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 - 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 - Selleng, Christian A1 - Meng, Birgit A1 - Gröger, K. A1 - Fontana, Patrick T1 - Einflussgrößen auf die Wirksamkeit einer Wärmebehandlung von Ultrahochfestem Beton (UHFB) T1 - Influencing factors for the effectivity of heat treatment of ultrahigh performance concrete (UHPC) N2 - Mittels Wärmebehandlung lassen sich die hervorragenden Eigenschaften von UHFB nochmals verbessern. Die für eine optimale Umsetzung relevanten Randbedingungen werden aktuell in der Fachwelt diskutiert. In dieser Veröffentlichung werden die Ergebnisse eines Forschungsprojekts vorgestellt, das die Wirkung verschiedener Einflussgrößen bei der Wärmebehandlung auf die Eigenschaften von UHFB zum Thema hatte. Dabei wurden die Art des Schutzes gegen das Austrocknen, die Vorlagerungszeit und die Haltezeit variiert. Um die zugrunde liegenden Prozesse zu verstehen, wurde der Phasenbestand mittels Röntgendiffraktometrie untersucht. Die höchsten Druckfestigkeiten des UHFB ließen sich bei einer Wärmebehandlung mit Wasserlagerung erzielen, da hierbei eine weitere Hydratation begünstigt wird. Vergleichsweise niedriger waren die Steigerungen bei einer Behandlung mit Schutz vor Austrocknung, während eine ungeschützte Behandlung zu deutlich geringeren Festigkeiten führte. Die Vorlagerungszeit beträgt im Idealfall einige Tage, um die Ausbildung eines offenbar günstigen Ausgangsgefüges sicherzustellen. Die Haltezeit sollte möglichst ausgedehnt sein, weil die Hydratation entsprechend lange gefördert wird. Im oberflächennahen Bereich war unter bestimmten Bedingungen eine Zonierung zu beobachten, deren Ursachen und Folgen, insbesondere in Bezug auf die Dauerhaftigkeit, weitere Forschung erfordern. KW - Ultra-Hochleistungsbeton KW - Wärmebehandlung KW - Behandlungsparameter KW - Vorlagerungszeit KW - Haltezeit KW - Festigkeitssteigerung KW - Zonierung KW - Ettringit PY - 2017 DO - https://doi.org/10.1002/best.201600059 SN - 0005-9900 VL - 112 IS - 1 SP - 12 EP - 21 PB - Ernst & Sohn AN - OPUS4-39171 LA - deu 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 - Sun, C. A1 - Tian, X. A1 - Wang, L. A1 - Liu, Y. A1 - Wirth, Cynthia A1 - Günster, Jens A1 - Li, D. A1 - Jin, Z. T1 - Effect of particle size gradation on the performance of glass-ceramic 3D printing process N2 - Particle size gradation is regarded as an effective method for overcoming the contradicting requirements in three-dimensional printing (3DP). In present work, particle size gradation was optimized to obtain both acceptable flowability of the powder material and high-strength 3D-printed glass-ceramic products. The effect of gradation on the printing process, sintering process and performance of the 3D-printed glass-ceramic products was investigated comprehensively. The glass-ceramic powders with three size ranges were mixed in certain proportions and applied to print parts. The result showed parts printed with powder mixed by 60 wt% 45–100 µm and 40 wt% 0–25 µm particles had satisfactory density of 1.60 g/cm³ and bending strength of 13.8 MPa. The flowability decreased with an increasing proportion of fine particles. Part density was determined by the powder bulk density in the powder bed as well as the shrinkage during sintering while strength of part was found to be dependent on the sintering degree. KW - Flowability KW - Glass-ceramic KW - Particle size gradation KW - Three-dimensional printing KW - Mechanical properties PY - 2017 DO - https://doi.org/10.1016/j.ceramint.2016.09.197 SN - 0272-8842 VL - 43 IS - 1 SP - 578 EP - 584 PB - Elsevier AN - OPUS4-39783 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 - TY - JOUR A1 - Weidner, Steffen A1 - Kricheldorf, H. R. T1 - The Role of Transesterification in SnOct 2 - Catalyzed Polymerizations of Lactides N2 - l-lactide or meso-lactide are polymerized either at 120 °C where the polymerization process of l-lactide is accompanied by crystallization, or at 180 °C where poly(l-lactide) remains in the molten state. Polymerizations at 120 °C initially yield even-numbered chains (with respect to lactic acid units) having relatively low dispersity, but the fraction of odd-numbered chains increases with time and the entire molecular weight distribution changes. Traces of cyclics are only formed after 7 d. Polymerizations at 180 °C yield equilibrium of even and odd-numbered chains from the beginning, but at low monomer/initiator ratios and short reaction times (<4 h) cyclics are again not formed. They appear at longer reaction times and entail higher dispersities. The results are discussed in terms of five different transesterification mechanisms. KW - Polylactides KW - MALDI KW - Transesterification KW - Sn catalysts PY - 2017 DO - https://doi.org/10.1002/macp.201600331 SN - 1022-1352 VL - 218 IS - 3 SP - 1600331 PB - Wiley AN - OPUS4-39753 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 - Klingelhoeffer, Hellmuth A1 - Aegerter, J. A1 - Scherm, T. A1 - Schenuit, E. A1 - Sotheran, S. A1 - Loveday, M. A1 - Bosch, P. A1 - Bloching, H. A1 - Olbricht, Jürgen A1 - McEnteggart, I. T1 - Discussion on "Analysis on the issues in ISO 6892-1 and TENSTAND WP4 report based on the data of confirm tests by 21 laboratories" N2 - The authors, Li et al., of the paper entitled “Analysis on the Issues in ISO 6892-1 and TENSTAND WP4 Report Based on Data to Confirm Tests by 21 Laboratories” (J. Test. Eval. DOI: 10.1520/JTE20150479 (online only)) have expressed views that the authors of this rebuttal believe to be based on fundamental misunderstandings and misinterpretations of the tensile testing standard ISO 6892-1:2009, ISO 6892-1:2016, and its former versions, thus leading to erroneous conclusions. This refutation is intended to clarify the understanding of ISO 6892-1 and to address the misunderstandings and the misinterpretations of the authors of the paper. The present standard ISO 6892-1:2016 has a long history dating back to the 1970s. At that time, the tensile testing procedure was standardized on the National and International scale in parallel. To understand the present standard, the knowledge of the history helps to understand the background of details of the testing procedure implemented today. The history of the tensile testing standard has been discussed extensively during the annual international standardization meeting of ISO committee TC 164 SC1 for the last few years, at which some of the authors of the Li et al. paper attended. The authors continue to disagree with facts that were agreed by the consortium of the European research project TENSTAND and by the present international experts involved in ISO TC 164 SC1. It appears that the principal objective of the authors regarding their present publication was to increase the testing speed during tensile testing. However, the international standardization community has previously declined similar proposals by some of the authors. Many arguments presented by Li et al. were thus refuted. The conclusions of their paper are misleading and the international standardization community for tensile testing refused to revise the present standard, ISO 6892-1 (2016), according the authors’ proposals. KW - Tensile testing procedure KW - ISO 6892-1 KW - TENSTAND WP4 Final Report PY - 2017 DO - https://doi.org/10.1520/JTE20160526 SN - 0090-3973 SN - 1945-7553 VL - 45 IS - 3 SP - 1105 EP - 1114 PB - ASTM International CY - West Conshohocken, PA, USA AN - OPUS4-40267 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -