TY - JOUR A1 - Wollschläger, Nicole A1 - Palasse, L. A1 - Häusler, Ines A1 - Dirscherl, K. A1 - Oswald, F. A1 - Narbey, S. A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan T1 - Characterization of the inner structure of porous TiO2 nanoparticle films in dye sensitive solar cells (DSSC) by focused ion beam (FIB) tomography and transmission Kikuchi diffraction (TKD) in the scanning electron microscope (SEM) N2 - A combined methodical approach is tested for the first time with respect to the characterization of the inner structure of porous TiO2 layers infiltrated with ruthenium molecular sensitizer as typically used in modern dye sensitized solar cells (DSSC). Their performance is directly linked to the surface area ‘offered’ by the pore Network to the dye. The micrometer thick layer employed was manufactured by screen-printing of a starting TiO2 powder constituted of shape-controlled, bipyramidal anatase nanoparticles (NPs) on FTO/glass substrates. The analytical methods exploited in our study are Focused Ion Beam (FIB) slicing followed by 3D reconstruction as well as the new approach transmission Kikuchi diffraction (TKD) technology in the scanning electron microscope (SEM). While the first method results in the visualization of the 3D pore network within the TiO2 layer, the second one can be successfully applied to analyze the crystal orientation of grains (i.e. NPs in our case) in nanometer resolution. Moreover, size and shape distribution of the TiO2 NPs within the layer can be extracted. SEM in transmission mode and atomic force microscopy (AFM) have been used to verify the dimensional data obtained by the new combined methodical approach. Its analytical benefits but also the challenges and limitations are highlighted. KW - Transmission Kikuchi diffraction KW - Focused ion beam tomography KW - Titanium dioxide KW - Nanoparticles KW - Porosity KW - Particle size KW - DSSC PY - 2017 DO - https://doi.org/10.1016/j.matchar.2017.06.030 SN - 1044-5803 SN - 1873-4189 VL - 131 SP - 39 EP - 48 PB - Elsevier AN - OPUS4-40875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 - 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 - 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 - 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 - 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 - 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 - Breitenbach, Romy A1 - Silbernagl, Dorothee A1 - Toepel, J. A1 - Sturm, Heinz A1 - Broughton, William J. A1 - Sassaki, G. L. A1 - Gorbushina, Anna T1 - Corrosive extracellular polysaccharides of the rock-inhabiting model fungus Knufia petricola N2 - Melanised cell walls and extracellular polymeric matrices protect rock-inhabiting microcolonial fungi from hostile environmental conditions. How extracellular polymeric substances (EPS) perform this protective role was investigated by following development of the model microcolonial black fungus Knufia petricola A95 grown as a sub-aerial biofilm. Extracellular substances were extracted with NaOH/formaldehyde and the structures of two excreted polymers studied by methylation as well as NMR analyses. The main polysaccharide (~ 80%) was pullulan, also known as α-1,4-; α-1,6-glucan, with different degrees of polymerisation. Αlpha-(1,4)-linked-Glcp and α-(1,6)-linked-Glcp were present in the molar ratios of 2:1. A branched galactofuromannan with an α-(1,2)-linked Manp main chain and a β-(1,6)-linked Galf side chain formed a minor fraction (~ 20%). To further understand the roles of EPS in the weathering of minerals and rocks, viscosity along with corrosive properties were studied using atomic force microscopy (AFM). The kinetic viscosity of extracellular K. petricola A95 polysaccharides (≈ 0.97 × 10-6 m2 s-1) ranged from the equivalent of 2% (w/v) to 5% glycerine, and could thus profoundly affect diffusion-dominated processes. The corrosive nature of rock-inhabiting fungal EPS was also demonstrated by its effects on the aluminium coating of the AFM cantilever and the silicon layer below. KW - Corrosion KW - EPS KW - Melanised microcolonial fungi (MCF) KW - Pullulan KW - Sub-aerial biofilms (SAB) KW - α-1,4- and α-1,6-glucans KW - AFM cantilever vibration KW - Nanoviscosity KW - Nanocorrosion of aluminium and silicon PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-435910 DO - https://doi.org/10.1007/s00792-017-0984-5 SN - 1433-4909 SN - 1431-0651 VL - 22 IS - 2 SP - 165 EP - 175 PB - Springer CY - Berlin AN - OPUS4-43591 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 - 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 - 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 - 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 - Erdmann, Maren A1 - Trappe, Volker A1 - Sturm, Heinz A1 - Braun, Ulrike A1 - Dümichen, Erik T1 - Cure conversion of structural epoxies by cure state analysis and in situ cure kinetics using nondestructive NIR spectroscopy N2 - Non-isothermal heating rate kinetics was applied to two epoxy resin systems. In situ near-infrared (NIR) measurements were taken with a heatable NIR cell which allowed the cure to be monitored by characteristic absorption bands. An autocatalyzed reaction of the nth order was shown to describe the epoxy conversion curves. Differential Scanning Calorimetry (DSC) was used as a complementary method. The kinetic models developed by both NIR and DSC are in good accordance with experimental epoxy conversion in the in situ NIR setup for single and multiple cure temperature ramps. A linear calibration curve of the characteristic absorption bands of epoxy normalized to aromatic vibrations was introduced. The curing degree of structural epoxies that were cured according to an industrial temperature cure profile was determined by NIR using the calibration curve. The epoxy conversions of the structural components showed good agreement with the experimental in situ NIR. Several degrees of cure for structural specimens were evaluated by NIR and residual reaction enthalpy by DSC. We present the non-destructive NIR spectroscopy as an alternative to determine fast and non-destructive epoxy conversion, particularly suitable for high degrees of cure on structural components. KW - Epoxy resin KW - Curing kinetics KW - In situ near-infrared (NIR) spectroscopy KW - Differential scanning calorimetry (DSC) PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S0040603117300205 DO - https://doi.org/10.1016/j.tca.2017.01.010 SN - 0040-6031 SN - 1872-762X VL - 650 SP - 8 EP - 17 PB - Elsevier B.V. AN - OPUS4-39123 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, Hans R. A1 - Weidner, Steffen A1 - Scheliga, Felix T1 - Cyclic poly(l-lactide) via ring-expansion polymerization by means of dibutyltin 4-tert-butylcatecholate N2 - Five new catalysts are prepared from dibutyltin oxide and catechol (HCa), 2,3-dihydroxynaphthalene (NaCa), 4-tert-butyl catechol (BuCa), 4-cyano catechol (CyCa), and 4-benzoyl catechol (BzCa), but only BuCa gives useful results. When benzyl alcohol is used as an initiator, linear chains having benzyl ester end groups are formed in a slow polymerization process. In contrast to cyclic or noncyclic dibutyltin bisalkoxides, neat BuCa yields cyclic poly(l-lactide)s via a fast ring-expansion polymerization. Under certain conditions, a high-melting crystalline phase (Tm = 191 °C) is obtained. At 160 °C and short reaction times even-numbered cycles are slightly prevailing, but, surprisingly, at 120 °C, odd-numbered cycles are predominantly formed. These results definitely prove that a ring-expansion mechanism is operating. KW - Lactides KW - MALDI TOF MS KW - Morphology KW - Ring-opening polymerization KW - Tin catalysts PY - 2017 DO - https://doi.org/10.1002/macp.201700274 SN - 1521-3935 SN - 1022-1352 VL - 218 IS - 22 SP - 1700274, 1 EP - 1700274, 10 PB - Wiley VCH CY - Weinheim AN - OPUS4-43583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen A1 - Scheliga, F. T1 - Cyclic poly(L-lactide)s via ring-expansion polymerizations catalysed by 2,2-dibutyl-2- stanna-1,3-dithiolane N2 - L-Lactides were polymerized in bulk at 120 or 160 °C with cyclic dibutyltin catalysts derived from 1,2-dimercaptoethane or 2-mercaptoethanol. Only linear chains having one benzyl ester and one OH-end group were obtained when benzyl alcohol was added. When L-lactides were polymerized with neat dibutyl-2-stanna-1,3-dithiolane, exclusively cyclic polylactides were formed even at 120 °C. The temperature, time and monomer/catalyst ratio (M/C) were varied. These results are best explained by a combination of ring-expansion polymerization and ring-extrusion of cyclic oligo- or polylactides with Elimination of the cyclic catalyst. Neither syntheses of linear polylactides nor of cyclic lactides involved racemization up to 20 h at 160 °C. KW - Ring-expansion polymerization KW - MALDI KW - Polylactides PY - 2017 DO - https://doi.org/10.1039/C6PY02166B SN - 1759-9954 SN - 1759-9962 VL - 8 IS - 9 SP - 1589 EP - 1596 PB - Royal Society of Chemistry AN - OPUS4-39748 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen A1 - Scheliga, F. T1 - Cyclic Polylactides via Simultaneous Ring-Opening Polymerization and Polycondensation Catalyzed by Dibutyltin Mercaptides N2 - L-Lactide is polymerized in bulk at 160 8C either with dibutyltin bis(benzylmercaptide) (SnSBzl), dibutyltin bis(benzothiazole 2-mercaptide) (SnMBT), or with dibutyltin bis(pentafluorothiophenolate) (SnSPF) as catalysts. SnSBzl yields linear polylactides having benzylthio-ester end groups in addition to cyclic polylactides, whereas SnMBT and SnSPF mainly or exclusively yield cyclic polylactides. This finding, together with model reactions, indicates that the SnS catalysts promote a combined ring-opening polymerization and polycondensation process including end-to-end cyclization. SnMBT caused slight racemization (3%–5%), when used at 160 8C. With SnSPF optically pure cyclic poly(L-lactide)s with high-molecular weights can be prepared at 160 8C. KW - Cyclopolymerization KW - Catalysts KW - MALDI-TOF MS KW - Polyester KW - Ring-opening polymerization PY - 2017 DO - https://doi.org/10.1002/pola.28762 VL - 55 IS - 22 SP - 3767 EP - 3775 PB - Wiley Periodicals AN - OPUS4-42600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. A1 - Weidner, Steffen A1 - Scheliga, F. ED - Shaplov, A. T1 - Cyclization and dispersity of polyesters N2 - Two classes of polyesters were prepared by irreversible polycondensations. The dependence of the dispersities on the experimental parameters such as synthetic method, chemical structure, molecular weight and initial monomer concentration was determined. At first it was demonstrated that it is essential for a correct calculation of Mn and Mw to include all oligomers down to the dimers in the evaluation of SEC curves. Furthermore, it was demonstrated for poly(e-caprolactone)s and polylactides that reversible polycondensations and ring-opening polymerizations with equilibration yield identical products. Finally, the dependence of the dispersity on various experimental Parameters was determined for equilibrated poly(e-caprolactone)s and polylactides. KW - Irreversible polycondensation KW - Polycaprolactone KW - Polylactide KW - Dispersity KW - MALDI-TOF MS PY - 2017 DO - https://doi.org/10.1002/masy.201600169 SN - 1022-1360 SN - 1521-3900 VL - 375 IS - 1 SP - Article 1600169, 1 EP - 6 PB - Wiley-VCH AN - OPUS4-42407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zerbst, Uwe A1 - Hilgenberg, Kai T1 - Damage development and damage tolerance of structures manufactured by selective laser melting - a review N2 - The additive manufacturing technology of Selective Laser Melting (SLM) experiences a rapid development within an increasing marked of quite different application fields. The properties of SLM materials and structures are influenced by a number of tech-nological parameters such as the metal powder (particle size, homogeneity, cleanliness), the laser tool (power, beam diameter, pulse lengths), the scanning operation (speed, sequence and orientation of melting paths), parameters of the over-all equipment (design and preheating of the base plate, currents and turbulence in the protective gas atmosphere) and, last not least, the hatching strategy including the build-up direction of the structure with respect to the loading direction of the component. For the perspective use of SLM structures as load carrying, safety-relevant components the knowledge of their mechanical properties is necessary. It is essential to understand these in the context of the manufacturing-related features and at the back-ground of the basic characteristics of metallic materials: crystal lattice, microstructure and material defects. The paper provides an overview on factors which affect the mechanical parameters stiffness, strength, ductility, toughness, fatigue crack propagation and fatigue strength in the context of selective laser melting. T2 - FDMD 2017 CY - Lecco, Italy DA - 19.09.2017 KW - Fatigue strength KW - Fracture mechanics KW - Initial crack size KW - Short crack propagation KW - Multiple crack propagation PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-438511 DO - https://doi.org/10.1016/j.prostr.2017.11.071 SN - 2452-3216 VL - 7 SP - 141 EP - 148 PB - ScienceDirect CY - Lecco, Italy AN - OPUS4-43851 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madkour, Sherif A1 - Szymoniak, Paulina A1 - Hertwig, Andreas A1 - Heidari, M. A1 - von Klitzing, R. A1 - Napolitano, S. A1 - Sferrazza, M. A1 - Schönhals, Andreas T1 - Decoupling of dynamic and thermal glass transition in thin films of a PVME/PS blend N2 - The discussions on the nanoconfinement effect on the glass transition and glassy dynamics phenomena have yielded many open questions. Here, the thickness dependence of the thermal glass transition temperature of thin films of a PVME/PS blend is investigated by ellipsometry. Its thickness dependence was compared to that of the dynamic glass transition (measured by specific heat spectroscopy), and the deduced Vogel temperature (T0). While and T0 showed a monotonous increase, with decreasing the film thickness, the dynamic glass transition temperature () measured at a finite frequency showed a non-monotonous dependence that peaks at 30 nm. This was discussed by assuming different cooperativity length scales at these temperatures, which have different sensitivities to composition and thickness. This non-monotonous thickness dependence of disappears for frequencies characteristic for T0. Further analysis of the fragility parameter, showed a change in the glassy dynamics from strong to fragile, with decreasing film thickness. KW - Thin polymeric films KW - Ellipsometry KW - Specific heat spectroscopy PY - 2017 DO - https://doi.org/10.1021/acsmacrolett.7b00625 SN - 2161-1653 VL - 6 IS - 10 SP - 1156 EP - 1161 PB - ACS Publications AN - OPUS4-42266 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 - Przondziono, R. A1 - Timothy, J. J. A1 - Weise, Frank A1 - Krütt, Enno A1 - Breitenbücher, R. A1 - Meschke, G. A1 - Hofmann, M. T1 - Degradation in concrete structures due to cyclic loading and its effect on transport processes - Experiments and modeling N2 - According to the objectives of the research group 1498, this paper deals with degradation effects in concrete structures that are caused by cyclic flexural loading. The goal is to determine their influence on the fluid transport processes within the material on the basis of experimental results and numerical simulations. The overall question was, to which extent the ingress of externally supplied alkalis and subsequently an alkali-silica reaction are affected by such modifications in the microstructure. Degradation in the concrete microstructure is characterized by ultrasonic wave measurements as well as by microscopic crack analysis. Furthermore, experiments on the penetration behavior of water into the investigated materials were performed. The penetration behavior into predamaged concrete microstructures was examined by the classical Karsten tube experiment, nuclear magnetic resonance method, and time domain reflectometry techniques. In order to create an appropriate model of the material's degradation on the water transport, the Darcy law was applied to describe the flow in partially saturated concrete. Material degradation is taken into account by an effective permeability that is dependent on the state of degradation. This effective permeability is obtained by the micromechanical homogenisation of the flow in an Representative Elementary Volume (REV) with distributed ellipsoidal microcracks embedded in a porous medium. The data gained in the microscopic crack analysis is used as input for the micromechanical model. Finite element simulations for unsaturated flow using the micromechanical model were compared with the experimental results showing good qualitative and quantitative agreement. KW - Alkali ingress KW - Alkali-silica reaction KW - Computational model for unsaturated flow KW - Cyclic loading KW - Degradation KW - Micromechanics model KW - Transport processes PY - 2017 DO - https://doi.org/10.1002/suco.201600180 SN - 1751-7648 SN - 1464-4177 VL - 18 IS - 4 SP - 519 EP - 527 PB - Ernst & Sohn AN - OPUS4-41008 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Daniel A1 - Hertwig, Andreas A1 - Beck, Uwe A1 - Negendank, Detlef A1 - Lohse, Volkmar A1 - Kormunda, M. A1 - Esser, N. T1 - Dependence of the optical constants and the performance in the SPREE gas measurement on the thickness of doped tin oxide over coatings N2 - In this study, thickness related changes of the optical properties of doped tin oxide were studied. Two different sets of samples were prepared. The first set was doped with iron or nickel on silicon substrate with thicknesses of 29–56 nm, the second was iron doped on gold/glass substrate with 1.6–6.3 nm. The optical constants were determined by using spectral ellipsometry (SE) followed by modelling of the dielectric function with an oscillator model using Gaussian peaks. The analysis of the optical constants shows a dependence of the refraction and the absorption on the thickness of the doped tin oxide coating. In addition to the tin oxide absorption in the UV, one additional absorption peak was found in the near-IR/red which is related to plasmonic effects due to the doping. This peak shifts from the near-IR to the red part of the visible spectrum and becomes stronger by reducing the thickness, probably due to the formation of metal nanoparticles in this layer. These results were found for two different sets of samples by using the same optical model. Afterwards the second sample set was tested in the Surface Plasmon Resonance Enhanced Ellipsometric (SPREE) gas measurement with CO gas. It was found that the thickness has significant influence on the sensitivity and thus the adsorption of the CO gas. By increasing the thickness from 1.6 nm to 5.1 nm, the sensing ability is enhanced due to a higher coverage of the surface with the over coating. This is explained by the high affinity of CO molecules to the incorporated Fe-nanoparticles in the tin oxide coating. By increasing the thickness further to 6.3 nm, the sensing ability drops because the layer disturbs the SPR sensing effect too much. T2 - 7th International Conference on Spectroscopic Ellipsometry (ICSE-7) DA - 06.06.2016 KW - Surface plasmon resonance KW - Spectroscopic ellipsometry KW - Doped tin oxide KW - Gas sensing KW - Plasmonic absorption PY - 2017 DO - https://doi.org/10.1016/j.apsusc.2016.11.188 SN - 0169-4332 VL - 421, Teil B SP - 480 EP - 486 PB - Elsevier B.V. AN - OPUS4-42692 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilrich, T. 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 - Seidel, R. A1 - Kraffert, K. A1 - Kabelitz, Anke A1 - Pohl, M.N. A1 - Kraehnert, R. A1 - Emmerling, Franziska A1 - Winter, B. T1 - Detection of the electronic structure of iron-(III)-oxo oligomers forming in aqueous solutions N2 - The nature of the small iron-oxo oligomers in iron-(III) aqueous solutions has a determining effect on the chemical processes that govern the formation of nanoparticles in aqueous phase. Here we report on a liquid-Jet photoelectron-spectroscopy experiment for the investigation of the electronic structure of the occurring iron-oxo oligomers in FeCl3 aqueous solutions. The only iron species in the as-prepared 0.75 M solution are Fe3+ monomers. Addition of NaOH initiates Fe3+ hydrolysis which is followed by the formation of iron-oxo oligomers. At small enough NaOH concentrations, corresponding to approximately [OH]/[Fe] = 0.2–0.25 ratio, the iron oligomers can be stabilized for several hours without engaging in further aggregation. Here, we apply a combination of non-resonant as well as iron 2p and Oxygen 1s resonant photoelectron spectroscopy from a liquid microjet to detect the electronic structure of the occurring species. Specifically, the oxygen 1s partial electron yield X-ray absorption (PEY-XA) spectra are found to exhibit a peak well below the onset of liquid water and OH (aq) absorption. The iron 2p absorption gives rise to signal centered between the main absorption bands typical for aqueous Fe3+. Absorption bands in both PEY-XA spectra are found to correlate with an enhanced photoelectron Peak near 20 eV binding energy, which demonstrates the sensitivity of resonant photoelectron (RPE) spectroscopy to mixing between iron and ligand orbitals. These various signals from the iron-oxo oligomers exhibit Maximum intensity at [OH]/[Fe] = 0.25 ratio. For the same ratio, we observe changes in the pH as well as in complementary Raman spectra, which can be assigned to the Transition from monomeric to oligomeric species. At approximately [OH]/[Fe] = 0.3 we begin to observe particles larger than 1 nm in radius, detected by small-angle X-ray scattering. KW - Iron-oxo oligomers KW - XPS KW - Electronic structure PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-433468 DO - https://doi.org/10.1039/c7cp06945f SN - 1463-9076 SN - 1463-9084 VL - 19 IS - 48 SP - 32226 EP - 32234 AN - OPUS4-43346 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute ED - Scholz, Norman ED - Behnke, Thomas T1 - Determination of the critical micelle concentration of neutral and ionic surfactants with fluorometry, conductometry, and surface tension - a method comparison N2 - Micelles are of increasing importance as versatile carriers for hydrophobic substances and nanoprobes for a wide range of pharmaceutical, diagnostic, medical, and therapeutic applications. A key Parameter indicating the Formation and stability of micelles is the critical micelle concentration (CMC). In this respect, we determined the CMC of common anionic, cationic, and non-ionic surfactants fluorometrically using different fluorescent probes and fluorescence Parameters for Signal detection and ompared the results with conductometric and surface Tension measurements. Based upon These results, requirements, Advantages, and pitfalls of each methods are discussed. Our study underlines the versatility of fluorometric methods that do not impose specific requirements on surfactants and are especially suited for the quantification of very low CMC values. Conductivity and surface Tension measurements yield smaller uncertainties particularly for high CMC values, yet are more time- and substance consuming and not suitable for every surfactant. KW - Fluorescence KW - Methods KW - Critical micelle concentration (CMC) KW - Conductometry KW - Fluorescence probe KW - Dye KW - Nile Red KW - Pitfalls KW - Method evaluation KW - Uncertainty PY - 2017 DO - https://doi.org/10.1007/s10895-018-2209-4 SN - 1053-0509 SN - 1573-4994 VL - 28 IS - 1 SP - 465 EP - 476 AN - OPUS4-43905 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 - Adel-Khattab, D. A1 - Giacomini, F. A1 - Gildenhaar, R. A1 - Berger, G. A1 - Gomes, Cynthia A1 - Linow, Ulf A1 - Hardt, M. A1 - Peleska, B. A1 - Günster, Jens A1 - Stiller, M. A1 - Houshmand, A. A1 - Ghaffar, K. A1 - Gamal, A. A1 - El-Mofty, M. A1 - Knabe, C. T1 - Development of a synthetic tissue engineered three- dimensional printed bioceramic-based bone graft with homogenously distributed osteoblasts and mineralizing bone matrix in vitro N2 - Over the last decade there have been increasing efforts to develop three-dimensional (3D) scaffolds for bone tissue Engineering from bioactive ceramics with 3D printing emerging as a promising technology. The overall objective of the present study was to generate a tissue engineered synthetic bone graft with homogenously distributed osteoblasts and mineralizing bone Matrix in vitro, thereby mimicking the advantageous properties of autogenous bone grafts and facilitating usage for reconstructing segmental discontinuity defects in vivo . To this end, 3D scaffolds were developed from a silica-containing calcium alkali orthophosphate, using, fi rst, a replica technique – the Schwartzwalder – Somers method – and, second, 3D printing, (i.e. rapid prototyping). The mechanical and physical scaffold properties and their potential to facilitate homogenous colonization by osteogenic cells and extracellular bone matrix formation throughout the porous scaffold architecture were examined. Osteoblastic cells were dynamically cultured for 7 days on both scaffold types with two different concentrations of 1.5 and 3 × 10⁹ cells/l. The amount of cells and bone matrix formed and osteogenic marker expression were evaluated using hard tissue histology, immunohistochemical and histomorphometric analysis. 3D-printed scaffolds (RPS) exhibited more micropores, greater compressive strength and silica release. RPS seeded with 3 × 10⁹ cells/l displayed greatest cell and extracellular Matrix formation, mineralization and osteocalcin expression. In conclusion, RPS displayed superior mechanical and biological properties and facilitated generating a tissue engineered synthetic bone graft in vitro, which mimics the advantageous properties of autogenous bone grafts, by containing homogenously distributed terminally differentiated osteoblasts and mineralizing bone matrix and therefore is suitable for subsequent in vivo implantation for regenerating segmental discontinuity bone defects. KW - Bone tissue engineering KW - Calcium alkali orthophosphate KW - Rapid prototyping KW - Scaffold KW - Mandible PY - 2017 DO - https://doi.org/10.1002/term.2362 SN - 1932-6254 SN - 1932-7005 VL - 12 IS - 1 SP - 44 EP - 58 PB - Wiley Online Library AN - OPUS4-40745 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Philipp A1 - Miccoli, Lorenzo A1 - Fontana, Patrick A1 - Ziegert, C. T1 - Development of partial safety factors for earth block masonry N2 - The main aim of the research was the development of a first valid database for material parameters of earth block masonry (EBM) with particular regard to statistical characteristics. A solid database is needed for the determination of the materials partial safety factor. Therefore, compressive strength tests were carried out with two types of earth blocks and two types of prefabricated earth mortar. The evaluation has shown that the mean variation of the compressive strength was remarkably less than expected, which indicates high quality standards of the components earth block and mortar with regard to industrial production. Using the reliability method, a partial safety factor for EBM subjected to compression was determined on the basis of these test results. The findings have shown that a common calculation method for EBM based on partial safety factors following the valid masonry construction standard is feasible. KW - Partial safety factor KW - Earth block masonry (EBM) KW - Reliability KW - Compressive strength PY - 2017 DO - https://doi.org/10.1617/s11527-016-0902-9 SN - 1871-6873 SN - 1359-5997 VL - 50 IS - 1 SP - 1 EP - 14 PB - Springer AN - OPUS4-38937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Asadujjaman, Asad A1 - Bertin, Annabelle A1 - Schönhals, Andreas T1 - Dielectric analysis of the upper critical solution temperature behaviour of a poly(acrylamide-coacrylonitrile) copolymer system in water N2 - A copolymer consisting of acrylamide (AAm) and acrylonitrile (AN) in aqueous solution was investigated using broadband dielectric spectroscopy at frequencies between 10⁻¹ Hz and 10⁶ Hz in the temperature range from 2 °C to 60 °C. This system shows an UCST phase behavior. The phase transition and aggregation behavior is monitored by both the temperature and frequency dependence of the complex conductivity σ*(f, T), where the AN fraction and the concentration of the solution were varied. Additionally, the dielectric data are compared with the results obtained from dynamic light scattering measurements. The temperature dependence of the DC conductivity (σDC) of the copolymer solution is monitored and the phase transition temperature (PTT) of the poly(AAm-co-AN) copolymer is deduced from a change in the T-dependence of the DC conductivity. The change in σDC can be explained by decreased effective charge carrier mobility and a reduction of the effective charge number density at temperatures below the phase Transition temperature of the poly(AAm-co-AN) solution. A pronounced interfacial polarization effect on the frequency dependence of the real part of the conductivity (σ') is observed at temperatures below the phase Transition temperature. The charge carriers are blocked at the formed aggregates giving rise to this interfacial polarization. The dependence of the interfacial polarization on the acrylonitrile fraction in the copolymer and the concentration of the solution is studied in detail and conclusions concerning the internal structures of the copolymer aggregates are drawn. KW - Thermoresponsive polymres PY - 2017 DO - https://doi.org/10.1039/c6sm02684b SN - 1744-6848 SN - 1744-683X VL - 13 IS - 12 SP - 2384 EP - 2393 PB - Royl Society of Chemistry Publishing AN - OPUS4-39556 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kömmling, Anja A1 - Chatzigiannakis, E. A1 - Beckmann, Jörg A1 - Wachtendorf, Volker A1 - von der Ehe, Kerstin A1 - Braun, Ulrike A1 - Jaunich, Matthias A1 - Schade, U. A1 - Wolff, Dietmar T1 - Discoloration Effects of High-Dose gamma-Irradiation and Long-Term Thermal Aging of (U) HMW-PE N2 - Two polyethylene types with ultra-high (UHMWPE) and high molecular weight (HMW-PE) used as neutron radiation shielding materials in casks for radioactive waste were irradiated with doses up to 600 kGy using a 60Co gammasource. Subsequently, thermal aging at 125∘C was applied for up to one year. Degradation effects in the materials were characterized using colorimetry, UV-Visspectroscopy, IR spectroscopy, and DSC. Both materials exhibited a yellowing upon irradiation.The discoloration of UHMW-PE disappeared again after thermal aging.Therefore, the yellowing is assumed to originate fromannealable color centers in the formof free radicals that are trapped in the crystalline regions of the polymer and recombine at elevated temperatures. For the antioxidantcontaining HMWPE, yellowing was observed after both irradiation and thermal aging. The color change was correlated mainly to decomposition products of the antioxidant in addition to trapped radicals as in UHMW-PE. Additionally, black spots appeared after thermal aging of HMW-PE. KW - Irradiation KW - UHMWPE KW - Colour center KW - Yellowness index PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-423992 DO - https://doi.org/10.1155/2017/1362491 SN - 1687-9422 VL - 2017 IS - Article ID 1362491 SP - 1 EP - 10 PB - Hindawi AN - OPUS4-42399 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 - TY - JOUR A1 - Klingelhöffer, 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” by H. Li, X. Zhou, J. Shen, and D. Luo. The regular article was published in journal of Testing and Evaluation, Vol. 45, No. 3, 2017, pp. 723–731, doi:10.1520/ JTE20150479. ISSN 0090-3973 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 - Tnsile testing KW - ISO 6892-1 KW - TENSTAND WP4 Report PY - 2017 UR - www.astm.org DO - https://doi.org/10.1520/JTE20160526 SN - 0090-3973 VL - 45 IS - 3 SP - 1105 EP - 1114 PB - ASTM CY - West Conshohocken, PA, USA AN - OPUS4-46690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bender, P A1 - Balceris, C. A1 - Ludwig, F A1 - Posth, O A1 - Bogart, L. K. A1 - Szczerba, Wojciech A1 - Castro, A A1 - Nilsson, L A1 - Costo, R A1 - Gavilan, H A1 - Gonzalez-Alonso, D A1 - de Pedro, I A1 - Barquin, L. F. A1 - Johansson, C T1 - Distribution functions of magnetic nanoparticles determined by a numerical inversion method N2 - In the present study, we applied a regularized inversion method to extract the particle size, magnetic moment and relaxation-time distribution of magnetic nanoparticles from small-angle x-ray scattering (SAXS), DC magnetization (DCM) and AC susceptibility (ACS) measurements. For the measurements the particles were colloidally dispersed in water. At first approximation the particles could be assumed to be spherically shaped and homogeneously magnetized single-domain particles. As model functions for the inversion, we used the particle form factor of a sphere (SAXS), the Langevin function (DCM) and the Debye model (ACS). The extracted distributions exhibited features/peaks that could be distinctly attributed to the individually dispersed and non-interacting nanoparticles. Further analysis of these peaks enabled, in combination with a prior characterization of the particle ensemble by electron microscopy and dynamic light scattering, a detailed structural and magnetic characterization of the particles. Additionally, all three extracted distributions featured peaks, which indicated deviations of the scattering (SAXS), magnetization (DCM) or relaxation (ACS) behavior from the one expected for individually dispersed, homogeneously magnetized nanoparticles. These deviations could be mainly attributed to partial agglomeration (SAXS, DCM, ACS), uncorrelated surface spins (DCM) and/or intra-well relaxation processes (ACS). The main advantage of the numerical inversion method is that no ad hoc assumptions regarding the line shape of the extracted distribution functions are required, which enabled the detection of these contributions. We highlighted this by comparing the results with the results obtained by standard model fits, where the functional form of the distributions was a priori assumed to be log-normal shaped. KW - SAXS KW - Small-angle X-ray scattering KW - Nanoparticle PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-429373 DO - https://doi.org/10.1088/1367-2630/aa73b4 SN - 1367-2630 VL - 19 SP - 073012, 1 EP - 073012, 19 PB - IOP Publ. Ltd. AN - OPUS4-42937 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 - Mitova, M. A1 - Iliev, M. A1 - Nováková, A. A1 - Gorbushina, Anna A1 - Groudeva, V.I. A1 - Martin-Sanchez, Pedro Maria T1 - Diversity and biocide susceptibility of fungal assemblages dwelling in the Art Gallery of Magura Cave, Bulgaria N2 - Magura Cave, north-western Bulgaria, possesses valuable rock-art paintings made with bat guano and dated from the period between the Eneolithic and Bronze Ages. Since 2008, the Art Gallery is closed to the general public in order to protect the paintings from vandalism, microclimatic changes caused by visitors and artificial illumination, and the consequent growth of fungi and phototrophs. Nevertheless, some tourist visits are allowed under the supervision of cave managers. This study provides the first scientific report on cultivable fungal assemblages dwelling different substrata in the Art Gallery. A total of 78 strains, belonging to 37 OTUs (Ascomycota 81%, Zygomycota 13%, Basidiomycota 5%), were isolated in the study. This fungal diversity was clearly dominated by Penicillium (50% of strains) and Aspergillus (13%). The most relevant visible fungal colonies were detected in sediments rich in bat guano, where, besides Penicillium, other guanophilic fungi such as Mucor, Mortierella, Trichosporon and Trichoderma were dominant. Conversely, scarce fungi were detected on rock surface of painted walls. Based on the biocide susceptibility assay, octylisothiazolinone (OIT) and benzalkonium chloride (BAC) were effective inhibiting the in vitro growth of dominant fungal species in Magura Cave, when applied at concentrations ranged from 100 to 1,000 mg/L. These data provide a valuable knowledge about Magura fungi, and exemplify a type of preliminary test that may be conducted before planning any biocide treatment. However, considering the irreversible effects of biocides on the ecological balance in caves, and the low fungal contamination in painted walls of Magura Cave, there is no reason to use conventional biocides in this cave. Further studies, monitoring microbial communities and microclimatic parameters, should be conducted to improve the knowledge on microbial ecology in Magura Cave and possible human impacts, as well as to allow the early detection of potential microbial outbreaks. KW - Fungi KW - Rock-art caves KW - Biocides PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-397436 DO - https://doi.org/10.5038/1827-806X.46.1.2061 SN - 0392-6672 VL - 46 IS - 1 SP - 67 EP - 80 PB - Scholar Commons CY - Tampa, FL, USA AN - OPUS4-39743 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lichtenstein, D. A1 - Meyer, T. A1 - Böhmert, L. A1 - Juling, S. A1 - Fahrenson, C. A1 - Selve, S. A1 - Thünemann, Andreas A1 - Meijer, J. A1 - Estrela-Lopis, I. A1 - Braeuning, A. A1 - Lampen, A. T1 - Dosimetric quantification of coating-related uptake of silver nanoparticles N2 - The elucidation of mechanisms underlying the cellular uptake of nanoparticles (NPs) is an important topic in nanotoxicological research. Most studies dealing with silver NP uptake provide only qualitative data about internalization efficiency and do not consider NP-specific dosimetry. Therefore, we performed a comprehensive comparison of the cellular uptake of differently coated silver NPs of comparable size in different human intestinal Caco-2 cell-derived models to cover also the influence of the intestinal mucus barrier and uptake-specialized M-cells. We used a combination of the Transwell system, transmission electron microscopy, atomic absorption spectroscopy, and ion beam microscopy techniques. The computational in vitro sedimentation, diffusion, and dosimetry (ISDD) model was used to determine the effective dose of the particles in vitro based on their individual physicochemical characteristics. Data indicate that silver NPs with a similar size and shape show coating-dependent differences in their uptake into Caco-2 cells. The internalization of silver NPs was enhanced in uptake-specialized M-cells while the mucus did not provide a substantial barrier for NP internalization. ISDD modeling revealed a fivefold underestimation of dose–response relationships of NPs in in vitro assays. In summary, the present study provides dosimetry-adjusted quantitative data about the influence of NP coating materials in cellular uptake into human intestinal cells. Underestimation of particle effects in vitro might be prevented by using dosimetry models and by considering cell models with greater proximity to the in vivo situation, such as the M-cell model. KW - Silver nanoparticles KW - Small-angle X-ray scattering KW - Saxs PY - 2017 DO - https://doi.org/10.1021/acs.langmuir.7b01851 SN - 0743-7463 VL - 33 IS - 45 SP - 13087 EP - 13097 PB - Americal Chemical Society AN - OPUS4-42875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Falkenreck, Thora A1 - Klein, M. A1 - Böllinghaus, Thomas T1 - Dynamic compressive behaviour of weld joints N2 - Materials used in military applications have to withstand multiple threats like ballistics and explosions. Thus, high-strength low alloyed (HSLA) steels are used. The main joining technique for metals is welding. Therefore, analysing the dynamic impact behaviour of high-strength welds is very important to fulfil these demands. Investigation of welds at high strain rates has rarely been conducted in the past. To determine the dynamic impact behaviour of hybrid laser-arc welds, the Split Hopkinson Pressure Bar (SHPB) technique was used. The base material was a quenched and tempered fine-grained armour steel with yield strength of 1100 MPa. First, a full hybrid laser-arc weld was investigated by extracting specimens consisting of weld metal and heat affected base material. The influence of two variables, the cooling time between 800 °C and 500 °C (t8/5) and strength of filler material, on the impact behaviour was studied. The cooling time t8/5 was varied by preheating to influence the microstructure in the HAZ and to analyse the effect on the hardness and dynamic compressive strength. Subsequent analysis to detail the original Investigation was carried out by dilatometer heat treatment of specimens to create homogenous subzones of the weld. These specimens have a homogenous microstructure of HAZ and were tested by SHPB to determine the stress-strain characteristics for the different microstructures of HAZ. The results of the weld specimen showed the effect of preheating and filler material strength on the dynamic compressive behaviour. The analysis of the different microstructures of the HAZ indicated that especially the tempered microstructure caused a reduction in dynamic compressive strength. KW - SHPB KW - Hybrid laser-arc weld KW - Dilatometry PY - 2017 DO - https://doi.org/10.1016/j.msea.2017.07.032 SN - 0921-5093 SN - 1873-4936 VL - 702 SP - 322 EP - 330 AN - OPUS4-41904 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Babutzka, Martin A1 - Heyn, A. T1 - Dynamic tafel factor adaption for the evaluation of instantaneous corrosion rates on zinc by using gel-type electrolytes N2 - The paper presents a new method for the determination and evaluation of tafel factors using gel-type electrolytes and electrochemical frequency modulation technique (EFM). This relatively new electrochemical method offers the possibility to determine both polarization resistances and tafel factors within one measurement and in short measuring intervals. Starting from a comprehensive parameter study it is shown that a direct relationship between the two values exists that can be described mathematically. This contribution presents the determined tafel factors for the system gel-type electrolyte/zinc and discusses their applicability and their limits. T2 - 19th Chemnitz Seminar on Materials Engineering – 19. Werkstofftechnisches Kolloquium CY - Chemnitz, Germany DA - 16.03.2017 KW - Gel-type electrolytes KW - Gelartige Elektrolyte KW - Zinc KW - Zink KW - Stern Geary constant KW - Stern-Geary-Konstante PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-394324 UR - http://iopscience.iop.org/article/10.1088/1757-899X/181/1/012021/pdf DO - https://doi.org/10.1088/1757-899X/181/1/012021 SN - 1757-899X SN - 1757-8981 VL - 181 IS - Conference 1 SP - Article UNSP 012021, 1 EP - 11 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-39432 LA - eng 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 - Schröter, Maria-Astrid A1 - Meyer, Susann A1 - Hahn, Marc Benjamin A1 - Solomun, Tihomir A1 - Sturm, Heinz A1 - Kunte, Hans-Jörg T1 - Ectoine protects DNA from damage by ionizing radiation N2 - Ectoine plays an important role in protecting biomolecules and entire cells against environmental stressors such as salinity, freezing, drying and high temperatures. Recent studies revealed that ectoine also provides effective protection for human skin cells from damage caused by UV-A radiation. These protective properties make ectoine a valuable compound and it is applied as an active ingredient in numerous pharmaceutical devices and cosmetics. Interestingly, the underlying mechanism resulting in protecting cells from radiation is not yet fully understood. Here we present a study on ectoine and its protective influence on DNA during electron irradiation. Applying gel electrophoresis and atomic force microscopy, we demonstrate for the first time that ectoine prevents DNA strand breaks caused by ionizing electron radiation. The results presented here point to future applications of ectoine for instance in cancer radiation therapy. KW - Plasmid DNA pUC19 KW - Electron irradiation 30 [kV] KW - Effective irradiation dose 0.2-16 [Gy] KW - Gel electrophoresis KW - AFM intermittent contact KW - Radioprotector ectoine KW - Compatible solute PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-428287 DO - https://doi.org/10.1038/s41598-017-15512-4 SN - 2045-2322 VL - 7 IS - 1 SP - 15272, 1 EP - 15272, 7 PB - Nature AN - OPUS4-42828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kingelhöffer, Hellmuth A1 - Affeldt, E. E. A1 - Bache, M. A1 - Bartsch, M. A1 - Beck, T. A1 - Christ, H. J. A1 - Fedelich, Bernard A1 - Hähner, P. A1 - Holdsworth, S. R. A1 - Lang, K.-H. A1 - McGaw, M. A1 - Olbricht, Jürgen A1 - Remy, L. A1 - Skrotzki, Birgit A1 - Stekovich, S. T1 - Editorial - Special issue: Recent developments in thermo-mechanical fatigue N2 - Components in the Aerospace, Power and Automotive engineering sectors are frequently subjected to cyclic stresses induced by thermal fluctuations and mechanical loads. For the design of such components, reliable material property data are required which need to be acquired using well accepted and reproducible test procedures for thermo-mechanical fatigue (TMF) loading. There is limited availability of proven TMF data indicating there is need for further research and testing. The TMF behaviour of materials is often desired to be simulated in models which describe the cyclic stress-strain behaviour, the fatigue life and the cyclic crack growth behaviour. There is a continuous need for the development and amendment of such models. Models can be validated by using materials in industrial applications which are subjected to TMF loading. The 3rd Workshop on Thermo-Mechanical Fatigue was held on 27–29 April 2016 at BAM, Berlin, Germany. The workshop was attended by 90 attendees coming from 17 countries in the world. 38 presentations including five poster presentations were held. The following topics were covered by the workshop: – TMF of materials coated with Thermal Barrier Coatings. – Thermal Gradient Mechanical Fatigue. – TMF crack growth. – TMF + High Cycle Fatigue. – TMF Modelling and Lifetime Prediction. – TMF Properties of steels, cast iron, Al-, Mg- and Ni-alloys – Advanced TMF Testing Techniques. – Industrial Applications. A panel discussion was held regarding the present state of TMF testing standards (ISO and ASTM) and their potential for improvement. The discussion and contributions were summarized and forwarded to the standard committees. The 3rd TMF-Workshop ensured the continuation of international exchange of knowledge providing a forum to present and discuss all recent developments in the field of thermo-mechanical fatigue. The current special issue publishes eleven selected papers of the 3rd TMF-Workshop 2016. The papers were peer reviewed by a number of experts in the Thermo-Mechanical Fatigue sector. I hope you will enjoy reading papers of this special issue. T2 - 3rd International Workshop on Thermo-Mechanical Fatigue (TMF-Workshop 2016) CY - Berlin, Germany DA - 27.04.2016 KW - Fatigue damage KW - Thermo-mechanical fatigue KW - Fatigue life time KW - Life time prediction KW - TMF PY - 2017 DO - https://doi.org/10.1016/j.ijfatigue.2017.02.002 SN - 0142-1123 VL - 99 IS - 2 SP - 215 PB - Elsevier CY - Oxford AN - OPUS4-40895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hertwig, Andreas A1 - Hinrichs, K. A1 - Beck, Uwe A1 - Esser, N. T1 - Editorial to the proceedings of the 7th conference on spectroscopic N2 - The 7th International Conference on Spectroscopic Ellipsometry (ICSE-7) was held in Berlin in June 2016, jointly organised by ICSE and BAM. The publication of the proceedings special issue in Applied Surface Science follows this event. In the special issue, about 100 articles on current topics of optics and surface science related to ellipsometry, polarimetry, and similar techniques are presented, underpinning the high significance of these techniques for many fields of materials science. T2 - 7th International Conference on Spectroscopic Ellipsometry, ICSE-7 CY - Berlin, Germany DA - 06.06.2016 KW - Spectroscopic ellipsomety PY - 2017 DO - https://doi.org/10.1016/j.apsusc.2017.04.081 SN - 0169-4332 VL - 2017 IS - 421 SP - 269 EP - 270 PB - Elsevier B.V. AN - OPUS4-42554 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaunich, Matthias T1 - Editorial: Shape memory polymers N2 - In this editorial the focus lies on the testing of shape memory materials. KW - Shape memory polymer KW - Testing PY - 2017 DO - https://doi.org/10.1016/j.polymertesting.2017.08.019 SN - 0142-9418 VL - 62 SP - A1 PB - Elsevier CY - Oxford AN - OPUS4-41714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Linhares, F.N. A1 - Kersch, M. A1 - Niebergall, Ute A1 - Leite, M.Ch.A.M. A1 - Altstädt, V. A1 - Furtado, C.R.G. T1 - Effect of different sulphur-based crosslink networks on the nitrile rubber resistance to biodiesel N2 - Biodiesel possesses some comparable physical properties to petroleum diesel in addition to its improved environmental benefits. Nonetheless, both fuels differ greatly with respect to their chemical compositions. Therefore, the compatibility of the materials, which are commonly employed in contact with diesel, must also be assured for biodiesel. This paper assessed the influence of sulphur-based curing systems on the resistance of nitrile rubber to soybean biodiesel. Formulations were prepared using highacrylonitrile-content nitrile rubber by employing a two-level experimental design. The amounts of two different accelerators and sulphur were varied to achieve different types of vulcanisation systems. Thermal analyses, mechanical tests and microscopy analyses were conducted to evaluate the behaviour of the material after contact with biodiesel. The results showed that the choice of the accelerator played an important role on the resistance of the rubber to the biofuel, and crosslink density was not a key factor with respect to the resistance. KW - Soyean oil KW - Nitrile rubber KW - Compatibility KW - Vulcanisation system KW - Biodiesel KW - Resistance PY - 2017 DO - https://doi.org/10.1016/j.fuel.2016.11.060 SN - 0016-2361 SN - 1873-7153 VL - 191 SP - 130 EP - 139 AN - OPUS4-39006 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cabeza, Sandra A1 - Garces, G. A1 - Adeva, Paloma A1 - Kabra, S. A1 - Gan, W. T1 - Effect of Extrusion Temperature on the Plastic Deformation of an Mg-Y-Zn Alloy Containing LPSO Phase Using In Situ Neutron Diffraction N2 - The evolution of the internal strains during in situ tension and compression tests has been measured in an MgY2Zn1 alloy containing long-period stacking ordered (LPSO) phase using neutron diffraction. The alloy was extruded at two different temperatures to study the influence of the microstructure and texture of the magnesium and the LPSO phases on the deformation mechanisms. The alloy extruded at 623 K (350 °C) exhibits a strong fiber texture with the basal plane parallel to the extrusion direction due to the presence of areas of coarse non-recrystallised grains. However, at 723 K (450 °C), the magnesium phase is fully recrystallised with grains randomly oriented. On the other hand, at the two extrusion temperatures, the LPSO phase orients their basal plane parallel to the extrusion direction. Yield stress is always slightly higher in compression than in tension. Independently on the stress sign and the extrusion temperature, the beginning of plasticity is controlled by the activation of the basal slip system in the dynamic recrystallized grains. Therefore, the elongated fiber-shaped LPSO phase which behaves as the reinforcement in a metal matrix composite is responsible for this tension–compression asymmetry. KW - Mg-Y-Zn Alloy KW - LPSO Phase KW - Neutron Diffraction PY - 2017 DO - https://doi.org/10.1007/s11661-017-4284-6 VL - 48A IS - 11 SP - 5332 EP - 5343 PB - Spinger AN - OPUS4-42935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nadammal, Naresh A1 - Cabeza, Sandra A1 - Mishurova, Tatiana A1 - Thiede, Tobias A1 - Kromm, Arne A1 - Seyfert, Christoph A1 - Farahbod, Lena A1 - Haberland, Christoph A1 - Schneider, Judith Ann A1 - Portella, Pedro Dolabella A1 - Bruno, Giovanni T1 - Effect of hatch length on the development of microstructure, texture and residual stresses in selective laser melted superalloy Inconel 718 N2 - In the present study, samples fabricated by varying the deposition hatch length during selective laser melting of nickel based superalloy Inconel 718 were investigated. Microstructure and texture of these samples was characterized using scanning electron microscopy, combined with electron back-scattered diffraction, and residual stress assessment, using neutron diffraction method. Textured columnar grains oriented along the sample building direction were observed in the shorter hatch length processed sample. A ten-fold increase in the hatch length reduced the texture intensity by a factor of two attributed to the formation of finer grains in the longer hatch length sample. Larger gradients of transverse residual stress in the longer hatch length sample were also observed. Along the build direction, compressive stresses in the shorter hatch length and negligible stresses for the longer hatch length specimen were observed. Changes to the temperature gradient (G) in response to the hatch length variation, influenced the G to growth rate (R) ratio and the product G × R, in agreement with the microstructures and textures formed. For the residual stress development, geometry of the part also played an important role. In summary, tailored isotropy could be induced in Inconel 718 by a careful selection of parameters during selective laser melting. KW - Additive manufacturing KW - Nickel-based superalloy KW - Microstructure and texture KW - Residual stress KW - Electron back-scattered diffraction KW - Neutron diffraction PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S0264127517308018 DO - https://doi.org/10.1016/j.matdes.2017.08.049 SN - 0264-1275 VL - 134 SP - 139 EP - 150 PB - Elsevier CY - Oxford, UK AN - OPUS4-41606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cooper, R. A1 - Bruno, Giovanni A1 - Shyam, A. A1 - Watkins, T. A1 - Pandey, A. A1 - Wheeler, M. T1 - Effect of microcracking on the uniaxial tensile response of beta-eucryptite ceramics: Experiments and constitutive model N2 - A constitutive model for the nonlinear or “pseudoplastic” mechanical behavior in a linear-elastic solid with thermally induced microcracks is developed and applied to experimental results. The model is termed strain dependent microcrack density approximation (SDMDA) and is an extension of the modified differential scheme that describes the slope of the stress-strain curves of microcracked solids. SDMDA allows a continuous variation in the microcrack density with tensile loading. Experimental uniaxial tensile response of β-eucryptite glass and ceramics with controlled levels of microcracking is reported. It is demonstrated that SDMDA can well describe the extent of non-linearity in the experimental uniaxial tensile response of β-eucryptite with varying levels of microcracking. The advantages of the SDMDA are discussed in regard to tensile loading. KW - Microcracking KW - β-eucryptite KW - Young's modulus KW - Modeling KW - Tensile behavior PY - 2017 DO - https://doi.org/10.1016/j.actamat.2017.06.033 SN - 1359-6454 SN - 1873-2453 VL - 135 SP - 361 EP - 371 PB - Elsevier Ltd. AN - OPUS4-40859 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiedmann, A. A1 - Weise, Frank A1 - Kotan, E. A1 - Müller, H. S. A1 - Meng, Birgit T1 - Effects of fatigue loading and alkali-silica reaction on the mechanical behaviour of pavement concrete N2 - The primary aim of this paper is to analyze the impact of mechanical pre-damage and alkali–silica reaction (ASR) on the fracture mechanical properties of pavement concrete. For this purpose, a four point bending test was applied to large format beams to produce a defined level of cyclic pre-damage. The fatigue-induced concrete degradation process was simultaneously recorded using a testing procedure specifically developed for the purpose. In addition, fatigue-induced cracks on extracted drilling cores were spatially visualized and quantified using micro X-ray 3D-computed tomography (3D-CT). The storage of the small-format test specimens, with and without cyclic pre-damage, in an ASR-conducive environment showed that pre-damage leads to an increase in ASR damage processes. Subsequent structural mechanical investigations on small format specimens with and without pre-damage show that fatigue loading and ASR significantly influence fracture mechanical parameters of the concrete. KW - Acoustic emissions analysis KW - Alkali-silica reaction KW - Concrete pavement KW - Fatigue loading KW - Fracture energy KW - Monitoring of damage KW - Tensile strength KW - Ultrasonic velocity PY - 2017 DO - https://doi.org/10.1002/suco.201600179 SN - 1751-7648 SN - 1464-4177 VL - 18 IS - 4 SP - 539 EP - 549 PB - Ernst & Sohn AN - OPUS4-41007 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 -