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 -