy consumption from the electricity grid. The results show that the energy efficiency is highly affected by the respective process and can be significantly enhanced by a TGMAW process. The wall-plug efficiency of the equipment shows no significant dependency on the power range or the material transfer mode. Moreover, the method of life cycle assessment (LCA) is adopted in order to investigate the influences of energy efficient welding on the environmental impacts. In the comparative LCA study, the demand of electrical energy is reduced up to 24%. In consequence, the indicator values for global warming potential (100), acidification potential, eutrophication potential, and photochemical ozone creation potential are reduced up to 11%. KW - Energy input KW - Tandem welding KW - MAG welding KW - Environment KW - Lifetime PY - 2017 DO - https://doi.org/10.1007/s40194-017-0460-y SN - 0043-2288 SN - 1878-6669 VL - 61 IS - 4 SP - 733 EP - 743 PB - Springer CY - Heidelberg AN - OPUS4-39877 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hennig, C. A1 - Weiss, S. A1 - Kraus, Werner A1 - Kretzschmar, J. A1 - Scheinost, A.C. T1 - Solution species and crystal structure of Zr(IV) acetate N2 - Complex formation and the coordination of zirconium with acetic acid were investigated with Zr K-edge extended X-ray absorption fine structure spectroscopy (EXAFS) and single-crystal diffraction. Zr K-edge EXAFS spectra show that a stepwise increase of acetic acid in aqueous solution with 0.1 M Zr(IV) leads to a structural rearrangement from initial tetranuclear hydrolysis species [Zr4(OH)8(OH2)16]8+ to a hexanuclear acetate species Zr6(O)4(OH)4(CH3COO)12. The solution species Zr6(O)4(OH)4(CH3COO)12 was preserved in crystals by slow evaporation of the aqueous solution. Single-crystal diffraction reveals an uncharged hexanuclear cluster in solid Zr6(μ3-O)4(μ3-OH)4(CH3COO)12·8.5H2O. EXAFS measurements show that the structures of the hexanuclear zirconium acetate cluster in solution and the solid state are identical. KW - Complex formation KW - Crystal structure KW - Zr(iV) compounds PY - 2017 DO - https://doi.org/10.1021/acs.inorgchem.6b01624 SN - 0020-1669 SN - 1520-510X VL - 56 IS - 5 SP - 2473 EP - 2480 PB - ACS AN - OPUS4-39677 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Joseph, A. A1 - Bernardes, C. E. S. A1 - Druzhinina, A. I. A1 - Varushchenko, R. M. A1 - Nguyen, Thi Yen A1 - Emmerling, Franziska A1 - Yuan, L. A1 - Dupray, V. A1 - Coquerel, G. A1 - Minas da Piedade, M. E. T1 - Polymorphic phase transition in 4′-hydroxyacetophenone: Equilibrium temperature, kinetic barrier, and the relative stability of Z′=1 and Z′=2 forms N2 - Particularly relevant in the context of polymorphism is understanding how structural, thermodynamic, and kinetic factors dictate the stability domains of polymorphs, their tendency to interconvert through phase transitions, or their possibility to exist in metastable states. These three aspects were investigated here for two 4′-hydroxyacetophenone (HAP) polymorphs, differing in crystal system, space group, and number and conformation of molecules in the asymmetric unit. The results led to a ΔfGm°-T phase diagram highlighting the enantiotropic nature of the system and the fact that the Z′=1 polymorph is not necessarily more stable than its Z′=2 counterpart. It was also shown that the form II → form I transition is entropy driven and is likely to occur through a nucleation and growth mechanism, which does not involve intermediate phases, and is characterized by a high activation energy. Finally, although it has been noted that conflicts between hydrogen bond formation and close packing are usually behind exceptions from the hypothesis of Z′=1 forms being more stable than their higher Z′ analogues, in this case, the HAP polymorph with stronger hydrogen bonds (Z′=2) is also the one with higher density. KW - Polymorphism KW - Polymorphic transition KW - 4'-hydroxyacetophenone PY - 2017 DO - https://doi.org/10.1021/acs.cgd.6b01876 SN - 1528-7483 SN - 1528-7505 VL - 17 IS - 4 SP - 1918 EP - 1932 PB - ACS AN - OPUS4-40167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Myrach, Philipp A1 - Jonietz, Florian A1 - Meinel, Dietmar A1 - Suwala, Hubert A1 - Ziegler, Mathias T1 - Calibration of thermographic spot weld testing with X-ray computed tomography N2 - The paper presents an attempt for the calibration of an active thermography method that is suitable for the non-destructive evaluation of spot welds. Nowadays, the quality of spot welds is commonly characterised by the application of random chisel tests, which are time consuming, expensive and destructive. Recently a non-destructive testing method by means of active thermography was proposed that relies on the fact that the mechanical connection formed by the spot weld also serves as a thermal bridge between the two steel sheets joined in the welding process. It is shown in this paper that this thermal bridge can be thermographically characterised by extracting a measure for the spot weld diameter and hence the quality of the spot weld. The determination of the absolute value of the diameter hereby relies on a calibration of the testing system, which is performed by means of X-ray computed tomography in this study. The experiments were carried out using different experimental approaches, namely transmission as well as reflection geometry wSetup in reflectionith laser illumination. A comprehensive evaluation of samples produced using different welding currents, hence different quality, was carried out in order to validate the thermographic results. KW - Thermography KW - Spot welds KW - Spot welding KW - Computed thomography KW - Non-destructive testing PY - 2017 DO - https://doi.org/10.1080/17686733.2017.1281554 SN - 1768-6733 SN - 2116-7176 VL - 14 IS - 1 SP - 122 EP - 131 PB - Taylor & Francis CY - London AN - OPUS4-40180 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietzsch, Michael A1 - Andrusenko, Iryna A1 - Branscheid, Robert A1 - Emmerling, Franziska A1 - Kolb, Ute A1 - Tremel, Wolfgang T1 - Snapshots of calcium carbonate Formation - a step by step analysis N2 - Recent advances in our understanding of CaCO, nucleation from solution have provoked new and challenging questions. We have studied CaC03 formation using precipitation by carbonate ester hydrolysis which ensures precipitation from a strictly homogeneous solution state and allows “titrating” carbonate to a solution with a given Ca2+ concentration on a timescale suited for kinetic studies. Nucleation and crystallization were traced by combining dynamic light Scattering (DLS) and transmission electron microscopy (TEM). DLS served as in situ technique to identify the nucleation time, to monitor particle size evolution, to discriminate different precipitation mechanisms and to validate reproducibility. TEM snapshots taken during different stages of the precipitation process identified different phases and morphologies. At a high level of supersaturation homogeneous nucleation in solution led to the formation of amorphous CaC03 particles (diameter=30 nm), which transformed via vaterite to calcite. Nucleation occurred uniformly in solution which appears to be unique for the CaC03 System. In the presence of Na-polymethacrylate (Na-PMA), heterogeneous nucleation was suppressed and Ca-polymer aggregates were formed in the prenucleation stage. Beyond a critical threshold supersaturation CaC03 particles formed in solution outside of these aggregates. The nucleation process resembled that without additive, indicating that Na-PMA exerts only a minor effect on the CaC03 nucleation. In the postnucleation stage, the polymer led to the formation of extended liquid-like networks, which served as a precursor phase for solid ACC particles that formed alongside the network. KW - biomineralization KW - calcium carbonate KW - nucleation KW - polymer additives PY - 2017 DO - https://doi.org/10.1515/zkri-2016-1973 SN - 2194-4946 SN - 2196-7105 VL - 232 IS - 1-3 SP - 255 EP - 265 PB - De Gruyter CY - Berlin AN - OPUS4-39863 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Bach, S. A1 - Gorelik, T. A1 - Kolb, U. A1 - Tremel, W. A1 - Emmerling, Franziska T1 - Divalent metal phosphonates – new aspects for syntheses, in situ characterization and structure solution N2 - Divalent metal phosphonates are promising hybrid materials with a broad field of application. The rich coordination chemistry of the phosphonate linkers enables the formation of structures with different dimensionalities ranging from isolated complexes and layered structures to porous frameworks incorporating various functionalities through the choice of the building blocks. In brief, metal phosphonates offer an interesting opportunity for the design of multifunctional materials. Here, we provide a short review on the class of divalent metal phosphonates discussing their syntheses, structures, and applications. We present the advantages of the recently introduced mechanochemical pathway for the Synthesis of divalent phosphonates as a possibility to generate new, in certain cases metastable compounds. The benefits of in situ investigation of synthesis mechanisms as well as the implementation of sophisticated methods for the structure analysis of the resulting compounds are discussed. KW - Metal phosphonate KW - Mechanochemistry PY - 2017 DO - https://doi.org/10.1515/zkri-2016-1971 SN - 2194-4946 SN - 2196-7105 VL - 232 IS - 1-3 SP - 209 EP - 222 PB - De Gruyter AN - OPUS4-40003 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Huang, S. G. A1 - Vleugels, J. A1 - Mohrbacher, H. A1 - Woydt, Mathias T1 - Microstructure and tribological performance of NbC-Ni cermets modified by VC and Mo2C N2 - The current study reports on the influence of the Addition of 5–15 vol% VC or/and Mo2C carbide on the microstructure and mechanical properties of nickel bonded NbC cermets, which are compared to cobalt bonded NbC cermets. The NbC, Ni and secondary carbides powder mixtures were liquid phase sintered for 1 h at 1420 °C in vacuum. The fully densified cermets are composed of a cubic NbC grains matrix and an evenly distributed fcc Ni binder. NbC grain growth was significantly inhibited and a homogeneous NbC grain size distribution was obtained in the cermets with VC/Mo2C additions. The mechanical properties of the NbC-Ni matrix cermets are strongly dependent on the carbide and Ni binder content and are directly compared to their NbC-Co equivalents. The liquid phase sintered NbC-12 vol% Ni cermet had a modest Vickers hardness (HV30) of 1077 ± 22 kg/mm2 and an indentation toughness of 9.1 ± 0.5 MPa·m1/2. With the addition of 10–15 vol% VC, the hardness increased to 1359 ± 15 kg/mm2, whereas the toughness increased to 11.3 ± 0.1 MPa·m1/2. Addition of 5 and 10 vol% Mo2C into a NbC-12 vol% Ni mixtures generated the same values in HV30 and KIC when compared to VC additions. A maximum flexural strength of 1899 ± 77 MPa was obtained in the cermet with 20 vol% Ni binder and 4 vol% VC+4 vol% Mo2C addition, exhibiting a high fracture toughness of 15.0 ± 0.5 MPa·m1/2, but associated with a loss in hardness due to the high Ni content. The dry sliding wear behaviour was established at room temperature and 400 °C from 0.1 to 10 m/s. KW - Cermet KW - Liquid phase sintering KW - Grain growth KW - Wear KW - Niobium carbide PY - 2017 DO - https://doi.org/10.1016/j.ijrmhm.2017.03.012 SN - 0263-4368 VL - 66 SP - 188 EP - 197 AN - OPUS4-40505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Kirner, Sabrina A1 - Koter, Robert A1 - Pentzien, Simone A1 - Spaltmann, Dirk A1 - Krüger, Jörg T1 - Femtosecond laser-induced periodic surface structures on titanium nitride coatings for tribological applications N2 - Titanium nitride (TiN) was coated on different substrate materials, namely pure titanium (Ti), titanium alloy (Ti6Al4V) and steel (100Cr6), generating 2.5 μm thick TiN layers. Using femtosecond laser pulses (30 fs, 790 nm, 1 kHz pulse repetition rate), large surface areas (5 mm × 5 mm) of laser-induced periodic surface structures (LIPSS) with sub-wavelength periods ranging between 470 nm and 600 nm were generated and characterized by optical microscopy (OM), white light interference microscopy (WLIM) and scanning electron microscopy (SEM). In tribological tests, coefficients of friction (COF) of the nanostructured surfaces were determined under reciprocating sliding conditions (1 Hz, 1.0 N normal load) against a 10-mm diameter ball of hardened 100Cr6 steel during 1000 cycles using two different lubricants, namely paraffin oil and engine oil. It turned out that the substrate material, the laser fluence and the lubricant are crucial for the tribological performance. However, friction and wear could not be significantly reduced by LIPSS on TiN layers in comparison to unstructured TiN surfaces. Finally, the resulting wear tracks on the nanostructured surfaces were investigated with respect to their morphology (OM, SEM), depth (WLIM) and chemical composition by energy dispersive X-ray spectroscopy (EDX) and, on one hand, compared with each other, on the other hand, with non-structured TiN surfaces. KW - Laser-induced periodic surface structures (LIPSS) KW - Femtosecond laser ablation KW - Titanium nitride films KW - Friction KW - Wear PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S0169433216322486 DO - https://doi.org/10.1016/j.apsusc.2016.10.132 SN - 0169-4332 SN - 1873-5584 VL - 418 IS - Part B SP - 572 EP - 579 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-40507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hermens, U. A1 - Kirner, Sabrina A1 - Emonts, C. A1 - Comanns, P. A1 - Skoulas, E. A1 - Mimidis, A. A1 - Mescheder, H. A1 - Winands, K. A1 - Krüger, Jörg A1 - Stratakis, E. A1 - Bonse, Jörn T1 - Mimicking lizard-like surface structures upon ultrashort laser pulse irradiation of inorganic materials N2 - Inorganic materials, such as steel, were functionalized by ultrashort laser pulse irradiation (fs- to ps-range) to modify the surface’s wetting behavior. The laser processing was performed by scanning the laser beam across the surface of initially polished flat sample material. A systematic experimental study of the laser processing parameters (peak fluence, scan velocity, line overlap) allowed the identification of different regimes associated with characteristic surface morphologies (laser-induced periodic surface structures, grooves, spikes, etc.). Analyses of the surface using optical as well as scanning electron microscopy revealed morphologies providing the optimum similarity to the natural skin of lizards. For mimicking skin structures of moisture-harvesting lizards towards an optimization of the surface wetting behavior, additionally a two-step laser processing strategy was established for realizing hierarchical microstructures. In this approach, micrometer-scaled capillaries (step 1) were superimposed by a laser-generated regular array of small dimples (step 2). Optical focus variation imaging measurements finally disclosed the three dimensional topography of the laser processed surfaces derived from lizard skin structures. The functionality of these surfaces was analyzed in view of wetting properties. KW - Femtosecond laser ablation KW - Laser-induced periodic surface structures KW - Lizard KW - Surface wetting KW - Fluid transport KW - Steel PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S0169433216328306 DO - https://doi.org/10.1016/j.apsusc.2016.12.112 SN - 0169-4332 SN - 1873-5584 VL - 418 IS - Part B SP - 499 EP - 507 PB - Elsevier, North-Holland CY - Amsterdam AN - OPUS4-40509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duffner, Eric A1 - Schoppa, André A1 - Szczepaniak, Mariusz T1 - Untersuchung der Haltbarkeit von Reparaturmaßnahmen an Bremsleitungsabschnitten durch hydraulische Berstdruckprüfungen N2 - Im Rahmen einer Bachelorarbeit zum Thema „Untersuchungen an Bremsleitungsabschnittsreparaturen“ zwischen der HTW Berlin und der TÜV Rheinland Kraftfahrt GmbH wurden in Zusammenarbeit mit der Bundesanstalt für Materialforschung und -prüfung (BAM) Berstdruckprüfungen durchgeführt. Im Rahmen der Kooperation sollte untersucht werden, inwiefern Reparaturmaßnahmen an beschädigten Bremsleitungsabschnitten sicherheitstechnisch unbedenklich sind, auch in Bezug auf die Verwendung unterschiedlicher auf dem Markt erhältlicher Bremsleitungsmaterialien. KW - Bremsleitung KW - Berstprüfung PY - 2017 SN - 2191-007 VL - 7 IS - 6 SP - 44 PB - Springer VDI-Verlag CY - Düsseldorf AN - OPUS4-40490 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Miccoli, Lorenzo A1 - Müller, U. A1 - Pospisil, S. T1 - Rammed earth walls strengthened with polyester fabric strips: Experimental analysis under in-plane cyclic loading N2 - This study analyses the mechanical behaviour under pseudo-dynamic loading of structural elements built in rammed earth and strengthened with polyester fabric strips. This strengthening technique was developed to exploit the strength potential of rammed earth and to solve its lack of tensile strength. For this reason, in-plane cyclic tests were carried out to investigate the shear behaviour of unstrengthened and strengthened walls. The strengthening technique requires low-tech equipment and workmanship, uses readily available, not expensive and industrially standardised materials. The experimental results were analysed in terms of stiffness degradation, energy dissipation capacity and equivalent viscous damping. Although the unstrengthened and strengthened walls confirmed a limited ductile behaviour, the findings confirm that the strengthening contributes to limit the spread of the diagonal cracks and provide an increase of strength in terms of horizontal load and displacement capacity. KW - Rammed earth KW - Pseudo-dynamic loads KW - Shear-compression tests KW - Strengthening KW - Polyester fabric strips PY - 2017 DO - https://doi.org/10.1016/j.conbuildmat.2017.05.115 IS - 149 SP - 29 EP - 36 PB - Elsevier Ltd. AN - OPUS4-40497 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Caricato, A.P. A1 - Focsa, C. A1 - Krüger, Jörg A1 - Palla Papavlu, A. T1 - European materials research society spring meeting 2016 symposium "Laser - materials interactions for tailoring future's applications" Preface N2 - This Conference Proceedings volume contains a selection of the contributions presented in Symposium C “Laser-material interactions for tailoring future applications” organized during the annual Spring Meeting of the European Materials Research Society (E-MRS) held from May 2nd to 6th 2016 in the Lille Grand Palais, France. T2 - EMRS Spring Meeting 2016, Symposium "“Laser-material interactions for tailoring future applications” CY - Lille, France DA - 02.05.2016 KW - European Materials Research Society (E-MRS) KW - Laser-material interactions KW - Spring Meeting 2016 PY - 2017 DO - https://doi.org/10.1016/j.apsusc.2017.04.089 SN - 0169-4332 SN - 1873-5584 VL - 418 IS - Part B SP - 419 EP - 419 PB - Elsevier B.V. AN - OPUS4-40570 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hönig, Gerald A1 - Westerkamp, S. A1 - Hoffmann, A. A1 - Callsen, G. T1 - Shielding electrostatic fields in polar semiconductor nanostructures N2 - Polar semiconductor materials enable a variety of classic and quantum-light sources, which are optimized continuously. However, one key problem—the inherent electric crystal polarization of such materials—remains unsolved and deteriorates the radiative exciton decay rate. We suggest a sequence of reverse interfaces to compensate these polarization effects, while the polar, natural crystal growth direction is maintained. Former research approaches, like growth on less-polar crystal planes or even the stabilization of unnatural phases, never reached industrial maturity. In contrast, our concept provides a way for the development of ultrafast devices based on established growth processes for polar materials, while the electric potential landscape becomes adjustable. KW - Piezopolarisation KW - Spontane Polarisation KW - Halbleiterphysik KW - Nanophysik KW - Optoelektronik PY - 2017 DO - https://doi.org/10.1103/PhysRevApplied.7.024004 SN - 2331-7019 VL - 7 IS - 2 SP - 024004-1 EP - 024004-12 PB - American Physical Society CY - College Park, MD 20740-3844 AN - OPUS4-39125 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalinka, Gerhard A1 - ElAbshihy, K. T1 - Circumventing boundary effects while characterizing epoxy/copper interphases using nanoindentation N2 - Characterization of the size and mechanical properties of interphases is essential when designing multicomponent materials. When nanoindentation is used to investigate the size and mechanical properties of an interphase, a common challenge is that the indenter or the stress zone formed around it are often restricted by the reinforcement, making it difficult to distinguish the mechanical property variations caused by the interphase itself from those caused by the boundary effect. In this work, a testing system was developed that allows determining the indent affected zone and accounting for it in the interphase measurements of an epoxy/Cu system. Using finite element analysis, we confirmed the validity of the proposed system. Nanoindentation was used to investigate the Interphase between copper and two different epoxy systems; amine-cured and anhydride-cured. Nanoindentation results showed that a copper layer that is only 10 nm thick still exhibits a constriction effect on the indentations in its vicinity. The amine-cured epoxy did not show any sign of interphase existence using the introduced method. However, a soft interphase with a thickness of ~1.7 μm was measured on theanhydride-cured epoxy. Furthermore, we show that the proposed system can be used to determine the interphase thickness as well as its relative mechanical properties regardless of the indentation depth. This system can be further used for investigating other polymer/metal interphases to better understand the factors influencing them, thus helping engineer the interphase size and properties to enhance composite performance. KW - Interphase KW - Polymer-metal KW - Epoxy KW - Copper KW - Composites KW - Nanoindentation PY - 2017 DO - https://doi.org/10.1080/09276440.2017.1286878 SN - 0927-6440 SN - 1568-5543 VL - 24 IS - 9 SP - 833 EP - 848 PB - Taylor & Francis CY - UK AN - OPUS4-39128 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 - Zhou, Peng A1 - Ogle, Kevin A1 - Erning, Johann Wilhelm A1 - Hutchinson, Michael John A1 - Scully, John T1 - An in situ kinetic study of brass dezincification and corrosion N2 - The kinetics of the anodic dissolution of brass (CuZn42 and CuZn21Si3P) in synthetic tap water were investigated by atomic emission spectroelectrochemistry. Elemental Cu and Zn dissolution rates were measured in situ and in real time during galvanostatic dissolution. A complete mass/charge balance for the system yielded, as a function of applied current and a function of time, the quantity of Cu in the dezincification layer and the quantity of Cu and Zn in the oxide layer. In this way, a complete kinetic characterization of the fundamental chemical processes occurring during dezincification was realized for the first time. The oxide layer was composed primarily of Cu2O as indicated by grazing incidence XRD and Raman analysis. The soluble Cu oxidation product was determined to be Cu(II) by a mass/charge balance. Zn was oxidized to soluble Zn(II) leaving behind a trivial amount of solid Zn corrosion product on the surface. The kinetic analysis depicts a two-stage dissolution process of dezincification: a first stage of a rapid growth of the dezincified layer and a second stage where the growth of dezincified layer was much slower. The Cu2O layer grows continually during the exposure. KW - Dezincification KW - Spectroelectrochemistry KW - Brass PY - 2017 DO - https://doi.org/10.1016/j.electacta.2017.01.078 SN - 0013-4686 SN - 1873-3859 VL - 229 SP - 141 EP - 154 PB - Elsevier AN - OPUS4-39164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yilmaz, M. A1 - Wollschläger, Nicole A1 - Esfahani, M. N. A1 - Österle, Werner A1 - Leblebici, Y. A1 - Alaca, B. E. T1 - Superplastic behavior of silica nanowires obtained by direct patterning of silsesquioxane-based precursors N2 - Silica nanowires spanning 10 μm-deep trenches are fabricated from different types of silsesquioxane-based precursors by direct e-beam patterning on silicon followed by release through deep reactive ion etching. Nanowire aspect ratios as large as 150 are achieved with a critical dimension of about 50 nm and nearly rectangular cross-sections. In situ bending tests are carried out inside a scanning electron microscope, where the etch depth of 10 mm provides sufficient space for deformation. Silica NWs are indeed observed to exhibit superplastic behavior without fracture with deflections reaching the full etch depth, about two orders of magnitude larger than the nanowire thickness. A large-deformation elastic bending model is utilized for predicting the deviation from the elastic behavior. The results of forty different tests indicate a critical stress level of 0.1–0.4 GPa for the onset of plasticity. The study hints at the possibility of fabricating silica nanowires in a monolithic Fashion through direct e-beam patterning of silsesquioxane-based resins. The fabrication technology is compatible with semiconductor manufacturing and provides silica nanowires with a very good structural integrity. KW - Silica nanowires KW - HSQ KW - Superplasticity KW - In situ bending tests PY - 2017 DO - https://doi.org/10.1088/1361-6528/aa5b80 SN - 0957-4484 SN - 1361-6528 VL - 28 IS - 11 SP - Article 115302, 1 EP - 10 AN - OPUS4-39166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yilmaz, M. A1 - Kilinc, Y. A1 - Nadar, G. A1 - Tasdemir, Z. A1 - Wollschläger, Nicole A1 - Österle, Werner A1 - Leblebici, Y. A1 - Alaca, B. E. T1 - Top-down technique for scaling to nano in silicon MEMS N2 - Nanoscale building blocks impart added functionalities to microelectromechanical systems (MEMS). The integration of silicon nanowires with MEMS-based sensors leading to miniaturization with improved sensitivity and higher noise immunity is one example highlighting the advantages of this multiscale approach. The accelerated pace of research in this area gives rise to an urgent need for batch-compatible solutions for scaling to nano. To address this challenge, a monolithic fabrication approach of silicon nanowires with 10-lm-thick silicon-on-insulator (SOI) MEMS is developed in this work. A two-step Si etching approach is adopted, where the first step creates a shallow surface protrusion and the second step releases it in the form of a nanowire. It is during this second deep etching step that MEMS—with at least a 2-order-of-magnitude scale difference - is formed as well. The technique provides a pathway for preserving the lithographic resolution and transforming it into a very high mechanical precision in the assembly of micro- and nanoscales with an extreme topography. Validation of the success of integration is carried out via in situ actuation of MEMS inside an electron microscope loading the nanowire up to its fracture. The technique yields nanowires on the top surface of MEMS, thereby providing ease of access for the purposes of carrying out surface processes such as doping and contact formation as well as in situ observation. As the first study demonstrating such monolithic integration in thick SOI, the work presents a pathway for scaling down to nano for future MEMS combining multiple scales. KW - Nanowires KW - Silicon KW - Top-down KW - MEMS PY - 2017 DO - https://doi.org/10.1116/1.4978047 SN - 1071-1023 VL - 35 IS - 2 SP - 022001-1 EP - 022001-7 PB - America Vacuum Society AN - OPUS4-39370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Jan P. A1 - Götschel, S. A1 - Maierhofer, Christiane A1 - Weiser, M. T1 - Determining the Material Parameters for the Reconstruction of Defects in Carbon Fiber Reinforced Polymers from Data Measured by Flash Thermography N2 - Flash thermography is a fast and reliable non-destructive testing method for the investigation of defects in carbon fiber reinforced polymer (CFRP) materials. In this paper numerical simulations of transient thermography data are presented, calculated for a quasi-isotropic flat bottom hole sample. They are compared to experimental data. These simulations are one important step towards the quantitative reconstruction of a flaw by assessing thermographic data. The applied numerical model is based on the finite-element method, extended by a semi-analytical treatment of the boundary of the sample, which is heated by the flash light. A crucial part for a reliable numerical model is the prior determination of the material parameters of the specimen as well as of the experimental parameters of the set-up. The material parameters in plane and in depth diffusivity are measured using laser line excitation. In addition, the absorption and heat transfer process of the first layers is investigated using an IR microscopic lens. The performance of the two distinct components of CFRP during heating – epoxy resin and carbon fibers – is examined. Finally, the material parameters are optimized by variation and comparison of the simulation results to the experimental data. The optimized parameters are compared to the measured ones and further methods to ensure precise material parameter measurements are discussed. T2 - 43rd Review of Progress in Quantitative Nondestructive Evaluation CY - Atlanta, GA, USA DA - 17.07.2016 KW - Aktive Thermografie KW - Thermische Diffusivität KW - Zerstörungsfreie Prüfung KW - Kohlenstofffaserverstärkter Kunststoff KW - CFK KW - Active thermography KW - Thermal diffusivity KW - Non-Destructive testing KW - Carbon fiber reinforced polymer KW - CFRP PY - 2017 SN - 978-0-7354-1474-7 DO - https://doi.org/10.1063/1.4974671 SN - 0094-243X VL - 1806 IS - 1 SP - UNSP 100006-1 EP - 11 PB - AIP Publishing CY - Melville, NY, USA AN - OPUS4-39332 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 - Fischer, Daniel A1 - Hertwig, Andreas A1 - Beck, Uwe A1 - Lohse, V. A1 - Negendank, D. A1 - Kormunda, M. A1 - Esser, N. T1 - Thin SnOx films for surface plasmon resonance enhanced ellipsometric gas sensing (SPREE) N2 - Background: Gas sensors are very important in several fields like gas monitoring, safety and environmental applications. In this approach, a new gas sensing concept is investigated which combines the powerful adsorption probability of metal oxide conductive sensors (MOS) with an optical ellipsometric readout. This concept Shows promising results to solve the problems of cross sensitivity of the MOS concept. Results: Undoped tin oxide (SnOx) and iron doped tin oxide (Fe:SnOx) thin add-on films were prepared by magnetron sputtering on the top of the actual surface plasmon resonance (SPR) sensing gold layer. The films were tested for their sensitivity to several gas species in the surface plasmon resonance enhanced (SPREE) gas measurement. It was found that the undoped tin oxide (SnOx) shows higher sensitivities to propane (C3H8) then to carbon monoxide (CO). By using Fe:SnOx, this relation is inverted. This behavior was explained by a change of the amount of binding sites for CO in the layer due to this iron doping. For hydrogen (H2) no such relation was found but the sensing ability was identical for both layer materials. This observation was related to a different sensing mechanism for H2 which is driven by the Diffusion into the layer instead of adsorption on the surface. Conclusion: The gas sensing selectivity can be enhanced by tuning the properties of the thin film overcoating. A relation of the binding sites in the doped and undoped SnOx films and the gas sensing abilities for CO and C3H8 was found. This could open the path for optimized gas sensing devices with different coated SPREE sensors. KW - Doped tin oxide KW - Ellipsometry KW - Gas sensing KW - Surface plasmon KW - Resonance KW - Thin films KW - Transparent conductive oxides PY - 2017 DO - https://doi.org/10.3762/bjnano.8.56 SN - 2190-4286 VL - 8 SP - 522 EP - 529 AN - OPUS4-39391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martins, M. S. S. A1 - Schartel, Bernhard A1 - Magalhães, F. D. A1 - Pereira, C. M. C. T1 - The effect of traditional flame retardants, nanoclays and carbon nanotubes in the fire performance of epoxy resin composites N2 - The effectiveness of distinct fillers, from micro to nano-size scaled, on the fire behaviour of an epoxy resin and its carbon fibre reinforced composites was assessed by cone calorimetry. The performance was compared not only regarding the reaction to fire performance, but also in terms of thermal stability, glass transition temperature and microstructure. Regarding the fire reaction behaviour of nanofilled epoxy resin, anionic nanoclays and thermally oxidized carbon nanotubes showed the best results, in agreement with more compact chars formed on the surface of the burning polymer. For carbon fibre reinforced composite plates, the cone calorimeter results of modified resin samples did not show significant improvements on the heat release rate curves. Poorly dispersed fillers in the resin additionally caused reductions on the glass transition temperature of the composite materials. KW - Epoxy resin KW - Carbon fibre reinforced composite KW - Nanoclays KW - Carbon nanotubes KW - Flame retardants PY - 2017 DO - https://doi.org/10.1002/fam.2370 SN - 1099-1018 SN - 0308-0501 VL - 41 IS - 2 SP - 111 EP - 130 PB - Wiley & Sons, Ltd. AN - OPUS4-39085 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leng, Jing A1 - Kang, N. A1 - Wang, D.-Y. A1 - Wurm, Andreas A1 - Schick, C. A1 - Schönhals, Andreas T1 - Crystallization behavior of nanocomposites based on poly(L-lactide) and MgAl layered double hydroxides - Unbiased determination of the rigid amorphous phases due to the crystals and the nanofiller N2 - Semicrystalline polymers have to be described by a three phase model consisting of a mobile amorphous (MAF), a crystalline (CF), and a rigid amorphous fraction (RAF). For nanocomposites based on a semicrystalline polymer the RAF is due to both the crystallites (RAFcrystal) and the filler (RAFfiller). Polymer nanocomposite based on poly(L-lactide) and MgAl layered double hydroxide nanofiller were prepared. Due to the low crystallization rate of PLA ist crystallization can be suppressed by a high enough cooling rate, and the RAF is due only to the nanofiller. The MAF, CF, and RAF were estimated by Temperature Modulated DSC. For the first time CF, MAF, RAFcrystal, and RAFfiller could be estimated. It was found, that RAFfiller increases linearly with the concentration of the nanofiller for this system. Furthermore, RAFcrystal is only slightly influenced by the presence of the nanofiller. KW - Polymer based nanocomposites PY - 2017 DO - https://doi.org/10.1016/j.polymer.2016.11.065 SN - 0032-3861 SN - 1873-2291 VL - 108 SP - 257 EP - 264 PB - Elesevier AN - OPUS4-39052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Höhm, S. A1 - Rosenfeld, A. A1 - Krüger, Jörg A1 - Bonse, Jörn T1 - Laser-induced periodic surface structures on zinc oxide crystals upon two-colour femtosecond double-pulse irradiation N2 - In order to study the temporally distributed energy deposition in the formation of laser-induced periodic surface structures (LIPSS) on single-crystalline zinc oxide (ZnO), two-colour double-fs-pulse experiments were performed. Parallel or cross-polarised double-pulse sequences at 400 and 800 nm wavelength were generated by a Mach–Zehnder interferometer, exhibiting inter-pulse delays up to a few picoseconds between the sub-ablation 50-fs-pulses. Twenty two-colour double-pulse sequences were collinearly focused by a spherical mirror to the sample surface. The resulting LIPSS periods and areas were analysed by scanning electron microscopy. The delay-dependence of these LIPSS characteristics shows a dissimilar behaviour when compared to the semiconductor silicon, the dielectric fused silica, or the metal titanium. A wavelength-dependent plasmonic mechanism is proposed to explain the delay-dependence of the LIPSS on ZnO when considering multi-photon excitation processes. Our results support the involvement of nonlinear processes for temporally overlapping pulses. These experiments extend previous two-colour studies on the indirect semiconductor silicon towards the direct wide band-gap semiconductor ZnO and further manifest the relevance of the ultrafast energy deposition for LIPSS formation. KW - Laser-induced periodic surface structures, LIPSS KW - Laser ablation KW - Surface plasmon polariton PY - 2017 DO - https://doi.org/10.1088/1402-4896/aa5578 SN - 1402-4896 SN - 0031-8949 VL - 92 IS - 3 SP - Article 034003, 1 EP - 7 PB - IOP CY - Bristol, UK AN - OPUS4-39082 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Winkelmann, Aimo T1 - Crystallometric and projective properties of Kikuchi diffraction patterns N2 - Kikuchi diffraction patterns can provide fundamental information about the lattice metric of a crystalline phase. In order to improve the possible precision and accuracy of lattice parameter determination from the features observed in Kikuchi patterns, some useful fundamental relationships of geometric crystal-lography are reviewed, which hold true independently of the actual crystal symmetry. The Kikuchi band positions and intersections and the Kikuchi band widths are highly interrelated, which is illustrated by the fact that all lattice plane trace positions of the crystal are predetermined by the definition of only four traces. If, additionally, the projection centre of the gnomonic projection is known, the lattice parameter ratios and the angles between the basis vectors are fixed. A further definition of one specific Kikuchi band width is sufficient to set the absolute sizes of all lattice parameters and to predict the widths of all Kikuchi bands. The mathematical properties of the gnomonic projection turn out to be central to an improved interpretation of Kikuchi pattern data, emphasizing the importance of the exact knowledge of the projection centre. KW - EBSD KW - Crystallography KW - Kikuchi patterns KW - Projective geometry PY - 2017 DO - https://doi.org/10.1107/S1600576716017477 SN - 1600-5767 VL - 50 IS - Part 1 SP - 102 EP - 119 PB - International Union of Crystallography AN - OPUS4-39061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unnikrishnakurup, Sreedhar A1 - Rouquette, Sebastien A1 - Soulie, Fabien A1 - Fras, Gilles T1 - Estimation of heat flux parameters during static gas tungsten arc welding spot under argon shielding N2 - A multi-physics modelling of a static Gas Tungsten Arc Welding (GTAW) operation has been established in order to estimate the heat flux exchanged between the arc plasma and the work-piece. The heat flux was described with a Gaussian function where two parameters required to be estimated: process efficiency and radial distribution. An inverse heat transfer problem (ihtp) has been developed in the aim to estimate these parameters from experimental data. Levenberg-Marquardt algorithm was used as the regularization method in addition to an iterative process. The experiment consisted in a static spot weld with GTAW process. The weld spot was on for 5 s under Argon shielding gas, 2.4 mm pure tungsten electrode on a SS304L disc. Temperatures were measured with thermocouples and weld pool growth monitored with a high speed camera. The experimental data were used to solve the ihtp what led to values such as 0.7 for process efficiency and average radial distribution of 1.8 mm. KW - Gas tungsten arc welding KW - Numerical simulation of welding KW - Heat flux estimation KW - Inverse heat transfer problem PY - 2017 DO - https://doi.org/10.1016/j.ijthermalsci.2016.12.008 SN - ISSN 1290-0729 VL - 114 SP - 205 EP - 212 PB - Elsevier Masson SAS AN - OPUS4-38905 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Philippen, Jan A1 - Guguschev, Christo A1 - Klimm, Detlef ED - Kuech, Thomas F. ED - Feigelson, Robert R. ED - Nakajima, K. ED - Stringfellow, G.B. T1 - Single crystal fiber growth of cerium doped strontium yttrate, SrY2O4:Ce3+ N2 - First single crystal fibers of cerium doped Strontium yttrate were fabricated using the laser-heated pedestal growth technique. Through thermodynamic Equilibrium calculations and by high-temperature mass spectrometry suitable growth conditions could be determined. The atmosphere played an important role during crystallization. It affected the composition shift, on the one hand, and the valence state of cerium, on the other hand. These dependencies can be explained by combining X-ray diffraction, elemental analysis, and optical spectroscopy. Crystallization in slightly reducing nitrogen atmosphere proved to be a reasonable choice, because evaporation is suppressed and trivalent cerium is stabilized. Strong green emission that depends on the Oxygen fugacity during crystallization could be excited using UV light. Optical properties of SrY2O4:Ce3+ were measured for the first time. KW - Laser heated pedestal growth KW - Oxides KW - Strontium yttrate KW - Single crystal fiber KW - LED phosphors PY - 2017 DO - https://doi.org/10.1016/j.jcrysgro.2016.11.033 SN - 0022-0248 SN - 1873-5002 VL - 459 SP - 17 EP - 22 PB - Elsevier CY - Amsterdam AN - OPUS4-39496 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ho, Y.T. A1 - Adriani, G A1 - Beyer, Sebastian A1 - Nhan, P.-T. A1 - Kamm, R. D. A1 - Kah, J.C.Y. T1 - A facile method to probe the vascular permeability of nanoparticles in nanomedicine applications N2 - The effectiveness of nanoparticles (NP) in nanomedicine depends on their ability to extravasate from vasculature towards the target tissue. This is determined by their permeability across the endothelial barrier. Unfortunately, a quantitative study of the diffusion permeability coefficients (Pd) of NPs is difficult with in vivo models. Here, we utilize a relevant model of vascular-tissue interface with tunable endothelial permeability in vitro based on microfluidics. Human umbilical vein endothelial cells (HUVECs) grown in microfluidic devices were treated with Angiopoietin 1 and cyclic adenosine monophosphate (cAMP) to vary the Pd of the HUVECs monolayer towards fluorescent polystyrene NPs (pNPs) of different sizes, which was determined from image analysis of their fluorescence intensity when diffusing across the monolayer. Using 70 kDa dextran as a probe, untreated HUVECs yielded a Pd that approximated tumor vasculature while HUVECs treated with 25 μg/mL cAMP had Pd that approximated healthy vasculature in vivo. As the size of pNPs increased, its Pd decreased in tumor vasculature, but remained largely unchanged in healthy vasculature, demonstrating a trend similar to tumor selectivity for smaller NPs. This microfluidic model of vascular-tissue interface can be used in any laboratory to perform quantitative assessment of the tumor selectivity of nanomedicine-based systems. KW - Nanoparticle PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-397053 DO - https://doi.org/10.1038/s41598-017-00750-3 SN - 2045-2322 VL - 7 IS - 1 SP - Article 707, 1 EP - 13 PB - Macmillan AN - OPUS4-39705 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nguyen, Thi Yen A1 - Roessler, Ernst A1 - Rademann, Klaus A1 - Emmerling, Franziska T1 - Control of organic polymorph formation: crystallization pathways in acoustically levitated droplets N2 - Theoretical and experimental studies indicate that crystal nucleation can take more complex pathways than expected on the ground of the classical nucleation theory. Among these pathways are the formation of pre-nucleation clusters and amorphous precursor phases. A direct in situ observation of the different pathways of nucleation from solution is challenging since the paths can be influenced by heterogeneous nucleation sites, such as container walls. Here, we provide insights into the crystallization process using the in situ combination of an acoustic levitator, Raman spectroscopy, and X-ray scattering. The contactless sample holder enables the observation of homogeneous crystallization processes and the detection of intermediates and final crystalline forms. We provide evidence for the existence of multiple pathways of nucleation based on the investigation of the crystallization of organic molecules from different solvents. Starting from a diluted solution, a supersaturation is reached during the experiment due to the evaporation of the solvent. The highly supersaturated solution reveals different pathways of crystallization. Depending on the degree of supersaturation either the thermodynamically stable or the metastable crystal form is observed. KW - Crystallization KW - In situ XRD KW - Polymorphism KW - Polyamorphism KW - Raman spectroscopy PY - 2017 DO - https://doi.org/10.1515/zkri-2016-1964 SN - 2194-4946 SN - 2196-7105 VL - 232 IS - 1-3 SP - 15 EP - 24 PB - De Gruyter CY - Berlin AN - OPUS4-39708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilrich, Thomas A1 - Wilrich, Cordula T1 - Der Brand des Zinkklumpens im Restmülleimer N2 - In dieser Veröffentlichung werden der Strafbefehl und das in der Revision erfolgte Urteil zu einem Unfall im Chemieunterricht diskutiert. Der Strafbefehl: Sie werden "beschuldigt, fahrlässig eine Räumlichkeit, die zeitweise dem Aufenthalt von Menschen dient, zu einer Zeit, in der Menschen sich dort aufzuhalten pflegen, in Brand gesetzt oder durch eine Brandlegung ganz oder teilweise zerstört, indem Sie, nachdem Sie in Ihrer Eigenschaft als Chemielehrer des X-Gymnasiums in Y am Morgen des vorgenannten Tages im Chemieunterricht Schülern ein Experiment vorgeführt hatten, bei dem Sie Zinkpulver mit Natronlauge reagieren ließen, gegen 9:20 Uhr die für das Experiment benutzten Gläser sowie den entstandenen Zinkklumpen im Chemievorbereitungsraum mit Säure neutralisierten sowie mit Wasser abspülten, den Zinkklumpen sodann jedoch einfach in einem Kunststoffmülleimer entsorgten, welcher sich dort entzündete, was zu einem Brand im Chemievorbereitungsraum führte, bei dem diverse Möbelstücke samt Laborutensilien durch das Feuer zerstört wurden, es zu lokalen Gebäudeschäden durch abgeplatzten Wand- und Deckenputz kam und die Räumlichkeiten großflächig durch Rauchgasniederschläge belastet wurden, was Sie als Chemielehrer aufgrund Ihrer besonderen Fachkenntnisse hätten vorhersehen können und müssen; die Kosten der notwendigen Sanierungsmaßnahmen betragen € 66.647,26". Sodann heißt es, dass "auf Antrag der Staatsanwaltschaft gegen Sie eine Geldstrafe von 50 Tagessätzen festgesetzt wird. Die Höhe eines Tagessatzes beträgt € 100,–, die Geldstrafe insgesamt mithin € 5.000,–". Das Urteil: Der Lehrer erhob gegen den Strafbefehl Einspruch und das Amtsgericht sprach ihn nach mündlicher Verhandlung mit Urteil vom 8. Juli 2015 frei. In der vorliegenden Veröffentlichung werden der Strafbefehl und das Urteil im Hinblick auf Pflichtwidrigkeit, Kausalität und Fahrlässigkeit diskutiert. Darüberhinaus wird besprochen, ob die zugrunde gelegte Arbeitsschutzvorschrift angemessen angewendet und vom Gericht korrekt interpretiert wurde. KW - Arbeitsschutz KW - Entsorgung gefährlicher Stoffe PY - 2017 DO - https://doi.org/10.37307/j.2365-7634.2017.04.10 SN - 2365-7626 IS - 4 SP - 176 EP - 178 PB - Erich Schmidt Verlag (ESV) CY - Berlin AN - OPUS4-39645 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulz, K. A1 - Schmack, R. A1 - Klemm, H. W. A1 - Kabelitz, Anke A1 - Schmidt, T. A1 - Emmerling, Franziska A1 - Kraehnert, R. T1 - Mechanism and kinetics of hematite crystallization in air: Linking bulk and surface models via mesoporous films with defined nanostructure N2 - Iron can form numerous oxides, hydroxides, and oxide−hydroxides. Despite their relevance, many of the transformation processes between these phases are still poorly understood. In particular the crystallization of quasi-amorphous hydroxides and oxide−hydroxides is difficult to assess, since typical diffraction and scattering methods provide only sampleaveraged information about the crystallized phases. We report a new approach for the investigation of the crystallization of oxide−hydroxides. The approach relies on model-type films that comprise a defined homogeneous nanostructure. The nanostructure allows quantitative linking of Information obtained by bulk-averaging diffraction techniques (XRD, SAXS) with locally resolved information, i.e., Domain sizes (SEM, TEM, LEEM) and phase composition (SAED). Using time-resolved imaging and diffraction we deduce mechanism and kinetics for the crystallization of ferrihydrite into hematite. Hematite forms via nucleation of hematite domains and subsequent Domain growth that terminates only upon complete transformation. A Johnson−Mehl−Avrami−Kolmogorov model describes the kinetics over a wide temperature range. The derived understanding enables the first synthesis of ferrihydrite films with ordered mesoporosity and quantitative control over the films’ hematite and ferrihydrite content. KW - Iron oxide KW - Crystallization KW - Mesoporous films KW - Nanostructure PY - 2017 DO - https://doi.org/10.1021/acs.chemmater.6b05185 SN - 0897-4756 SN - 1520-5002 VL - 29 IS - 4 SP - 1724 EP - 1734 AN - OPUS4-39690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Hielscher, R. A1 - Winkelmann, Aimo T1 - Electron backscatter diffraction beyond the mainstream N2 - We present special applications of electron backscatter diffraction (EBSD) which aim to overcome some of the limitations of this technique as it is currently applied in the scanning electron microscope. We stress that the raw EBSD signal carries additional information which is useful beyond the conventional orientation determination. The background signal underlying the backscattered Kikuchi diffraction (BKD) patterns reflects the chemical composition and surface topography but also contains channeling-in information which is used for qualitative real-time orientation imaging using various backscattered electron signals. A significantly improved orientation precision can be achieved when dynamically simulated pattern are matched to the experimental BKD patterns. The breaking of Friedel’s rule makes it possible to obtain orientation mappings with respect to the point-group symmetries. Finally, we discuss the determination of lattice parameters from individual BKD patterns. Subgrain structure in a single quartz grain. The increased noise level in the left map reflects the lower precision of a standard orientation determination using band detection by the Hough transform. The right map results from the same experimental raw data after orientation refinement using a pattern matching approach. The colors correspond an adapted inverse pole figure color key with a maximum angular deviation of about 2° from the mean orientation. KW - Electron backscatter diffraction PY - 2017 DO - https://doi.org/10.1002/crat.201600252 SN - Online 1521-4079 VL - 52 IS - 1 SP - Special Issue - Article Number: UNSP 1600252, 1 EP - 24 PB - WILEY-VCH AN - OPUS4-37935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martin, S. A1 - Walnsch, A. A1 - Nolze, Gert A1 - Leineweber, A. A1 - Léaux, F. A1 - Scheuerlein, C. T1 - The crystal structure of (Nb0.75Cu0.25)Sn-2 in the Cu-Nb-Sn system N2 - During the processing of superconducting Nb3Sn wire, several intermediate intermetallic phases including a previously encountered Cu-Nb-Sn phase show up. The yet unknown crystal structure of this phase is now identified by a combination of different experimental techniques and database search to be of the hexagonal NiMg2 type with a proposed composition of about (Nb0.75Cu0.25)Sn2. The structure determination started from an evaluation of the lattice parameters from EBSD Kikuchi patterns from quenched material suggesting hexagonal or orthorhombic symmetry. A database search then led to the hexagonal NiMg2 type structure, the presence of which was confirmed by a Rietveld analysis on the basis of high energy synchrotron X-ray powder diffraction data. Assuming a partial substitution of Nb in orthorhombic NbSn2 by Cu, the change of the valence electron concentration provokes a structural transformation from the CuMg2 type for NbSn2 to the NiMg2 type for (Nb0.75Cu0.25)Sn2. In the previous literature the (Nb0.75Cu0.25)Sn2 phase described here has occasionally been referred to as Nausite. KW - Electron backscatter diffraction KW - X-ray diffraction KW - Intermetallic compound KW - Structure solution KW - Superconductor PY - 2017 DO - https://doi.org/10.1016/j.intermet.2016.09.008 SN - 0966-9795 SN - 1879-0216 VL - 80 SP - 16 EP - 21 PB - Elsevier Ltd. AN - OPUS4-37874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heck, Christian A1 - Prinz, Julia A1 - Dathe, A. A1 - Merck, V. A1 - Stranik, O. A1 - Fritzsche, W. A1 - Kneipp, Janina A1 - Bald, Ilko T1 - Gold nanolenses self-assembled by DNA origami N2 - Nanolenses are self-similar chains of metal nanoparticles, which can theoretically provide extremely high field enhancements. Yet, the complex structure renders their synthesis challenging and has hampered closer analyses so far. Here, DNA origami is used to self-assemble 10, 20, and 60 nm gold nanoparticles as plasmonic gold nanolenses (AuNLs) in solution and in billions of copies. Three different geometrical arrangements are assembled, and for each of the three designs, surface-enhanced Raman scattering (SERS) capabilities of single AuNLs are assessed. For the design which shows the best properties, SERS signals from the two different internal gaps are compared by selectively placing probe dyes. The highest Raman enhancement is found for the gap between the small and medium nanoparticle, which is indicative of a cascaded field enhancement. KW - DNA origami KW - SERS KW - Gold nanoparticles KW - Plasmonics PY - 2017 UR - http://pubs.acs.org/doi/pdf/10.1021/acsphotonics.6b00946 DO - https://doi.org/10.1021/acsphotonics.6b00946 SN - 2330-4022 VL - 4 IS - 5 SP - 1123 EP - 1130 AN - OPUS4-40587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottlieb, Cassian A1 - Millar, Steven A1 - Grothe, S. A1 - Wilsch, Gerd T1 - 2D evaluation of spectral LIBS data derived from heterogeneous materials using cluster algorithm N2 - Laser-induced Breakdown Spectroscopy (LIBS) is capable of providing spatially resolved element maps in regard to the chemical composition of the sample. The evaluation of heterogeneous materials is often a challenging task, especially in the case of phase boundaries. In order to determine information about a certain phase of a material, the need for a method that offers an objective evaluation is necessary. This paper will introduce a cluster algorithm in the case of heterogeneous building materials (concrete) to separate the spectral information of non-relevant aggregates and cement matrix. In civil engineering, the information about the quantitative ingress of harmful species like Cl−, Na+ and SO2−4 is of great interest in the evaluation of the remaining lifetime of structures (Millar et al., 2015; Wilsch et al., 2005). These species trigger different damage processes such as the alkali-silica reaction (ASR) or the chloride-induced corrosion of the reinforcement. Therefore, a discrimination between the different phases, mainly cement matrix and aggregates, is highly important (Weritz et al., 2006). For the 2D evaluation, the expectation-maximizationalgorithm (EM algorithm; Ester and Sander, 2000) has been tested for the application presented in this work. The method has been introduced and different figures of merit have been presented according to recommendations given in Haddad et al. (2014). Advantages of this method will be highlighted. After phase separation, non-relevant information can be excluded and only the wanted phase displayed. Using a set of samples with known and unknown composition, the EM-clustering method has been validated regarding to Gustavo González and Ángeles Herrador (2007). KW - LIBS KW - Concrete KW - EM-clustering KW - Heterogeneity PY - 2017 DO - https://doi.org/10.1016/j.sab.2017.06.005 SN - 0584-8547 VL - 2017 IS - 134 SP - 58 EP - 68 PB - Elsevier B.V. AN - OPUS4-40644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maierhofer, Christiane A1 - Krankenhagen, Rainer A1 - Röllig, Mathias A1 - Rehmer, Birgit A1 - Gower, M. A1 - Baker, G. A1 - Lodeiro, M. A1 - Aktas, A. A1 - Monte, C. A1 - Adibekyan, A. A1 - Gutschwager, B. T1 - Defect characterisation of tensile loaded CFRP and GFRP laminates used in energy applications by means of infrared thermography N2 - The increased use of fibre reinforced plastic (FRP) composites for improved efficiency and reliability in energy related applications, e.g. wind and marine turbine blades, nacelles, oil and gas flexible risers, also increases the demand for innovative non-destructive testing technologies. In this contribution, results concerning the characterisation of CFRP and GFRP during and after quasi-static tensile loading are presented. It includes the measurement of optical properties in the infrared spectral range, tensile loading tests with the observation of the temperature distribution at one or both sides of the specimens using an infrared camera for the preparation and monitoring of intended natural defects, and active thermography inspections after tensile loading. It is shown that the defect preparation was successful. Thermographic monitoring during and active thermography testing after tensile loading enable the detection of the lateral extend of the generated defects. Differences between CFRP and GFRP materials are discussed. KW - Tensile loading KW - Fibre reinforced composites KW - Active and passive thermography KW - Emissivity PY - 2017 DO - https://doi.org/10.1080/17686733.2017.1334312 SN - 1768-6733 SN - 2116-7176 VL - 15 IS - 1 SP - 17 EP - 36 PB - Taylor and Francis CY - London AN - OPUS4-40968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröder, Volkmar A1 - Molnarne, Maria T1 - Flammability of gases in focus of European and US standards N2 - The presentation will discuss the difference between EU and US standards for the determination of explosion (flammability) limits and limiting oxygen concentration. Small differences observed in measured values can be traced back to the different test apparatuses and criteria. The discrepancies can be much greater in the case of limiting oxygen concentration because of the high amount of inert gases and the corresponding low laminar burning velocities. The paper describes some examples and the influence of the chosen criteria on the results. The European and US standards use the criteria of flame propagation in open test vessels and of pressure rise in closed ones. The examples discussed show that flame propagation is still possible at very small pressure rise values, as observed much below the pressure rise criterion of usual standards. However, flame propagation in a process plant can cause an accident or explosion and must be avoided. Therefore, the flame propagation criterion is recommended to be used in chemical safety engineering. The European safety database CHEMSAFE contains expertevaluated safety data for cases where the determination method and criteria are known. Flammability characteristics based on the pressure rise criterion may suffice in certain cases, e.g. for explosion protection in closed vessels without any connecting pipes. KW - Flammability KW - Limiting oxygen concentration KW - Test methods KW - Standards PY - 2017 DO - https://doi.org/10.1016/j.jlp.2017.05.012 SN - 0950-4230 SN - 1873-3352 VL - 48 SP - 297 EP - 304 PB - Elsevier CY - Amsterdam AN - OPUS4-40980 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krütt, Enno T1 - Ermüdungsbedingte Degradation von Fahrbahnbeton - Einfluss auf den Stofftransport T1 - Fatigue-induced degradation of deck concrete influence on the material transport N2 - In den letzten 15 Jahren hat im deutschen Autobahnnetz die Anzahl von Schäden an Betonfahrbahnen, die vor 2005 er-richtet wurden zugenommen. Dies führt oft zu einer Vermin-derung der Lebensdauer von 30 auf 10 bis 15 Jahre. Trotz umfassender Untersuchungen wurde die Ursache bis jetzt nicht eindeutig geklärt, jedoch scheint die Alkali-Kieselsäure-Reaktion (AKR) hierbei eine Rolle zu spielen. Vor diesem Hintergrund wurden AKR-Performance-Tests entwickelt, die jedoch die mechanischen Einwirkungen aus Klima und Ver-kehr nicht berücksichtigen. Aus diesem Grund wurde eine AKR-Forschergruppe von der Deutschen Forschungsgemein-schaft ins Leben gerufen, welche sich experimentell und auf Simulationsebene mit diesem Thema befasst. Inhalt dieses Beitrages sind ausgewählte Ergebnisse des an der BAM bear-beiteten experimentellen Projektteils, welche in eine auf die Auswirkung einer mechanischen Degradation fokussierte Promotionsarbeit einfließen. Ziel der ausgewählten Untersuchung ist es, den Einfluss einer mechanisch induzierten Betondegradation auf den Stofftrans-port herauszuarbeiten. Hierzu wird ein großformatiger Balken einem zyklischen Vier-Punkt Biegezugversuch mit einer Anzahl von 5 Mio. Lastwechseln unterzogen. Während des Versuches findet ein Schadensmonitoring mit verschiedenen zerstörungsfreien Prüftechniken statt. Hierzu zählen Deh-nungsmessungen, Schallemissionsanalyse und Ultraschall-messungen. Nach dem zyklischen Belastungs-versuch werden kleinformatige Probekörper aus dem belasteten Balken entnommen. Als Referenz dienen unbelas-tete Probekörper aus der gleichen Herstellungscharge. Die Oberflächen der entnommenen Probekörper werden in einem kapillaren Saugversuch zum einen mit deionisiertem Wasser und zum anderen mit einer 3,6 %igen NaCl-Lösung beauf-schlagt. Während der Saugversuche dienen verschiedene zerstörungsfreie bzw. -arme Messmethoden dazu, die Feuch-teaufnahme bzw. -verteilung in den Probekörpern zu messen. Hierzu gehören neben der Gravimetrie die Messung mit NMR (Nuclear-Magnetic-Resonance) sowie TDR (Time-Domain-Reflectometry). Nach den Saugversuchen wird die Na- und Cl-Verteilung an den mit NaCl-Lösung beaufschlagten Pro-bekörpern zerstörend mittels LIBS (Laser-Induced-Breakdown-Spectroscopy) ermittelt. Erste Ergebnisse zeigen, dass die zyklische Ermüdungsdegradation den Stofftransport tendenziell verstärkt. KW - Degradation KW - Stofftransport KW - Fahrbahnbeton PY - 2017 SN - 0005-9900 SN - 1437-1006 VL - 112 IS - 7 SP - 458 EP - 458 AN - OPUS4-41097 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bochnig, M. S. A1 - Oh, M.-J. A1 - Nagel, T. A1 - Jost-Brinkmann, P.-G. A1 - Ziegler, Fred T1 - Comparison of the shock absorption capacities of different mouthguards N2 - In this in vitro study, the protective qualities of different mouthguard types were examined during small hard object collisions. The aim was to investigate inconclusive aspects of hard inserts, nylon nets, and air spaces as reinforcements in the anterior region and the protection qualities of ethylene vinyl acetate (EVA). Five different mouthguards with a labial thickness between 2 mm and 11 mm made of materials of varying stiffness were investigated. As a negative control, the same experiments were performed without a mouthguard. Different combinations of EVA and labial inserts ((polyethylene terephthalate glycol-modified [PETG]), nylon mesh, air space) were tested. Using a stainless steel pendulum device, blows of different energy (0.07-2.85 joules) were applied to the center of the crown of a pivoted tooth in a custom-built jaw model. A laser Doppler vibrometer measured the tooth deflection, while an acceleration sensor attached to the pendulum measured the braking accelerations. Tooth deflection was reduced up to 99.7% compared to no mouthguard, and the braking acceleration was reduced up to 72.2% by increasing the mouthguards' labial thickness in combination with labial inserts of different stiffness and a built-in air space between the front teeth and the mouthguard. The mouthguards made of soft materials (EVA with nylon mesh) showed slightly better protection qualities than the more rigid mouthguards of similar thickness (PETG; P<.05). However, with increasing impact energy, their protective capacities decreased to a greater extent than the stiffer mouthguards. The combination of increased labial thickness and labial inserts of varying stiffness and eventually an air space offers the best protection capacities for hard, small object collisions. KW - Shock absorbtion KW - Hard object collisions KW - Mouthguard PY - 2017 DO - https://doi.org/10.1111/edt.12324 SN - 1600-4469 VL - 33 IS - 3 SP - 205 EP - 213 PB - John Wiley & Sons, Ltd CY - Hoboken, NJ, USA AN - OPUS4-41098 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dutto, Paola A1 - Stickle, M. M. A1 - Pastor, M. A1 - Manzanal, D. A1 - Yague, A. A1 - Tayyebi, S. A1 - Lin, C. A1 - Elizalde, M. D. ED - Cervera, Miguel T1 - Modelling of fluidised geomaterials: the case of the Aberfan and the Gypsum tailings impoundment flowslides N2 - The choice of a pure cohesive or a pure frictional viscoplastic model to represent the rheological behaviour of a flowslide is of paramount importance in order to obtain accurate results for real cases. The principal Goal of the present work is to clarify the influence of the type of viscous model—pure cohesive versus pure frictional—with the numerical reproduction of two different real flowslides that occurred in 1966: the Aberfan flowslide and the Gypsum tailings impoundment flowslide. In the present work, a depth-integrated model based on the v-pw Biot–Zienkiewicz formulation, enhanced with a diffusion-like equation to account for the pore pressure Evolution within the soil mass, is applied to both 1966 cases. For the Aberfan flowslide, a frictional viscous model based on Perzyna viscoplasticity is considered, while a pure cohesive viscous model (Bingham model) is considered for the case of the Gypsum flowslide. The numerical approach followed is the SPH method, which has been enriched by adding a 1D finite difference grid to each SPH node in order to improve the description of the pore water evolution in the propagating mixture. The results obtained by the performed simulations are in agreement with the documentation obtained through the UK National Archive (Aberfan flowslide) and the International Commission of large Dams (Gypsum flowslide). KW - Aberfan flowslide KW - SPH KW - Landslide propagation modelling KW - Perzyna viscoplasticity PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-410493 DO - https://doi.org/10.3390/ma10050562 SN - 1996-1944 VL - 10 IS - 5 SP - 562, 1 EP - 562, 21 AN - OPUS4-41049 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kohler, C. A1 - Nikfalazar, M. A1 - Heunisch, Andreas A1 - Schulz, Bärbel A1 - Mikolajek, M. A1 - Rabe, Torsten A1 - Jakoby, R. A1 - Binder, J. T1 - Implementation of Ba0.6Sr0.4TiO3-ZnO-B2O3 based tunable microwave phase shifters in LTCC technology N2 - Tunable dielectric Ba0.6Sr0.4TiO3-ZnO-B2O3 thick-films were analyzed regarding their integration potential into the LTCC technology. Therefore, tunable loaded line phase shifters based on metal-insulator-metal varactors with single- and double- printed BST thick-films were fabricated and co-sintered inside a four layer LTCC module. Microstructural and chemical investigations showed a sufficient compatibility and adhesion between the silver, BST composite and LTCC layers and a resulting morphology depending on the processing route. The microwave characterization of the LTCC-embedded phase shifters revealed comparable results to phase shifters with the same design on alumina substrates. KW - Thick films KW - Dielectric materials KW - Electroceramics PY - 2017 DO - https://doi.org/10.1111/ijac.12687 SN - 1546-542X SN - 1744-7402 VL - 14 IS - 4 SP - 574 EP - 582 PB - Wiley CY - Hoboken, NY, USA AN - OPUS4-41086 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Daly, M. A1 - Burnett, T. L. A1 - Pickering, E. J. A1 - Tuck, O. C. G. A1 - Léonard, Fabien A1 - Kelley, R. A1 - Withers, P. J. A1 - Sherry, A. H. T1 - A multi-scale correlative investigation of ductile fracture N2 - The use of novel multi-scale correlative methods, which involve the coordinated characterisation of matter across a range of length scales, are becoming of increasing value to materials scientists. Here, we describe for the first time how a multi-scale correlative approach can be used to investigate the nature of ductile fracture in metals. Specimens of a nuclear pressure vessel steel, SA508 Grade 3, are examined following ductile fracture using medium and high-resolution 3D X-ray computed tomography (CT) analyses, and a site-specific analysis using a dual beam plasma focused ion beam scanning electron microscope (PFIB-SEM). The methods are employed sequentially to characterise damage by void nucleation and growth in one volume of interest, allowing for the imaging of voids that ranged in size from less than 100 nm to over 100 mm. This enables the examination of voids initiated at carbide particles to be detected, as well as the large voids initiated at inclusions. We demonstrate that this multi-scale correlative approach is a powerful tool, which not only enhances our understanding of ductile failure through detailed characterisation of microstructure, but also provides quantitative information about the size, volume fractions and spatial distributions of voids that can be used to inform models of failure. It isfound that the vast majority of large voids nucleated at MnS inclusions, and that the volume of a void varied according to the volume of its initiating inclusion raised to the power 3/2. The most severe voiding was concentrated within 500 mm of the fracture surface, but measurable damage was found to extend to a depth of at least 3 mm. Microvoids associated with carbides (carbide-initiated voids) were found to be concentrated around larger inclusion-initiated voids at depths of at least 400 mm. Methods for quantifying X-ray CT void data are discussed, and a procedure for using this data to calibrate parameters in the Gurson-Tvergaard Needleman (GTN) model for ductile failure is also introduced. KW - Gurson model KW - SA508 KW - Correlative tomography KW - Void nucleation & growth KW - X-ray computed tomography PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-414547 UR - http://www.sciencedirect.com/science/article/pii/S1359645417302203?via%3Dihub DO - https://doi.org/10.1016/j.actamat.2017.03.028 VL - 130 SP - 56 EP - 68 PB - Elsevier AN - OPUS4-41454 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Kabelitz, Anke A1 - Zimathies, Annett A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Crystal structure and in situ investigation of a mechanochemical synthesized 3D zinc N-(phosphonomethyl)glycinate N2 - The mechanochemical synthesis of the zinc N-(phosphonomethyl)glycinate Zn(O₃PCH₂NH₂CH₂CO₂) H₂O is presented. The structure was solved from powder X-ray diffraction (PXRD) data. In the three-dimensional pillared structure, the Zn atoms are coordinated tetrahedrally. In situ investigations of the reaction process with synchrotron PXRD and Raman spectroscopy reveal a two-step process including the formation of an intermediate. KW - Mechanochemistry KW - Metal phosphonate KW - In situ PY - 2017 DO - https://doi.org/10.1007/s10853-017-1121-7 SN - 0022-2461 SN - 1573-4803 VL - 52 IS - 20 SP - 12013 EP - 12020 PB - Springer CY - New York AN - OPUS4-41490 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matoga, D. A1 - Roztocki, K. A1 - Wilke, Manuel A1 - Emmerling, Franziska A1 - Oszajca, M. A1 - Fitta, M. A1 - Bałanda, M. T1 - Crystalline bilayers unzipped and rezipped: solid-state reaction cycle of a metal–organic framework with triple rearrangement of intralayer bonds N2 - We present a series of remarkable structural transformations for a family of layered metal–organic frameworks (MOFs) in a three-step solid-state reaction cycle. The cycle represents new dynamic behavior of 2D coordination polymers and involves the sequence of reactions: {[Mn2(ina)4(H2O)2]·2EtOH}n (JUK-1) → {(NH4)2[Mn(ina)2(NCS)2]}n·xH2O (JUK-2) → {[Mn2(ina)2(Hina)2(NCS)2]}n (JUK-3) → JUK-1 (Hina = isonicotinic acid), each accompanied by rearrangement of intralayer coordination bonds and each induced by a different external stimulus. In situ investigation of the first step of the cycle by combined synchrotron X-ray diffraction and Raman spectroscopy reveals direct mechanochemical unzipping of JUK-1 bilayers to respective JUK-2 layers with reaction rates dependent on the milling conditions. In contrast, the reverse zipping of JUK-2 layers involves two steps and proceeds through a new MOF (JUK-3) whose structure was elucidated by powder X-ray diffraction. Magnetic measurements confirm conversions of manganese nodes in the reaction cycle. The findings indicate the possibility of developing coordination-based assemblies with large structural responses for use in smart stimuli-responsive systems and sensor technologies. KW - Mechanochemistry KW - In situ KW - XRD KW - MOF PY - 2017 UR - http://pubs.rsc.org/is/content/articlehtml/2017/ce/c7ce00655a DO - https://doi.org/10.1039/C7CE00655A VL - 19 SP - 2987 EP - 2995 AN - OPUS4-41517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moldenhauer, Laura A1 - Helmerich, Rosemarie A1 - Köppe, Enrico A1 - Haamkens, Frank A1 - Wittmann, Jochen ED - Emri, Igor T1 - Experimental feasibility study about moisture in building materials measured with Bluetooth N2 - Structural health monitoring contributes to early damage detection in the built infrastructure. During the last two decades, sensor networks transferred from wired to wireless sensor networks. Several methods exist to measure moisture in building materials. Most of the introduced commercial moisture measurement methods provide information about the local or near surface moisture. A feasibility study is presented to demonstrate, how the Received Signal Strength Indicator (RSSI) of a Bluetooth Low Energy (BLE) signal, transmitted from the BLE-module embedded in building materials, correlate with changing moisture content. The feasibility of this influence was investigated in the presented study. The maximum and minimum RSSI were systematically recorded and analysed. T2 - 33nd Danubia Adria Symposium on Advances in Experimental Mechanics CY - Portoroz, Slovenia DA - 20.09.2016 KW - BLE KW - Long-Term Monitoring KW - Network KW - Structural Health Monitoring KW - Moisture Measurement KW - RSSI KW - Bluetooth Low Energy KW - Sensor PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S2214785317308398 DO - https://doi.org/10.1016/j.matpr.2017.06.053 SN - 2214-7853 VL - 4 IS - 5, Part 1 SP - 5889 EP - 5892 PB - Elsevier Ltd. AN - OPUS4-41585 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schumacher, David A1 - Antin, K.-N. A1 - Zscherpel, Uwe A1 - Vilaça, P. T1 - Application of different X-ray techniques to improve in-service carbon fiber reinforced rope inspection N2 - Carbon fiber reinforced polymer ropes are gaining in significance in the fields of civil engineering and hoisting applications. Thus, methods of non-destructive testing (NDT) need to be developed and evaluated with respect to new challenges and types of defects. Particularly important is the development of in-service testing solutions which allow the integration in global online monitoring systems. Conventional methods like electrical resistivity or strain measurements using optical fibers are already in use. This study investigates the possibility of using various X-ray techniques to increase the reliability and significance of NDT and their applicability to in-service testing. Conventional film radiography is the most common technique; however, even after image enhancement of the digitized film, this technique lacks contrast sensitivity and dynamic range compared to digital detector array (DDA) radiography. The DDA radiography is a highly sensitive method; yet, the limitation is that it delivers 2D images of 3D objects. By the use of co-planar translational laminography the detectability of planar defects is superior to 2D methods due to multiple projection angles. Apart from this, it can be used on-site due to a rather simple setup and robust equipment. In this work two photon counting detectors (PCD) with different sensor materials (Si and CdTe) were used. The results show that the resolution and defect recognition is lower in case of DDA radiography and laminography using PCDs compared to high-resolution computed tomography. However, the DDA radiography and laminography are sensitive enough to both fiber breakage and delaminations and can be significantly advantageous in terms of measurement time and adaptability for on-site monitoring. KW - X-ray imaging KW - Digital radiography KW - Co-planar translational laminography KW - Computed tomography KW - Photon counting detectors KW - Carbon fiber reinforced polymer KW - Rope PY - 2017 DO - https://doi.org/10.1007/s10921-017-0441-5 SN - 0195-9298 SN - 1573-4862 VL - 36 IS - 4 SP - Paper 62, 1 PB - Springer International Publishing AG CY - Cham, Switzerland AN - OPUS4-41781 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Poyet, S. A1 - Dridi, W. A1 - L'Hostis, V. A1 - Meinel, Dietmar T1 - Microstructure and diffusion coefficient of an old corrosion product layer and impact on steel rebar corrosion in carbonated concrete N2 - Corrosion is the major degradation pathway affecting reinforced concrete structures. In the long-term, the rust layer might become thick and slow down the diffusion of oxygen from the atmosphere to the steel. With this in mind, the mineralogy, microstructure and diffusion properties of an old and thick corrosion product layer were investigated. Despite the presence of macropores, the gas diffusion coefficient was found to be low. The impact of the layer on the oxygen diffusion was evaluated using Fick’s law. The results showed that the layer could reduce the flux of oxygen only in a specific configuration. KW - Steel reinforced concrete KW - Rust KW - X-ray computed tomography KW - Micro-CT PY - 2017 DO - https://doi.org/10.1016/j.corsci.2017.06.002 VL - 2017 IS - 125 SP - 48 EP - 58 PB - Elsevier B.V. CY - Radarweg 29, 1043 NX Amsterdam, The Netherlands AN - OPUS4-41784 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, Anja A1 - Kranzmann, Axel A1 - Wolthusen, Helmut T1 - Unusual Corrosion Behavior of 1.4542 Exposed a Laboratory Saline Aquifer Water CCS-Environment N2 - Differently heat treated coupons of 1.4542 were kept at T=60 °C and ambient pressure as well as p=100 bar for 700 h - 8000 h in an a) water saturated supercritical CO2 and b) CO2-saturated synthetic aquifer environment similar to on-shore CCS-sites in the Northern German Basin. Surface corrosion layers are homogeneous but unusually discontinuously ellipsoidal. After 8000 h at 100 bar maximum corrosion rate in the liquid phase is approximately 0.014 mm/year, with normalizing providing best corrosion resistance and approximately 0.003 mm/year in the supercritical phase where hardening+tempering at 670 °C leads to lowest corrosion rates. KW - CO2-storage KW - Supercritical CO2 KW - Steel KW - Pipeline KW - Corrosion KW - CCS PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-418472 DO - https://doi.org/10.1016/j.egypro.2017.03.1679 VL - 114 SP - 5229 EP - 5240 PB - Elsevier Ltd. AN - OPUS4-41847 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Taabache, Soraya A1 - Bertin, Annabelle T1 - Vesicles from amphiphilic dumbbells and Janus dendrimers: bioinspired self-assembled structures for biomedical applications N2 - The current review focuses on vesicles obtained from the self-assembly of two types of dendritic macromolecules, namely amphiphilic Janus dendrimers (forming dendrimersomes) and amphiphilic dumbbells. In the first part, we will present some synthetic strategies and the various building blocks that can be used to obtain dendritic-based macromolecules, thereby showing their structural versatility. We put our focus on amphiphilic Janus dendrimers and amphiphilic dumbbells that form vesicles in water but we also encompass vesicles formed thereof in organic solvents. The second part of this review deals with the production methods of these vesicles at the nanoscale but also at the microscale. Furthermore, the influence of various parameters (intrinsic to the amphiphilic JD and extrinsic—from the environment) on the type of vesicle formed will be discussed. In the third part, we will review the numerous biomedical applications of these vesicles of nano- or micron-size. KW - Janus dendrimers KW - Amphiphilic dumbbells KW - Self-assembled structures KW - Dendrimersomes KW - Artificial cells PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-418245 DO - https://doi.org/10.3390/polym9070280 SN - 2073-4360 VL - 9 IS - 7 SP - Article 280, 1 EP - 36 AN - OPUS4-41824 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hentrich, D. A1 - Taabache, Soraya A1 - Brezesinski, G. A1 - Lange, Nele A1 - Unger, Wolfgang A1 - Kübel, C. A1 - Bertin, Annabelle A1 - Taubert, A. T1 - A dendritic amphiphile for efficient control of biomimetic calcium phosphate mineralization N2 - The phase behavior of a dendritic amphiphile containing a Newkome-type dendron as the hydrophilic moiety and a cholesterol unit as the hydrophobic segment is investigated at the air–liquid interface. The amphiphile forms stable monomolecular films at the air–liquid interface on different subphases. Furthermore, the mineralization of calcium Phosphate beneath the monolayer at different calcium and phosphate concentrations versus mineralization time shows that at low calcium and Phosphate concentrations needles form, whereas flakes and spheres dominate at higher concentrations. Energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, and electron diffraction confirm the formation of calcium phosphate. High-resolution transmission electron microscopy and electron diffraction confirm the predominant formation of octacalcium phosphate and hydroxyapatite. The data also indicate that the final products form via a complex multistep reaction, including an association step, where nano-needles aggregate into larger flake-like objects. KW - Dendritic amphiphile KW - Calcium phosphate KW - Biomineralization PY - 2017 DO - https://doi.org/10.1002/mabi.201600524 SN - 1616-5187 SN - 1616-5195 VL - 17 IS - 8 SP - Article 1600524, 1 EP - 14 AN - OPUS4-41825 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stelzner, Ludwig A1 - Powierza, Bartosz T1 - Thermisch induzierter Feuchtetransport in HPC T1 - Thermally induced Moisture Transport in structure density High-performance Concrete N2 - Die Entwicklung von leistungsfähigen Fließmitteln in den letzten Jahrzehnten ermöglicht die Herstellung von Beton mit sehr geringem w/z-Wert, bei gleichzeitig guter Verarbeitbar-keit. Die Reduzierung des w/z-Wertes geht dabei mit einer Erhöhung der Festigkeit und einer Verdichtung der Gefü-gestruktur einher. Aufgrund der hohen Druckfestigkeit finden diese Hochleistungsbetone vermehrten Einsatz im Hoch-, Brücken-, und Tunnelbau. Unter Brandbeanspruchung neigen diese Hochleistungsbetone allerdings zu explosionsartigen Abplatzungen. Diese werden nach derzeitigem Stand auf thermomechanische und thermohydraulische Prozesse zurückgeführt. Letztere beruhen auf der Generierung hoher Wasserdampfdrücke in einseitig brandbeanspruchten Beton-bauteilen, die zum einen auf die geringe Permeabilität des Hochleistungsbetons und zum anderen auf die Bildung einer wassergesättigten Zone, der sogenannten „moisture clog“ zurückzuführen sind. Dabei spielen Verdampfungs- und Kondensationsvorgänge sowie der vorhandene Temperatur-gradient eine wichtige Rolle. Die Interaktion des Feuchtetra-nsportes mit den Gefügeveränderungen während der thermi-schen Beanspruchung soll im Rahmen weiterer Versuche eingehend untersucht werden. Zur Analyse des Feuchtetransports während der thermischen Beanspruchung wurden miniaturisierte Prüfkörper aus Hoch-leistungsbeton hergestellt, die mit Hilfe eines elektrischen Heizelements einseitig erwärmt wurden. Zur Sicherstellung eines eindimensionalen Wärme- und Feuchtetransportes ist der Betonprüfkörper mit einer speziellen Glaskeramik und einer Hochtemperaturwolle ummantelt. Simultan zur Erwär-mung werden eine Reihe röntgentomographischer Aufnah-men durchgeführt. Durch Differenzbildung aufeinanderfol-gender Aufnahmen können Dichteveränderungen lokal und zeitlich aufgelöst werden. Diese lassen Rückschlüsse auf Än-derungen der Feuchteverteilung im Prüfkörper während der Erwärmung zu. Parallel dazu werden Untersuchungen mittels NMR-Relaxometrie (nuclear magnetic resonance) vor und nach der thermischen Beanspruchung durchgeführt. Diese Prüfmethodologie ermöglicht es erstmals, die Veränderungen der Feuchteverteilung infolge thermischer Beanspruchung im Hochleistungsbeton von den Gelporen bis hin zu vorhande-nen Verdichtungsporen abzubilden. So zeigen erste Ergebnis-se, dass die gewählten Untersuchungsmethoden Veränderun-gen der Feuchteverteilung im Prüfkörper räumlich und zeitlich auflösen können. KW - Abplatzen KW - Spalling KW - Brand KW - Feuchtetransport KW - Hochleistungsbeton KW - Röntgen-3D-Computertomographie KW - NMR KW - Fire KW - Moisture clog KW - Moisture transport KW - HPC KW - HSC KW - X-ray CT PY - 2017 DO - https://doi.org/10.1002/best.201700022 SN - 0005-9900 SN - 1437-1006 VL - 112 IS - 7 SP - 486 EP - 486 PB - Ernst & Sohn CY - Berlin AN - OPUS4-41826 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meißner, G. A1 - Dirican, D. A1 - Jäger, Christian A1 - Braun, T. A1 - Kemnitz, E. T1 - Et3GeH versus Et3SiH: controlling reaction pathways in catalytic C–F bond activations at a nanoscopic aluminum chlorofluoride† N2 - Catalytic C–F bond activation reactions of mono- and polyfluoroalkanes at Lewis acidic amorphous aluminum chlorofluoride (ACF) are presented. The hydrogen sources Et3GeH or Et3SiH control the selectivity of the conversions. The immobilization of Et3GeH at ACF resulted in catalytic dehydrohalogenation reactions to yield olefins under very mild conditions. In contrast, if Et3SiH is immobilized at ACF, C–C coupling occured and the formation of Friedel–Crafts products was observed. MAS NMR spectroscopic studies revealed information about the surface binding of the substrates. KW - Vapor-phase hydrofluorination KW - Carbon-fluorine bonds KW - Vinyl fluoride KW - Phosphine-ligands KW - Room-temperature KW - Building-blocks KW - Etal-complexes KW - Germylium ions KW - Lewis-acids KW - Hydrodefluorination PY - 2017 DO - https://doi.org/10.1039/c7cy00845g SN - 2044-4753 SN - 2044-4761 VL - 7 IS - 15 SP - 3348 EP - 3354 PB - The Royal Society of Chemistry AN - OPUS4-41836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, Anja A1 - Kranzmann, Axel T1 - Potential of martensitic stainless steel X5CrNiCuNb 16-4 as pipe steel in corrosive CCS environment N2 - Pipe steels suitable for carbon capture and storage technology (CCS) require resistance against the corrosive environment of a potential CCS-site (heat, pressure, salinity of the aquifer, CO2-partial pressure). X5CrNiCuNb16-4 has been proven to be sufficient resistant in corrosive environments, but shows rather unusual corrosion behaviour in CCS environment. Therefore differently heat treated coupons of 1.4542 were kept at T=60 °C and ambient pressure as well as p=100 bar for 700 h - 8000 h in an a) water saturated supercritical CO2 and b) CO2-saturated synthetic aquifer environment similar to on-shore CCS-sites in the Northern German Basin. Additionally fatigue tests were performed via push-pull tests with a series of 30 specimens was tested at stress amplitudes between 150 MPa and 500 MPa (sinusoidal dynamic test loads, R=-1; resonant frequency ~ 30 Hz). Best corrosion resistance in the liquid phase is achieved via normalizing prior to exposure and hardening+tempering at 670 °C leads to lowest corrosion rates in the supercritical phase. With no regard to atmosphere discontinuously ellipsoidal surface corrosion regions appear after exposure of 4000 h and more. The endurance limit of X5CrNiCuNb16-4 measured in air is reduced by more than 50% when exposed to CCS environment (maximum number of cycles (10 x 106) at a stress amplitude of 150 MPa) The scatter range TN = 1:34 is disproportionately large contributing to an overall unusual corrosion behaviour. KW - Corrosion KW - CCS KW - Carbon storage KW - Aquifer KW - Heat treatment KW - Fatigue KW - Endurance limit PY - 2017 DO - https://doi.org/10.18178/ijesd.2017.8.7.998 SN - 2010-0264 VL - 8 IS - 7 SP - 466 EP - 473 AN - OPUS4-41863 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosemann, Paul A1 - Müller, C. A1 - Kauss, N. A1 - Halle, T. T1 - Einfluss der Wärmebehandlung auf die Korrosionsbeständigkeit von Schneidwaren N2 - Härte und Korrosionsbeständigkeit sind die wichtigsten Qualitätsmerkmale von Schneidwaren. Diese werden nur durch eine optimal durchgeführte Wärmebehandlung des martensitischen nichtrostenden Stahls 1.4116 (X50CrMoV15) erreicht. In der industriellen Fertigung wird die Korrosionsbeständigkeit von Schneidwaren durch Wechseltauchversuche überprüft, die herstellerübergreifend eine große Schwankung der Korrosionsbeständigkeit belegen. In den letzten Jahren wurden neue elektrochemische Untersuchungsmethoden für die Werkstoffgruppe der martensitischen nichtrostenden Stähle entwickelt, welche die geringe Lochkorrosionsbeständigkeit von Schneidwaren auf das Phänomen der Chromverarmung zurückzuführen. Derzeit wird in der wissenschaftlichen und in der industriellen Gemeinschaft der Schritt des Anlassens als Hauptursache der Chromverarmung angesehen. Bei Schneidwaren sind die Anlasstemperaturen aber zu gering, um die auftretende Chromverarmung zu erklären. Aus diesem Grund wurden drei verschiedene Wärmebehandlungsparameter (Austenitisierungsdauer, Abkühlgeschwindigkeit und Anlasstemperatur) systematische untersucht, um deren Beitrag zur Chromverarmung darzustellen. Dazu wird die Untersuchungsmethode der elektrochemisch potentiodynamischen Reaktivierung (EPR) eingesetzt, die sehr sensibel auf Veränderungen im Gefüge reagiert und den Grad an Chromverarmung ermittelt. Außerdem wurde die KorroPad-Prüfung durchgeführt und kritische Lochkorrosionspotentiale ermittelt, um den Zusammenhang zwischen Chromverarmung und Lochkorrosionsbeständigkeit herzustellen. Die Ergebnisse aller Untersuchungen verdeutlichen wie eng das Prozessfenster ist, in dem Schneidwaren mit hoher Korrosionsbeständigkeit hergestellt werden können. T2 - 72. HärtereiKongress CY - Cologne, Germany DA - 26.10.2016 KW - Schneidwaren KW - Wärmebehandlung KW - nichtrostender Stahl KW - martensitisch KW - Lochkorrosion KW - EPR KW - KorroPad PY - 2017 DO - https://doi.org/10.3139/105.110317 SN - 1867-2493 VL - 72 IS - 2 SP - 87 EP - 98 PB - Carl Hanser CY - München AN - OPUS4-41241 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, Susann A1 - Schröter, Maria-Astrid A1 - Hahn, Marc Benjamin A1 - Solumon, Tihomir A1 - Strum, Heinz A1 - Kunte, Hans-Jörg T1 - Ectoine can enhance structural changes in DNA in vitro N2 - Strand breaks and conformational changes of DNA have consequences for the physiological role of DNA. The natural protecting molecule ectoine is beneficial to entire bacterial cells and biomolecules such as proteins by mitigating detrimental effects of environmental stresses. It was postulated that ectoine-like molecules bind to negatively charged spheres that mimic DNA surfaces. We investigated the effect of ectoine on DNA and whether ectoine is able to protect DNA from damages caused by ultraviolet radiation (UV-A). In order to determine different isoforms of DNA, agarose gel electrophoresis and atomic force microscopy experiments were carried out with plasmid pUC19 DNA. Our quantitative results revealed that a prolonged incubation of DNA with ectoine leads to an increase in transitions from supercoiled (undamaged) to open circular (single-strand break) conformation at pH 6.6. The effect is pH dependent and no significant changes were observed at physiological pH of 7.5. After UV-A irradiation in ectoine solution, changes in DNA conformation were even more pronounced and this effect was pH dependent. We hypothesize that ectoine is attracted to the negatively charge surface of DNA at lower pH and therefore fails to act as a stabilizing agent for DNA in our in vitro experiments. KW - Ectoine KW - DNA KW - UV radiation PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-413139 DO - https://doi.org/10.1038/s41598-017-07441-z VL - 7 IS - 1 SP - Article 7170, 1 EP - 10 AN - OPUS4-41313 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn T1 - Scattering on scattering N2 - Ultrafast experiments can reveal the spatiotemporal dynamics of nanostructure formation via scattering in background-free optical dark-field microscopy. KW - Ultrafast microscopy KW - Scattering KW - Darkfield microscopy KW - Laser ablation PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-411596 DO - https://doi.org/10.1038/lsa.2017.88 SN - 2047-7538 VL - 6 SP - e17088, 1 EP - 2 PB - Springer Nature AN - OPUS4-41159 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kropidlowski, K. A1 - Uhlmann, E. A1 - Woydt, Mathias T1 - Außen-Längs-Runddrehen mit Niobcarbid-Schneidstoff N2 - Als Alternative zu Wolframcarbid wird zurzeit Niobcarbid beim Drehen unter extremen Bedingungen untersucht, vorerst ohne Beschichtungen und ohne Kühlschmierstoffe. Aufgrund seiner besonderen Eigenschaften zeigt Niobcarbid als Schneidstoff ein großes Potenzial. KW - Niobcarbid KW - Drehen KW - Schneidstoff PY - 2017 IS - 7-8 SP - 58 EP - 61 PB - Carl Hanser CY - München AN - OPUS4-41129 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Woydt, Mathias T1 - VGP 2013 - Propelling marine lubricants N2 - This letter to the Editor directs attention to EN 16807-2016:12, Liquid Petroleum products - Bio lubricants - Criteria and requirements of bio lubricants and bio-based lubricants. KW - Bio lubricants KW - Liquid petroleum products KW - EN 16807-2016:12 PY - 2017 SN - 1545-858X VL - 73 IS - 7 SP - 7 PB - Society of Tribologists and Lubrication Engineers CY - Park Ridge, IL AN - OPUS4-41342 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yin, Huajie A1 - Chapala, P. A1 - Bermeshev, M. A1 - Schönhals, Andreas A1 - Böhning, Martin T1 - Molecular Mobility and Physical Aging of a Highly Permeable Glassy Polynorbornene as Revealed by Dielectric Spectroscopy N2 - Polymeric membranes represent a cost- and energy efficient solution for gas separation. Recently superglassy polymers with high free volume outperform many conventional dense polymers in terms of gas permeability and selectivity. However, such polymers are prone to pronounced physical aging, resulting in a dramatic reduction in the gas permeability. Molecular mobility of polymer segments plays an important role in the physical aging and the gas transport performance of polymeric membranes. Molecular mobility and physical aging of a representative superglassy polynorbornene with very high gas permeability, PTCNSi2g, was monitored by using dielectric spectroscopy with state-of-the-art high-resolution analyzers. This work helps to shed some light on the structure−property relationship of superglassy polymers on a molecular level and to provide practical “design rules” for the development of high performance polymers for gas separation. KW - Molecular mobility KW - Gas separation membrane KW - Broadband dielectric spectroscopy KW - Polymer KW - Physical ageing PY - 2017 DO - https://doi.org/10.1021/acsmacrolett.7b00456 SN - 2161-1653 VL - 6 IS - 8 SP - 813 EP - 818 PB - ACS CY - Washington DC, USA AN - OPUS4-41354 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grohmann, Maria A1 - Müller, Sabine A1 - Niederleithinger, Ernst A1 - Sieber, S. T1 - Reverse time migration: introducing a new imaging technique for ultrasonic measurements in civil engineering N2 - Ultrasonic echo testing is widely used in non-destructive testing in civil engineering to investigate concrete structures, to measure thickness, and to locate and characterise built-in components or inhomogeneities. Currently, synthetic aperture focusing techniques are mostly used for imaging. These algorithms are highly developed but have some limitations. For example, it is not possible to image the lower boundary of built-in components like tendon ducts or vertical reflectors. We adopted reverse time migration for non-destructive testing in civil engineering in order to improve the imaging of complicated structures in concrete. By using the entire wavefield, including waves reflected more than once, there are fewer limitations compared to synthetic aperture focusing technique algorithms. As a drawback, the required computation is significantly higher than that for the techniques currently used. Simulations for polyamide and concrete structures showed the potential for non-destructive testing. The simulations were followed by experiments at a polyamide specimen. Here, having acquired almost noise-free measurement data to test the algorithm, we were able to determine the shape and size of boreholes with sufficient accuracy. After these successful tests, we performed experiments at a reinforced concrete foundation slab. We obtained information from the data by reverse time migration, which was not accessible by traditional imaging. The imaging of the location and structure of the lower boundary of the concrete foundation slab was improved. Furthermore, vertical reflectors inside the slab were imaged clearly, and more flaws were found. It has been shown that reverse time migration is a step forward in ultrasonic testing in civil engineering. KW - Ultrasonic echo technique KW - Reverse time migration PY - 2017 DO - https://doi.org/10.3997/1873-0604.2017006 SN - 1569-4445 SN - 1873-0604 VL - 15 IS - 3 SP - 242 EP - 258 PB - Wiley AN - OPUS4-41921 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lehmann, Jens A1 - Leonhard, H. T1 - Unsichtbares sichtbar machen - Oberflächenschnelltest auf Korrosionsgefahr N2 - Eine Passivschicht schützt die Oberfläche nichtrostender Stähle vor Materialauflösung. Sie darf nicht unvollständig oder beschädigt sein. Sonst drohen Schadensfälle durch Korrosion an Rohrsystemen und Behältern. TÜV SÜD Chemie Service zeigt ein von der Bundesanstalt für Materialforschung und -prüfung (BAM) entwickeltes Verfahren zur Überprüfung der Passivschicht. Der Test nimmt nur 15 Minuten in Anspruch. KW - Nichtrostender Stahl KW - Korrosionsschnelltest KW - KorroPad KW - Passivschicht PY - 2017 SN - 1436-2597 VL - 20 IS - 9 SP - 53 EP - 54 PB - Wiley-VCH Verlag GmbH & Co. KGaG CY - Weinheim AN - OPUS4-41911 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Giebson, C. A1 - Voland, K. A1 - Ludwig, H.-M. A1 - Meng, Birgit T1 - Alkali-silica reaction performance testing of concrete considering external alkalis and preexisting microcrack N2 - In concrete elements, simultaneously subjected to cyclic loadings and external alkalis, the risk for damage caused by or under participation of an alkali-silica reaction (ASR) is particularly high. This is of particular concern for concrete pavements due to the increasing heavy vehicle traffic and the application of sodium chloride (NaCl) de-icer during winter. Since 2004, the climate simulation concrete prism test (CS-CPT) has been used successfully to evaluate job mixtures for pavements by considering the impact of alkali-containing de-icers. However, the role of mechanical predamage on ASR is largely unclear. In a joint research project, the CS-CPT has been used to investigate the influence of preexisting microcracks on ASR. It was evident that an ASR initiated earlier in the predamaged concrete prisms due to the more rapid ingress of NaCl solution through the microcracks. KW - Alkali-silica reaction KW - Climate simulation concrete prism test KW - External alkalis KW - Laser-induced breakdown spectroscopy KW - Microcracks KW - Pavement concrete PY - 2017 DO - https://doi.org/10.1002/suco.201600173 SN - 1464-4177 SN - 1751-7648 VL - 18 IS - 4 SP - 528 EP - 538 PB - Ernst & Sohn AN - OPUS4-42574 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epperlein, Nadja A1 - Menzel, Friederike A1 - Schwibbert, Karin A1 - Koter, Robert A1 - Bonse, Jörn A1 - Sameith, Janin A1 - Krüger, Jörg A1 - Toepel, Jörg T1 - Influence of femtosecond laser produced nanostructures on biofilm growth on steel N2 - Biofilm formation poses high risks in multiple industrial and medical settings. However, the robust nature of biofilms makes them also attractive for industrial applications where cell biocatalysts are increasingly in use. Since tailoring material properties that affect bacterial growth or its inhibition is gaining attention, here we focus on the effects of femtosecond laser produced nanostructures on bacterial adhesion. Large area periodic surface structures were generated on steel surfaces using 30-fs laser pulses at 790 nm wavelength. Two types of steel exhibiting a different corrosion resistance were used, i.e., a plain structural steel (corrodible) and a stainless steel (resistant to corrosion). Homogeneous fields of laser-induced periodic surface structures (LIPSS) were realized utilizing laser fluences close to the ablation threshold while scanning the sample under the focused laser beam in a multi-pulse regime. The nanostructures were characterized with optical and scanning electron microscopy. For each type of steel, more than ten identical samples were laser-processed. Subsequently, the samples were subjected to microbial adhesion tests. Bacteria of different shape and adhesion behavior (Escherichia coli and Staphylococcus aureus) were exposed to laser structures and to polished reference surfaces. Our results indicate that E. coli preferentially avoids adhesion to the LIPSS-covered areas, whereas S. aureus favors these areas for colonization. KW - Laser-induced periodic surface structures KW - Femtosecond laser KW - Steel KW - Biofilms KW - Microbial adhesion tests PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S0169433217305470 DO - https://doi.org/10.1016/j.apsusc.2017.02.174 SN - 0169-4332 SN - 1873-5584 VL - 418 IS - Part B SP - 420 EP - 424 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-40565 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Frasca, Daniele A1 - Schulze, Dietmar A1 - Böhning, Martin A1 - Krafft, Bernd A1 - Schartel, Bernhard T1 - Chlorbutylkautschuk/Multilayergraphen-Nanocomposites N2 - In den letzten Jahren werden zunehmend Nanopartikel als Füllstoff für Polymere vorgeschlagen und auch erfolgreich in Elastomer-Nanocomposites eingesetzt. In dieser Arbeit wird Multilayergraphen (MLG) als Nanofüllstoff näher untersucht, der sich bereits bei geringen Konzentrationen als effizient erweist. MLG besteht aus nur etwa zehn Graphenlagen. Chlorbutylkautschuk (CIIR)/MLG-Nanocomposites mit verschiedenen MLG-Gehalten wurden mit Hilfe eines ultraschallunterstützen Mischverfahrens in Lösung hergestellt und auf einem Walzwerk weiterverarbeitet. Das Einmischen von MLG führt zu einer deutlichen Verbesserung der rheologischen und mechanischen Eigenschaften, des Vernetzungsverhaltens sowie der Barrierewirkung gegenüber Gasen. Bereits der Zusatz von 3 phr MLG zu CIIR führt zu einem mehr als zweifach höheren E-Modul und zu einer Reduktion der Permeabilität von O2 und CO2 um 30 %. Höhere Konzentrationen an Nanofüllstoff resultieren in einer weiteren Verbesserung der Eigenschaften der Nanocomposites. Weiterhin zeigten die CIIR/MLG-Nanocomposites auch eine geringere Entflammbarkeit. KW - Elastomere KW - Nanokomposite KW - Graphen KW - Chlorbutylkautschuk PY - 2017 SN - 0176-1625 VL - 70 IS - 5 SP - 311 EP - 322 PB - Dr. Gupta Verlag CY - Ratingen AN - OPUS4-40327 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Böhning, Martin A1 - Oehler, H. A1 - Alig, I. A1 - Niebergall, Ute T1 - Environmental stress cracking of polyethylene high density (PE-HD) induced by liquid media – Validation and verification of the full-notch creep test (FNCT) T1 - Umgebungsinduzierte Spannungsrissbildung von Polyethylen- Werkstoffen hoher Dichte durch flüssige Medien – Validierung und Verifizierung des Kriechversuchs an Probekörpern mit umlaufender Kerbe N2 - The full-notch creep test (FNCT) is widely used to characterize the slow crack growth (SCG) behavior of polyolefin materials in “inert” media as well as effects of environmental stress cracking (ESC) in which the medium has decisive influence on damage mechanism and time to failure. The test is of greatest importance for pipe and blow molding types of polyethylene, high density (PE-HD). Usually the full-notch creep test is applied as a standardized testing method (ISO 16770) using a few universal liquid media, such as solutions of Arkopal N 100. In our study, selected relevant polyethylene, high density materials are investigated also in real media – practical formulations as well as representative pure chemicals – and influences of temperature and geometry of specimen and notch are explicitly addressed. Furthermore, the investigations comprise also the environmental stress cracking behavior of polyethylene, high density in media that are sorbed to a significant extent – examples are diesel and biodiesel – based on comparison with samples previously saturated with those media. Thus, also the underlying diffusion controlled sorption process has to be assessed before. The investigations were performed using a full-notch creep testing device with 12 individual sub-stations, each equipped with individual electronic stress and temperature control and continuous online monitoring of the specimen elongation. N2 - Der Kriechversuch an Probekörpern mit umlaufender Kerbe (FNCT) wird flächendeckend angewendet, um das Verhalten von Polyolefinen sowohl gegenüber langsamen Risswachstums (SCG) bei Kontakt mit „inerten“ Medien als auch gegenüber umgebungsbedingtem Spannungsrisswachstum (ESC), bei welchem das umgebende Medium entscheidenden Einfluss auf den Schädigungsmechanismus und die Standzeit hat, zu charakterisieren. Der Test ist von großer Bedeutung bei der Analyse von hochdichten Polyethylen-Typen, die als Rohr- und Blasformwerkstoffe angewendet werden – dabei besonders für Transport und Verpackung von Gefahrstoffen, aber auch für weitere Hochleistungsanwendungen. Üblicherweise wird der Kriechversuch an Probekörpern mit umlaufender Kerbe als Normmethode (ISO 16770) unter Verwendung einiger weniger universeller Modellflüssigkeiten, wie z. B. Arkopal N 100, durchgeführt. In dieser Studie werden ausgewählte, marktrelevante Polyethylen-Werkstoffe hoher Dichte in realen Medien – praktisch verwendete Gefahrgüter sowie repräsentative reine Chemikalien – untersucht und explizit die Einflüsse von Temperatur und Prüfkörper- sowie Kerbgeometrie adressiert. Weiterhin beinhalten die Untersuchungen die Analyse des umgebungsbedingten Spannungsriss-Verhaltens von Polyethylen hoher Dichte in Medien, die maßgeblich vom Werkstoff sorbiert sind – beispielsweise mit Kraftstoffen wie diesel und biodiesel – basierend auf dem Vergleich mit vorgesättigten Probekörpern. Der dabei vorliegende diffusionsgesteuerte Sorptionsprozess muss dementsprechend zuvor evaluiert werden. Alle Untersuchungen wurden mithilfe einer Kriechversuchsanlage an Probekörpern mit umlaufender Kerbe mit 12 Stationen durchgeführt, welche jeweils mit einer individuell ansteuerbaren elektronischen Spannungs- und Temperatursteuerung sowie fortwährender Online-Überwachung der Prüfkörperdehnung ausgestattet sind. KW - Full-notch creep test (FNCT) KW - Polyethylene (PE-HD) KW - Environmental stress cracking (ESC) KW - Slow crack growth (SCG) KW - Biodiesel PY - 2017 DO - https://doi.org/10.1002/mawe.201700065 SN - 1521-4052 SN - 0933-5137 VL - 48 IS - 9 SP - 846 EP - 854 PB - Wiley-VCH CY - Weinheim AN - OPUS4-41885 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Konnertz, Nora A1 - Ding, Yi A1 - Harrison, W.J. A1 - Budd, P.M. A1 - Schönhals, Andreas A1 - Böhning, Martin T1 - Molecular mobility and gas transport properties of nanocomposites based on PIM-1 and polyhedral oligomeric phenethyl-silsesquioxanes (POSS) N2 - Polymers with intrinsic microporosity (PIMs) are of great interest in the field of gas separation membranes. Already the first synthesized PIM-1 shows extraordinary permeability and selectivity. Unfortunately, PIM-1 is susceptible to physical aging and thus gradually loses its outstanding properties. In this study a polyhedral oligomeric silsesquioxane with phenethyl substituents (PhenethylPOSS) was used as a nanofiller (0–40 wt%) in the PIM-1 matrix to potentially improve the gas transport properties and prevent physical aging. The molecular mobility of the solution-cast nanocomposite films was analyzed by Broadband Dielectric Spectroscopy (BDS). Furthermore, gas permeability was determined with the time lag method (0–20 bar upstream pressure) at 35 °C for N2, O2, CH4 and CO2. KW - Broadband Dielectric Spectroscopy KW - Gas separation KW - Gas permeation KW - Polymers of intrinsic microporosity KW - Nanocomposite KW - POSS KW - PIM-1 PY - 2017 DO - https://doi.org/10.1016/j.memsci.2017.02.007 SN - 0376-7388 SN - 1873-3123 VL - 529 SP - 274 EP - 285 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-39169 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Niebergall, Ute A1 - Böhning, Martin T1 - Full notch creep test (FNCT) of PE-HD – Characterization and differentiation of brittle and ductile fracture behavior during environmental stress cracking (ESC) N2 - The damage mechanisms slow crack growth (SCG) and environmental stress cracking (ESC), relevant for PE-HD materials are characterized based on improved full notch creep testing (FNCT) of two selected typical PE-HD materials for container applications. In this context, a distinction of the failure mechanisms as well as a categorization of involved media is suggested. Employing a novel FNCT device, elongation data were obtained in addition to conventional time-to-failure results of stress-dependent as well as temperature-dependent measurements. Changes in failure behavior, as determined by fracture surface analysis based on light microscopy (LM) and laser scanning microscopy (LSM), are correlated with FNCT results and used to introduce an additional possibility for the identification of brittle/ductile fracture behavior. KW - Environmental stress cracking (ESC) KW - Slow crack growth (SCG) KW - Full notch creep test (FNCT) KW - High-density polyethylene (PE-HD) PY - 2017 DO - https://doi.org/10.1016/j.polymertesting.2017.09.043 SN - 0142-9418 SN - 1873-2348 VL - 64 SP - 156 EP - 166 PB - Elsevier CY - Amsterdam AN - OPUS4-42484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bachmann, Marcel A1 - Carstensen, J. A1 - Bergmann, L. A1 - dos Santos, J. F. A1 - Wu, C. S. A1 - Rethmeier, Michael T1 - Numerical simulation of thermally induced residual stresses in friction stir welding of aluminum alloy 2024-T3 at different welding speeds N2 - The paper deals with a numerical finite element simulation of the residual stress evolution in friction stir welding of 6 mm thick aluminum alloy AA2024-T3. The transient thermal field during the welding process was calculated with the commercial code COMSOL Multiphysics 5.0. Therefore, a thermal-pseudo-mechanical (TPM) heat source was implemented. A subsequent mechanical simulation was performed with varying hardening models for different welding speeds of 60 and 300 mm/min. The influence of softening of the material, which was due to hardening precipitation dissolution associated to the heating, was also investigated. Experiments in terms of thermocouple measurements as well as Vickers hardness and X-ray measurements of the residual stresses were conducted and compared to numerically obtained results. A qualitatively as well as quantitatively good agreement was found for different applied welding speeds. KW - Friction stir welding KW - Residual stress KW - Finite element simulation KW - Thermal softening KW - Aluminum alloy 2024-T3 PY - 2017 DO - https://doi.org/10.1007/s00170-016-9793-8 SN - 0268-3768 SN - 1433-3015 VL - 91 SP - 1443 EP - 1452 PB - Springer CY - London AN - OPUS4-40511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sproesser, G. A1 - Chang, Y.-J. A1 - Pittner, Andreas A1 - Finkbeiner, M. A1 - Rethmeier, Michael T1 - Energy efficiency and environmental impacts of high power gas metal arc welding N2 - Single-wire gas metal arc welding (SGMAW) and high power tandem GMAW (TGMAW) are evaluated with respect to energy efficiency. The key performance indicator electrical deposition efficiency is applied to reflect the energy efficiency of GMAW in different material transfer modes. Additionally, the wall-plug efficiency of the equipment is determined in order to identify the overall energy consumption. The results show that energy efficiency can be increased by 24% and welding time is reduced over 50% by application of the tandem processes. A comparative life cycle assessment of a 30-mm-thick weld is conducted to investigate the influences of the energy efficiency on the environmental impacts. The environmental impacts on the categories global warming potential, acidification potential, eutrophication potential, and photochemical ozone creation potential can be reduced up to 11% using an energy-efficient TGMAW process. KW - Tandem gas metal arc welding KW - Life cycle assessment (LCA) KW - Energy efficiency KW - High power welding PY - 2017 DO - https://doi.org/10.1007/s00170-017-9996-7 SN - 0268-3768 SN - 1433-3015 VL - 91 IS - 9-12 SP - 3503 EP - 3513 PB - Springer CY - London AN - OPUS4-39564 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröpfer, Dirk A1 - Kromm, Arne A1 - Kannengießer, Thomas T1 - Optimization of welding loads with narrow groove and application of modified spray arc process N2 - Current efforts for lightweight design result in a growing application of high-strength fine-grained structural steel in modern constructions, e.g. mobile cranes, with yield strength from 960 MPa. The design of welded structures and welding processes becomes more challenging with increasing material strength and elastic ratios. High residual stresses are able to diminish lifetime, load capacity and component safety and should be avoided. Recent analyses have shown strong influences of heat control and restraint of the weld due to arising reaction stresses, superimposing with local residual welding stresses. Modern inverter technologies allowed the development of numerous modified spray arc processes driven by power source manufacturers, which provide virtually similar features and several benefits, enabling welding of narrower seams with reduced weld volumes and total heat inputs. This research focuses on welding loads due to modified weld seams. The global reaction forces and moments and their superposition with local residual stresses in welded components due to external shrinkage restraints were investigated using a special testing facility and XRD. The restraint intensity, weld seam geometry and welding process were varied for statistical evaluations of resulting welding loads. When welding under restraint, a reduction of the weld seam volume causes significantly lower reaction stress levels. KW - Residual stresses KW - MAG welding KW - Restraint KW - High-strength steels KW - Process parameters PY - 2017 DO - https://doi.org/10.1007/s40194-017-0484-3 SN - 1878-6669 SN - 0043-2288 VL - 61 IS - 6 SP - 1077 EP - 1087 PB - Springer CY - Berlin Heidelberg AN - OPUS4-41071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lamiel, C. A1 - Lee, Y. R. A1 - Cho, M. H. A1 - Tuma, Dirk A1 - Shim, J.-J. T1 - Enhanced electrochemical performance of nickel-cobalt-oxide@reduced graphene oxide//activated carbon asymmetric supercapacitors by the addition of a redox-active electrolyte N2 - Supercapacitors are an emerging energy-storage system with a wide range of potential applications. In this study, highly porous nickel-cobalt-oxide@reduced graphene oxide (Ni-Co-O@RGO-s) nanosheets were synthesized as an active material for supercapacitors using a surfactant-assisted microwave irradiation technique. The RGO-modified nanocomposite showed a larger specific area, better conductivity, and lower resistivity than the unmodified nanocomposite because the RGO facilitated faster ion diffusion/transport for improved redox activity. The synergistic effect of Ni-Co-O@RGO-s resulted in a high capacitance of 1903 F/g (at 0.8 A/g) in a mixed KOH/redox active K3Fe(CN)6 electrolyte. The asymmetric Ni-Co-O@RGO-s//AC supercapacitor device yielded a high energy density and power density of 39 Wh/kg and 7500 W/kg, respectively. The porous structure and combination of redox couples from both the electrode and electrolyte provided a highly synergistic effect, which improved the performance of the supercapacitor device. KW - Ni-Co oxide KW - Reduced graphene oxide KW - Nanocomposite KW - Supercapacitor PY - 2017 DO - https://doi.org/10.1016/j.jcis.2017.08.003 SN - 0021-9797 SN - 1095-7103 VL - 507 SP - 300 EP - 309 PB - Elsevier Inc. CY - Amsterdam AN - OPUS4-41284 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mady, A. H. A1 - Baynosa, M. L. A1 - Tuma, Dirk A1 - Shim, J.-J. T1 - Facile microwave-assisted green synthesis of Ag-ZnFe2O4@rGO nanocomposites for efficient removal of organic dyes under UV- and visible-light irradiation N2 - Nanocomposites of Ag-ZnFe2O4@reduced graphene oxide (rGO) were synthesized using a one-pot microwave-assisted self-assembly method. The morphology and structure of the Ag-ZnFe2O4@rGO nanocomposites were characterized. The nanocomposites formed with 15.2 wt% rGO showed excellent adsorption properties and high photocatalytic activity for the degradation of methylene blue (MB), rhodamine B (RhB), and methyl orange (MO). The synergistic interactions between Ag, ZnFe2O4, and rGO decreased the aggregation of the nanoparticles (NPs) and increased the surface area, resulting in better absorption in both UV and visible light. Such a structure was helpful for separating the photoexcited electron-hole pairs and accelerating electron transfer. Electrochemical impedance spectroscopy (EIS) revealed a smaller resistance in the solid-state interface layer and charge transfer on the composite surface than that of the bare ZnFe2O4 NPs and ZnFe2O4@rGO nanocomposite. The Ag-ZnFe2O4@rGO nanocomposite could be recovered easily by a magnet and reused five times with no significant decrease in photocatalytic activity. The as-prepared Ag-ZnFe2O4@rGO nanocomposite catalyst could be applied to the removal of hard-to-degrade waste materials owing to its high efficiency in both UV and visible light and its excellent reusability. KW - nanoparticles KW - microwave synthesis KW - photocatalysis PY - 2017 DO - https://doi.org/10.1016/j.apcatb.2016.10.033 SN - 0926-3373 SN - 1873-3883 VL - 203 SP - 416 EP - 427 PB - Elsevier B. V. CY - Amsterdam AN - OPUS4-37962 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröpfer, Dirk A1 - Kromm, Arne A1 - Kannengießer, Thomas T1 - Engineering approach to assess residual stresses in welded components N2 - Present trends to lightweight design lead to an expanding relevance of high-strength fine-grained structural steels especially in mobile crane constructions. With growing material strength, the challenge for welding fabrication increases, since high loading capacities and safety requirements have to be accomplished. The utilisation of the high strength potential often requires complex constructions associated with high restraint conditions while welding. Increased residual stresses may occur due to superimposing reaction and restraint stresses, which have to be quantified and evaluated to ensure the safety and integrity of high-strength steel constructions. Particularly, the scope of residual stresses has to be taken into account for different effects in the HAZ, notches, weld and base metal. Commonly, conservative assumptions of residual stresses lead to distinct underestimations of the load bearing capacity particularly for welded high-strength steel constructions. This study concludes results of recent works of the researchers regarding the complex interaction among heat control, material and restraint intensity on the residual stress state in welded components. These analyses are extended by further experiments. Based on the obtained major effects, an approach for a welding residual stress assessment regarding component design according to prevailing standards for crane construction, an important application for high-strength steels, is presented. KW - Process parameters KW - Residual stresses KW - MAG welding KW - Restraint KW - High-strength steels PY - 2017 DO - https://doi.org/10.1007/s40194-016-0394-9 SN - 0043-2288 SN - 1878-6669 VL - 91 IS - 1 SP - 91 EP - 106 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-39044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schaupp, Thomas A1 - Schröpfer, Dirk A1 - Kromm, Arne A1 - Kannengießer, Thomas T1 - Welding residual stresses in 960 MPa grade QT and TMCP high-strength steels N2 - High-strength steels with yield strengths ≥ 690 MPa are becoming increasingly significant for modern steel constructions. Both quenched and tempered (QT) high-strength steels and steels produced by the thermo-mechanically controlled process (TMCP) are currently available. TMCP-steels are usually provided with a typical mill scale. Apart from the manufacturing process these steels differ also in their chemical composition. The influence of these differences are investigated here with focus on the residual stresses formed during TIG welding. Bead on plate welds have shown characteristic residual stress distributions depending on the type of steel as well as on the heat input and preheat temperature. The following work demonstrates that the fluid flow, induced by the elements present in the mill scale, leads to a deeper penetration of the material. This can also lead to increased residual stresses in the surface of the weld and the HAZ. Furthermore, higher heat input and preheat temperature can induce higher tensile residual stresses − which are evident in the present study. KW - Residual stresses KW - High-strength steel KW - Welding KW - Mill scale KW - Phase transformation PY - 2017 DO - https://doi.org/10.1016/j.jmapro.2017.05.006 SN - 1526-6125 VL - 27 SP - 226 EP - 232 PB - ELSEVIER AN - OPUS4-40312 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steppan, Enrico A1 - Mantzke, Philipp A1 - Steffens, Benjamin A1 - Rhode, Michael A1 - Kannengießer, Thomas T1 - Thermal desorption analysis for hydrogen trapping in microalloyed high-strength steels N2 - Hydrogen can have an extreme degradation effects in steels, particularly concerning the mechanical properties. These effects can lead to hydrogen-assisted cracking in microalloyed high-strength steels during fabrication and/or operation in industrial applications. In order to study these effects, electrochemically charged tensile specimens were tested to elucidate the degradation of their properties. The carrier gas hot extraction (CGHE) method, which functionally combines a mass spectrometer with a thermal desorption analysis (TDA) process, was used for the detection of ultra-low diffusible hydrogen concentrations in the material specimens. The mass spectrometer provided rapid and automatic determination of hydrogen concentration, whereas the TDA presented the activation energy within the respective test specimen at the specific temperature. Additionally, specimen temperature was carefully monitored to reduce the evaluation error for local effusion peaks. A quenching and deformation dilatometer was used for the analysis of typical heat-affected zones during the welding process for a high reproducibility of the homogenous microstructures that were studied. The present work shows the interaction between hydrogen and lattice defects in different microalloyed materials and heat-affected zones of weldable fine-grained steels. These steels were prepared in a quenched and tempered condition and in a thermo-mechanically rolled condition. These preparations were made according to German standard DIN EN 10025-6 and to DIN EN 10149-2, respectively. The trapping characteristics of two steel grades, S690QL and S700MC, were studied with respect to the activation energy dependent on carbon content and microalloying elements such as Ti, Nb, Mo, Cr, and V. The two steel grades exhibited several types of traps: carbide formations, dislocations, and/or grain boundaries were common, which can influence activation energy and hydrogen solubility. The type and dimension of inclusions or particles also affected the hydrogen trapping behavior. A decrease of carbon and specific alloying elements in thermo-mechanically hot rolled steels led to a change in the activation energy binding the trapped hydrogen. This thermo-mechanically hot rolled steel revealed an increased interaction between hydrogen and precipitations. The higher carbon content in the quenched and tempered steel led to a higher interaction between hydrogen and iron carbide, specifically in the martensitic phase. Furthermore, the trapping behavior in heat-affected zones showed a significant increase in activation energy, especially in the coarse-grained microstructure. These previously mentioned various effects were studied to better understand the degradation of mechanical properties in these two steels. KW - Microalloyed steels KW - Hydrogen embrittlement KW - Heating KW - Chemical analysis KW - Microstructure KW - Heat-affected zone PY - 2017 DO - https://doi.org/10.1007/s40194-017-0451-z SN - 0043-2288 SN - 1878-6669 VL - 61 IS - 4 SP - 637 EP - 648 PB - Springer CY - Berlin Heidelberg AN - OPUS4-40190 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gollnow, C. A1 - Griesche, Axel A1 - Weidemann, Jens A1 - Kannengießer, Thomas T1 - Influence of external loads on a characteristic angle between grains and solidus line as an indicator for hot cracking susceptibility during GTA welding N2 - A long list of criteria determining the hot cracking susceptibility already exists. A main influence on solidification cracking can result from the design of the welded construction, i.e. from the influence of external loads. Using the Controlled Tensile Weldability (CTW) test, an external load hot cracking test, the influence of constant pre-load and different extension rates on the solidification cracking behavior of GTA (Gas Tungsten Arc) welds in an austenitic (AISI 309) and a ferritic (AISI 441) steel were investigated. Compared to specimens welded allowing free shrinkage and welded with an applied constant tensile pre-load, the specimens welded during the application of increasing tensile load show solidification cracks. In the weld seams, a characteristic angle α between the predominantly columnar grains and the fusion line can be observed. Specimens showing solidification cracks show a significantly larger angle α compared to the crack-free specimens. Based on these observations, the characteristic angle α is proposed as a new hot cracking criterion. KW - Hot cracking KW - External load test KW - Component design KW - Crack criterion KW - Grain growth PY - 2017 DO - https://doi.org/10.1016/j.jmatprotec.2016.08.013 VL - 239 SP - 172 EP - 177 PB - Elsevier AN - OPUS4-37278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hilgenberg, Kai A1 - Rethmeier, Michael A1 - Steinhoff, K. T1 - Surface structuring by pulsed laser implantation N2 - Micrometric surface topologies are required for a wide range of technical applications. While lowered surface features have been used for many years to improve the tribological behavior of contacting surfaces, there are also other fields of application, where the potential of elevated surface features is known, e. g. for metal forming tools. However, the demand for a high wear resistance of these structures often inhibits an industrial application. A solution is offered by structuring techniques that use additional material. A promising approach is the localized dispersing of hard ceramic particles by pulsed laser radiation, the so-called laser implantation. This paper describes the potential to adjust the geometry as well as the mechanical properties of laser implanted surfaces by means of microstructural and topological investigations. Afterwards, results of a wear test are given and different applications for this structuring technique are discussed. It can be shown that dome-shaped or ring-shaped structures on a micrometric scale can be produced with high hardness and wear resistance. KW - Laser implantation KW - Surface structuring PY - 2017 DO - https://doi.org/10.4028/www.scientific.net/MSF.879.750 SN - 0255-5476 SN - 1662-9752 VL - 879 SP - 750 EP - 755 PB - Trans Tech Publications AN - OPUS4-38263 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ward, H. A1 - Burger, M. A1 - Chang, Y.-J. A1 - Fürstmann, P. A1 - Neugebauer, S. A1 - Radebach, A. A1 - Sproesser, G. A1 - Pittner, Andreas A1 - Rethmeier, Michael A1 - Uhlmann, E. A1 - Steckel, J. Ch. T1 - Assessing carbon dioxide emission reduction potentials of improved manufacturing processes using multiregional input output frameworks N2 - Evaluating innovative process technologies has become highly important within the last decades. As standard tools different Life Cycle Assessment methods have been established, which are continuously improved. While those are designed for evaluating single processes they run into difficulties when it comes to assessing environmental impacts of process innovations at macroeconomic level. In this paper we develop a multi-step evaluation framework building on multi regional inputeoutput data that allows estimating macroeconomic impacts of new process technologies, considering the network characteristics of the global economy. Our procedure is as follows: i) we measure differences in material usage of process alternatives, ii) we identify where the standard processes are located within economic networks and virtually replace those by innovative process technologies, iii) we account for changes within economic systems and evaluate impacts on emissions. Within this paper we exemplarily apply the methodology to two recently developed innovative technologies: longitudinal large diameter steel pipe welding and turning of high-temperature resistant materials. While we find the macroeconomic impacts of very specific process innovations to be small, its conclusions can significantly differ from traditional process based approaches. Furthermore, information gained from the methodology provides relevant additional insights for decision makers extending the picture gained from traditional process life cycle assessment. KW - Economic wide technology replacement KW - Sustainability assessment KW - Multi-regional inputeoutput data KW - Life-cycle assessment KW - Greenhouse gas mitigation KW - Process innovations PY - 2017 DO - https://doi.org/10.1016/j.jclepro.2016.02.062 SN - 0959-6526 SN - 1879-1786 VL - 163 SP - 154 EP - 165 PB - Elsevier Ltd. AN - OPUS4-41356 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neubert, S. A1 - Pittner, Andreas A1 - Rethmeier, Michael T1 - Influence of non-uniform martensitic transformation on residual stresses and distortion of GMA-welding N2 - A combined experimental and numerical approach is applied for a numerical analysis of the non-uniform martensitic transformation kinetic on welding residual stresses and distortion of a single pass weld. The (γ → α)-transformation kinetic within the weld pool region is governed by a non-uniform distribution of the elements chromium and nickel. The single-pass weld was performed by use of the low-alloyed high-strength steel S960QL with the high-alloyed high-strength filler wire CN 13/4-IG®. A thermo-mechanical FE model of the welding process was experimentally validated against temperature field, solid phase distribution, transformation behaviour, X-Ray stress measurements and transient optical distortion measurements. The experimentally determined and calculated weld residual stresses and transient distortion are in good agreement. It can be shown that the change on the (γ → α)-transformation kinetic driven by the inhomogeneous distribution of the chemical contents causes a strong influence on the weld residual stresses within the volume of the weld pool, which could promote crack propagation within the solidified weld pool by use of high-alloyed filler materials. Furthermore, a significant influence on the development of the transient welding distortion is visible. This influence should be respected during numerically calculation of welding distortion in case of multi-pass welding using interpass temperatures and high-alloyed filler materials. KW - Welding residual stresses KW - FEA KW - Welding simulation KW - Dissimilar welding KW - Transformable steels PY - 2017 DO - https://doi.org/10.1016/j.jcsr.2016.08.020 SN - 0143-974X SN - 1873-5983 VL - 128 SP - 193 EP - 200 PB - Elsevier Ltd. AN - OPUS4-37276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gook, S. A1 - Gumenyuk, Andrey A1 - Rethmeier, Michael T1 - Hybrid laser arc welding of high grade X80 and X120 pipeline steels N2 - The aim of the present work was to investigate the possibilities of hybrid laser arc welding regarding reliable production of longitudinal welds of high strength pipe steels X80 and X120 and to evaluate achievable mechanical properties of laser hybrid welds. The study focused on weld toughness examination in low temperature range up to -60 °C. SЮТЭКЛХО ПТХХОЫ ЦКЭОЫТКХЬ were identified in the context of this task. It could be shown that metal cored electrodes guaranteed sufficient Charpy impact toughness at low temperature for both investigated materials. Modern arc welding technologies such as modified pulsed spray arc were used to promote deeper Penetration of the filler material into the narrow laser welding gap. Edge preparation with a 14 mm deep root face was considered as optimum, because no penetration of the filler material could be detected beyond this depth limit and therefore any metallurgical influences on the weld metal properties through the welding wire could be excluded. KW - High strength steel KW - Longitudinal weld KW - Modified spray arc KW - Pipeline KW - Hybrid laser arc welding PY - 2017 SN - 2499-9733 SN - 2305-414Х VL - 1 IS - 22 SP - 21 EP - 35 AN - OPUS4-44343 LA - rus AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Marko, A. A1 - Graf, B. A1 - Gook, S. A1 - Rethmeier, Michael T1 - Application of D-optimum experimental designs in consideration of restrictions for laser metal deposition N2 - The process of laser metal deposition can be applied in many ways. Mostly, it is relevant to coating, for repair welding and for additive manufacturing. To increase the effectiveness and the productiveness, a good process understanding is necessary. Statistical test planning is effectual and often used for this purpose. For financial and temporal reasons, a restriction of the test space is reasonable. In this case, it is recommended to use a D-optimal experimental design which is practically applied to extend existing test plans or if process Limits are known. This paper investigates the applicability of a D-optimum experimental design for the laser metal deposition. The results are compared to the current results of a full factorial test plan. Known restrictions are used for the limitation of the test space. Ti6Al4 is utilized as Substrate material and powder. Comparable results of the D-optimal experimental design and of the full factorial test plan can be demonstrated. However, 80 % of time can be saved by the experimental procedure. For this reason, the application of D-optimal experimental design for laser metal deposition is recommend. KW - Design of experiments KW - Repair welding KW - Additive manufacturing KW - Cladding parameter KW - Laser metal deposition KW - Laser cladding PY - 2017 SN - 2499-9733 SN - 2305-414Х VL - 3 IS - 24 SP - 46 EP - 60 AN - OPUS4-44344 LA - rus AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rethmeier, Michael A1 - Finkbeiner, M. T1 - Licht ist grüner als Strom N2 - Laserschweißen gegen Widerstandspunktschweißen: Die Die Entscheidung fällt am Flansch. Beide Verfahren sind sehr schnell und hoch automatisierbar. KW - Laserschweißen KW - Widerstandspunktschweißen PY - 2017 VL - 24 SP - 6 EP - 6 AN - OPUS4-40413 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bakir, Nasim A1 - Gumenyuk, Andrey A1 - Rethmeier, Michael T1 - Investigation of solidification cracking susceptibility during laser beam welding using an in-situ observation technique N2 - Using the novel optical measurement technique together with the optical flow algorithm, a twodimensional deformation analysis during welding has been conducted. This technique provides for the first time a measurement of the strain field locally in the immediate vicinity of the assumed solidification front. The described procedure of the opticalmeasurement allows to determine the real martial-dependent values of critical strain and strain rate characterising transition to the hot cracking during laser welding processes. The local critical strain that obtained in the assumed solidification showed that the local critical strain decreases as the strain rate increases. Moreover, this phenomenon has also been shown with results from the CTW-test, since the global strain decreases with an increase in the external strain rate. KW - Novel optical measurement KW - Local critical strain KW - Solidification cracking KW - Laser beam Welding PY - 2017 DO - https://doi.org/10.1080/13621718.2017.1367550 SN - 1362-1718 SP - 1 EP - 7 PB - Taylor & Francis AN - OPUS4-42918 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mushtaq, S. A1 - Steers, E.B.M. A1 - Barnhart, D. A1 - Churchill, G. A1 - Kasik, M. A1 - Richter, Silke A1 - Pfeifer, Jens A1 - Putyera, K. T1 - The production of doubly charged sample ions by “charge transfer and ionization” (CTI) in analytical GD-MS N2 - Normally, in analytical GD-MS, the doubly charged metallic ion signals from the sample are several orders of magnitude less than the corresponding singly charged signals. However, we have observed that using a neon plasma, the M++ signals of some elements, which have double ionization energies close to the first ionization energy of neon, are of the same order as the M+ signal. Doubly charged ions may be produced directly in the discharge cell by electron ionization (EI), and also by two electron Penning ionization (TEP), but these processes cannot explain the above effect. In this paper, we suggest that an additional process named as ‘Charge Transfer and Ionization’ (CTI) produces such ions either in their ionic ground state or in an excited state. To confirm that this process is typical of the discharges used in GD-MS and not an artefact of any particular form of cell and ion extraction system, we have carried out comprehensive experimental measurements using three different GD-MS instruments, viz., Nu Astrum, VG9000 and ELEMENT GD and our results provide clear evidence for CTI. This is the first time the process has been identified as an ionization process in analytical GD-MS. CTI must be differentiated from Asymmetric Charge Transfer (ACT), which is a “selective” process and requires a close energy match (e.g. ΔE < 0.5 eV for a strong effect). On the other hand, CTI is “non-selective” in the sense that a close energy match is not required (e.g. a strong effect is observed with ΔE ∼ 2 eV), although the process only occurs for a limited number of elements, depending on the plasma gas used and the total energy required to doubly ionize the metallic atom. KW - Titanium KW - Glow discharge processes KW - Doubly charged ions KW - The charge transfer and ionization process (CTI) KW - Krypton KW - Neon PY - 2017 DO - https://doi.org/10.1039/C6JA00415F SN - 0267-9477 SN - 1364-5544 VL - 32 IS - 9 SP - 1721 EP - 1729 PB - Royal Society of Chemistry AN - OPUS4-41108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wachtendorf, Volker A1 - Kalbe, Ute A1 - Krüger, O. A1 - Bandow, Nicole ED - Brown, R. ED - Gedde, U.W. ED - Hedenqvist, M.S. T1 - Influence of weathering on the leaching behaviour of zinc and PAH from synthetic sports surfaces N2 - Synthetic materials used for outdoor sports grounds consist of a mix of inorganic, organic and polymeric compounds that show ageing due to weathering and a complex leaching behaviour by percolation of rainwater, which can limit its lifetime. Additionally, weathering exposure induces degradation processes in the polymers, which leads to the formation of new surfaces allowing water to access additional reservoirs of leachable compounds. A laboratory test comprising artificial weathering, ozonisation and subsequent leaching was developed to investigate this behaviour in a reproducible and controllable way. The experiments showed a general decline of Zn, polycyclic aromatic hydrocarbons (PAH) and total organic carbon (TOC) concentrations after an initial increase. Within this general trend, the course of concentration over exposure duration is very specific for individual sample materials and the analyte under investigation. The results indicate that weathering and degradation behaviour cannot be predicted from initial material conditions. Thus, weathering experiments are recommended to fill this gap of knowledge. KW - Athletic tracks KW - Artificial turf KW - Ageing KW - Artificial weathering KW - Polymer degradation KW - Rubber granules KW - Leaching KW - Contamination PY - 2017 DO - https://doi.org/10.1016/j.polymertesting.2017.09.021 SN - 0142-9418 SN - 1873-2348 VL - 63 IS - October SP - 621 EP - 631 PB - Elsevier Ltd. CY - Amsterdam, The Netherlands AN - OPUS4-42205 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friedrich, Jörg A1 - Altmann, Korinna A1 - Wettmarshausen, Sascha A1 - Hidde, Gundula T1 - Coating of carbon fibers with adhesion-promoting thin polymer layers using plasma polymerization or electrospray ionization technique—A comparison N2 - Plasma polymers and electrospray-ionization (ESI) polymer layers are compared for most efficient adhesion promotion in carbon fiber-epoxy resin composites. The ultra-thin ESI layers (2–30 nm) of commercial poly(acrylic acid) and poly-(hydroxyethylmethacrylate) produce an significant increase of adhesion measured by single-fiber pull out tests. However, plasma Treatment has also advantages, such as simultaneous activation of the fiber substrate. Chemical structure and composition are rather far from the regular structure of commercial polymers as deposited by ESI processing. KW - Plasma polymers KW - Electrospray ionization polymers KW - Poly(acrylic acid) KW - Poly- (hydroxyethylmethacrylate) PY - 2017 DO - https://doi.org/10.1002/ppap.201600074 SN - 1612-8869 SN - 1612-8850 VL - 14 IS - 3 SP - e1600074-1 EP - 14 AN - OPUS4-40510 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Launert, B. A1 - Szczerba, R. A1 - Gajewski, M. A1 - Rhode, Michael A1 - Pasternak, H. A1 - Gizejowski, M. T1 - The buckling resistance of welded plate girders taking into account the influence of post-welding imperfections - Part 1: Parameter study N2 - Welding is the most important joining technique and offers the advantage of customizable plate thicknesses. On the other hand, welding causes residual stresses and deformations influencing the load carrying capacity. Their consideration in the design requires simple and fast models. Though welding simulation has contributed to accurately access to these values nowadays, their application to large components remains still in a less practicable range. Nevertheless, many studies emphasized the need to make corrections in recently available simplified models. Especially the influence of residual stresses seems somewhat overestimated in many cases if comparing conventional structural steel S355 and high-strength steel S690. In the age of computer-aided design, an improved procedure to implement weld-inducted imperfections appears overdue. This will be presented in two parts. The first part illustrates the potential influence of post-welding imperfections exemplified for weak axis buckling in comparison with the general method in accordance with Eurocode 3. Residual stresses and initial crookedness were varied systematically in order to produce a scatter band of capacities. An approach to characterize the borders of these imperfections was untertaken before that. The excessive scattering of reduction factors for the load bearing capacity demonstrates the importance of these variables. Results were finally evaluated against advanced simulation models which will be further detailed in part two of this contribution. KW - Welded Plate Girders KW - Stability KW - Post-welding Imperfections KW - Residual Stresses KW - Parameter Study PY - 2017 DO - https://doi.org/10.3139/120.110964 SN - 0025-5300 SN - 2195-8572 VL - 59 IS - 1 SP - 47 EP - 56 PB - Carl Hanser Verlag CY - München AN - OPUS4-38922 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 - Vollert, J. A1 - Dixneit, Jonny A1 - Kromm, Arne A1 - Buslaps, Th. A1 - Kannengießer, Thomas T1 - In situ EDXRD study of MAG-welding using LTT weld filler materials under structural restraint N2 - Welding using low transformation temperature (LTT) filler materials is an innovative approach to mitigate detrimental welding residual stresses without cost-intensive post weldtreatments. Due to the local Generation of compressive residual stresses in the weld line by means of a delayed martensite transformation a significant enhancement of the cold cracking resistance of highly stressed welded components can be expected. For the effective usage of These materials a deeper understanding of the microstructural evolution inside the weld material is necessary to determine the complex processes that cause the residual stress formation during welding. Solid-state phase transformation kinetics and the evolution of strain in LTT weld filler materials are monitored in-situ at the instrument ID15A at the ESRF in Grenoble, France. The transferability to real components is implemented by using a realistic MAG welding process under consideration of structural restraint. During welding of multilayer joints, the phase Transformation and phase specific strain evolution of each individual layer is investigated in transmission geometry by means of energy-dispersive X-ray diffraction EDXRD using high energy synchrotron Radiation with a counting rate of 2.5 Hz. The measurement results of a 10% Cr / 10% Ni LTT weld filler are compared to data monitored for the conventional weld filler material G89. The in-situ data clearly indicate a strong effect on the local strain evolution and the formation of compressive strain. This results from the restraint volume expansion during the postponed austenite to martensite transformation of the LTT weld filler, which counteracts the thermal shrinkage. In contrast, for the conventional weld filler material the thermal contraction strains lead to tensile residual strain during welding. Furthermore, the results of in-situ observation during welding Show that the transformation kinetic is dependent on the welding sequence. KW - High energy synchrotron diffraction KW - Low transformation temperature KW - Weld filler KW - Residual stress KW - Welding PY - 2017 DO - https://doi.org/10.4028/www.scientific.net/MSF.905.107 SN - 1662-9752 VL - 905 SP - 107 EP - 113 PB - Trans Tech Publications CY - Switzerland AN - OPUS4-41806 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 - Greiser, Sebastian A1 - Benemann, Sigrid A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Knowing When To Stop-Trapping Metastable Polymorphs in Mechanochemical Reactions N2 - The cocrystal formation of pyrazinamide (PZA) with malonic acid (MA) was studied in situ. The mechanochemical reaction proceeds via conversion of a crystalline intermediate (PZA:MA II) into the thermodynamically more stable form (PZA:MA I) upon further grinding. The information derived from in situ powder X-ray diffraction (PXRD) enabled the isolation of this new metastable polymorph. On the basis of the PXRD data, the crystal structure of the 1:1 cocrystal PZA:MA II was solved. The polymorphs were further characterized and compared by Raman spectroscopy, solid-state NMR spectroscopy, differential thermal analysis/thermogravimetric analysis, and scanning electron microscopy. Our study demonstrates how monitoring mechanochemical reactions by in situ PXRD can direct the discovery and isolation of even short-lived intermediates not yet accessed by conventional methods. KW - Mechanochemistry KW - Polymorphs KW - Metastable KW - In situ PXRD KW - Cocrystal KW - Pyrazinamide PY - 2017 DO - https://doi.org/10.1021/acs.cgd.6b01572 SN - 1528-7483 SN - 1528-7505 VL - 17 IS - 3 SP - 1190 EP - 1196 AN - OPUS4-39420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dixneit, Jonny A1 - Kromm, Arne A1 - Boin, M. A1 - Wimpory, Robert A1 - Kannengießer, Thomas A1 - Gibmeier, J. A1 - Schröpfer, Dirk T1 - Residual stresses of LTT welds in large-scale components N2 - Residual stresses of welds become more and more important influencing cold cracking as well as the fatigue life of welded components. Low transformation temperature (LTT) filler materials offer the opportunity to alter the residual stresses already during the welding process by means of ad- justed martensite phase transformation temperature (MS). In the current paper, welding residual stresses are studied putting the focus on MS while joining heavy steel sections with a thickness of 20 and 25 mm, respectively. The residual stress state was determined at the top surface using X-ray diffraction as well as in the bulk by neutron diffraction. The results com- pare the residual stresses present in a conventional weld and LTT welds when multi-pass welding of large-scale compo- nents was applied. Repeated phase transformation in the case of the LTT weld is more vital for the residual stresses present in the real-life-like joints. This accounts for the top surface in longitudinal direction but is most pronounced for the bulk of the welds. Detrimental tensile residual stresses are mainly re- duced in the bulk in comparison to a conventional filler wire even in multi-pass welds of thick steel sections. T2 - IIW AA 2016 CY - Melbourne, Australia DA - 10.07.2016 KW - LTT KW - Welding residual stress KW - Phase transformation KW - Interpass temperature PY - 2017 DO - https://doi.org/10.1007/s40194-017-0502-5 SN - 0043-2288 SN - 1878-6669 VL - 61 IS - 6 SP - 1089 EP - 1097 PB - Springer CY - Heidelberg AN - OPUS4-41169 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geißler, Daniel A1 - Würth, Christian A1 - Wolter, C. A1 - Weller, H. A1 - Resch-Genger, Ute T1 - Excitation wavelength dependence of the photoluminescence quantum yield and decay behavior of CdSe/CdS quantum dot/quantum rods with different aspect ratios N2 - The excitation wavelength (lexc) dependence of the photoluminescence (PL) quantum yield (FPL) and decay behavior (tPL) of a series of CdSe/CdS quantum dot/Quantum rods (QDQRs), consisting of the same spherical CdSe core and rod-shaped CdS shells, with aspect ratios ranging from 2 to 20 was characterized. lexc between 400–565 nm were chosen to cover the first excitonic absorption band of the CdSe core material, the onset of absorption of the CDs shell, and the region of predominant shell absorption. A strong lexc dependence of relative and absolutely measured FPL and tPL was found particularly for the longer QDQRs with higher aspect ratios. This is attributed to combined contributions from a length-dependent shell-to-core exciton localization efficiency, an increasing number of defect states within the shell for the longest QDQRs, and probably also the presence of absorbing, yet non-emitting shell material. Although the FPL values of the QDQRs decrease at shorter wavelength, the extremely high extinction coefficients introduced by the shell outweigh this effect, leading to significantly higher brightness values at wavelengths below the absorption onset of the CdS Shell compared with direct excitation of the CdSe cores. Moreover, our results present also an interesting example for the comparability of absolutely measured FPL using an integrating sphere setup and FPL values measured relative to common FPL standards, and underline the Need for a correction for particle scattering for QDQRs with high aspect ratios. KW - Quantum dot KW - Quantum rod KW - Quantum yield KW - Integrating sphere KW - Decay time PY - 2017 DO - https://doi.org/10.1039/C7CP02142A SN - 1463-9076 SN - 1463-9084 VL - 19 IS - 19 SP - 12509 EP - 12516 PB - Royal Society of Chemistry (RSC) AN - OPUS4-40814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Würth, Christian A1 - Kaiser, Martin A1 - Wilhelm, Stefan A1 - Grauel, Bettina A1 - Hirsch, Th. A1 - Resch-Genger, Ute T1 - Excitation power dependent population pathways and absolute quantum yields of upconversion nanoparticles in different solvents N2 - The rational design of brighter upconversion nanoparticles (UCNPs) requires a better understanding of the radiationless deactivation pathways in these materials. Here, we demonstrate the potential of excitation power density (P)-dependent studies of upconversion (UC) luminescence intensities, slope factors, and absolute quantum yields (ΦUC) of popular β-NaYF4:20% Yb3+,2% Er3+ UCNPs of different surface chemistries in organic solvents, D2O, and water as a tool to gain deeper insight into the UC mechanism including population and deactivation pathways particularly of the red emission. Our measurements, covering a P regime of three orders of magnitude, reveal a strong difference of the P-dependence of the ratio of the green and red luminescence bands (Ig/r) in water and organic solvents and P-dependent population pathways of the different emissive energy levels of Er3+. In summary, we provide experimental evidence for three photon processes in UCNPs, particularly for the red emission. Moreover, we demonstrate changes in the excited population dynamics via bi- and triphotonic processes dependent on the environment, surface chemistry, and P, and validate our findings theoretically KW - Upconverion KW - Quantum Yield KW - Photo physics PY - 2017 UR - http://pubs.rsc.org/en/content/articlepdf/2017/nr/c7nr00092h DO - https://doi.org/10.1039/c7nr00092h SN - 2040-3364 SN - 2040-3372 VL - 9 IS - 12 SP - 4283 EP - 4294 PB - The Royal Society of Chemistry AN - OPUS4-39849 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -