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 -