TY - JOUR A1 - Steppan, Enrico A1 - Mantzke, Philipp A1 - Steffens, Benjamin A1 - Rhode, Michael A1 - Kannengießer, Thomas T1 - Thermal desorption analysis for hydrogen trapping in microalloyed high-strength steels N2 - Hydrogen can have an extreme degradation effects in steels, particularly concerning the mechanical properties. These effects can lead to hydrogen-assisted cracking in microalloyed high-strength steels during fabrication and/or operation in industrial applications. In order to study these effects, electrochemically charged tensile specimens were tested to elucidate the degradation of their properties. The carrier gas hot extraction (CGHE) method, which functionally combines a mass spectrometer with a thermal desorption analysis (TDA) process, was used for the detection of ultra-low diffusible hydrogen concentrations in the material specimens. The mass spectrometer provided rapid and automatic determination of hydrogen concentration, whereas the TDA presented the activation energy within the respective test specimen at the specific temperature. Additionally, specimen temperature was carefully monitored to reduce the evaluation error for local effusion peaks. A quenching and deformation dilatometer was used for the analysis of typical heat-affected zones during the welding process for a high reproducibility of the homogenous microstructures that were studied. The present work shows the interaction between hydrogen and lattice defects in different microalloyed materials and heat-affected zones of weldable fine-grained steels. These steels were prepared in a quenched and tempered condition and in a thermo-mechanically rolled condition. These preparations were made according to German standard DIN EN 10025-6 and to DIN EN 10149-2, respectively. The trapping characteristics of two steel grades, S690QL and S700MC, were studied with respect to the activation energy dependent on carbon content and microalloying elements such as Ti, Nb, Mo, Cr, and V. The two steel grades exhibited several types of traps: carbide formations, dislocations, and/or grain boundaries were common, which can influence activation energy and hydrogen solubility. The type and dimension of inclusions or particles also affected the hydrogen trapping behavior. A decrease of carbon and specific alloying elements in thermo-mechanically hot rolled steels led to a change in the activation energy binding the trapped hydrogen. This thermo-mechanically hot rolled steel revealed an increased interaction between hydrogen and precipitations. The higher carbon content in the quenched and tempered steel led to a higher interaction between hydrogen and iron carbide, specifically in the martensitic phase. Furthermore, the trapping behavior in heat-affected zones showed a significant increase in activation energy, especially in the coarse-grained microstructure. These previously mentioned various effects were studied to better understand the degradation of mechanical properties in these two steels. KW - Microalloyed steels KW - Hydrogen embrittlement KW - Heating KW - Chemical analysis KW - Microstructure KW - Heat-affected zone PY - 2017 DO - https://doi.org/10.1007/s40194-017-0451-z SN - 0043-2288 SN - 1878-6669 VL - 61 IS - 4 SP - 637 EP - 648 PB - Springer CY - Berlin Heidelberg AN - OPUS4-40190 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gollnow, C. A1 - Griesche, Axel A1 - Weidemann, Jens A1 - Kannengießer, Thomas T1 - Influence of external loads on a characteristic angle between grains and solidus line as an indicator for hot cracking susceptibility during GTA welding N2 - A long list of criteria determining the hot cracking susceptibility already exists. A main influence on solidification cracking can result from the design of the welded construction, i.e. from the influence of external loads. Using the Controlled Tensile Weldability (CTW) test, an external load hot cracking test, the influence of constant pre-load and different extension rates on the solidification cracking behavior of GTA (Gas Tungsten Arc) welds in an austenitic (AISI 309) and a ferritic (AISI 441) steel were investigated. Compared to specimens welded allowing free shrinkage and welded with an applied constant tensile pre-load, the specimens welded during the application of increasing tensile load show solidification cracks. In the weld seams, a characteristic angle α between the predominantly columnar grains and the fusion line can be observed. Specimens showing solidification cracks show a significantly larger angle α compared to the crack-free specimens. Based on these observations, the characteristic angle α is proposed as a new hot cracking criterion. KW - Hot cracking KW - External load test KW - Component design KW - Crack criterion KW - Grain growth PY - 2017 DO - https://doi.org/10.1016/j.jmatprotec.2016.08.013 VL - 239 SP - 172 EP - 177 PB - Elsevier AN - OPUS4-37278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hilgenberg, Kai A1 - Rethmeier, Michael A1 - Steinhoff, K. T1 - Surface structuring by pulsed laser implantation N2 - Micrometric surface topologies are required for a wide range of technical applications. While lowered surface features have been used for many years to improve the tribological behavior of contacting surfaces, there are also other fields of application, where the potential of elevated surface features is known, e. g. for metal forming tools. However, the demand for a high wear resistance of these structures often inhibits an industrial application. A solution is offered by structuring techniques that use additional material. A promising approach is the localized dispersing of hard ceramic particles by pulsed laser radiation, the so-called laser implantation. This paper describes the potential to adjust the geometry as well as the mechanical properties of laser implanted surfaces by means of microstructural and topological investigations. Afterwards, results of a wear test are given and different applications for this structuring technique are discussed. It can be shown that dome-shaped or ring-shaped structures on a micrometric scale can be produced with high hardness and wear resistance. KW - Laser implantation KW - Surface structuring PY - 2017 DO - https://doi.org/10.4028/www.scientific.net/MSF.879.750 SN - 0255-5476 SN - 1662-9752 VL - 879 SP - 750 EP - 755 PB - Trans Tech Publications AN - OPUS4-38263 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ward, H. A1 - Burger, M. A1 - Chang, Y.-J. A1 - Fürstmann, P. A1 - Neugebauer, S. A1 - Radebach, A. A1 - Sproesser, G. A1 - Pittner, Andreas A1 - Rethmeier, Michael A1 - Uhlmann, E. A1 - Steckel, J. Ch. T1 - Assessing carbon dioxide emission reduction potentials of improved manufacturing processes using multiregional input output frameworks N2 - Evaluating innovative process technologies has become highly important within the last decades. As standard tools different Life Cycle Assessment methods have been established, which are continuously improved. While those are designed for evaluating single processes they run into difficulties when it comes to assessing environmental impacts of process innovations at macroeconomic level. In this paper we develop a multi-step evaluation framework building on multi regional inputeoutput data that allows estimating macroeconomic impacts of new process technologies, considering the network characteristics of the global economy. Our procedure is as follows: i) we measure differences in material usage of process alternatives, ii) we identify where the standard processes are located within economic networks and virtually replace those by innovative process technologies, iii) we account for changes within economic systems and evaluate impacts on emissions. Within this paper we exemplarily apply the methodology to two recently developed innovative technologies: longitudinal large diameter steel pipe welding and turning of high-temperature resistant materials. While we find the macroeconomic impacts of very specific process innovations to be small, its conclusions can significantly differ from traditional process based approaches. Furthermore, information gained from the methodology provides relevant additional insights for decision makers extending the picture gained from traditional process life cycle assessment. KW - Economic wide technology replacement KW - Sustainability assessment KW - Multi-regional inputeoutput data KW - Life-cycle assessment KW - Greenhouse gas mitigation KW - Process innovations PY - 2017 DO - https://doi.org/10.1016/j.jclepro.2016.02.062 SN - 0959-6526 SN - 1879-1786 VL - 163 SP - 154 EP - 165 PB - Elsevier Ltd. AN - OPUS4-41356 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neubert, S. A1 - Pittner, Andreas A1 - Rethmeier, Michael T1 - Influence of non-uniform martensitic transformation on residual stresses and distortion of GMA-welding N2 - A combined experimental and numerical approach is applied for a numerical analysis of the non-uniform martensitic transformation kinetic on welding residual stresses and distortion of a single pass weld. The (γ → α)-transformation kinetic within the weld pool region is governed by a non-uniform distribution of the elements chromium and nickel. The single-pass weld was performed by use of the low-alloyed high-strength steel S960QL with the high-alloyed high-strength filler wire CN 13/4-IG®. A thermo-mechanical FE model of the welding process was experimentally validated against temperature field, solid phase distribution, transformation behaviour, X-Ray stress measurements and transient optical distortion measurements. The experimentally determined and calculated weld residual stresses and transient distortion are in good agreement. It can be shown that the change on the (γ → α)-transformation kinetic driven by the inhomogeneous distribution of the chemical contents causes a strong influence on the weld residual stresses within the volume of the weld pool, which could promote crack propagation within the solidified weld pool by use of high-alloyed filler materials. Furthermore, a significant influence on the development of the transient welding distortion is visible. This influence should be respected during numerically calculation of welding distortion in case of multi-pass welding using interpass temperatures and high-alloyed filler materials. KW - Welding residual stresses KW - FEA KW - Welding simulation KW - Dissimilar welding KW - Transformable steels PY - 2017 DO - https://doi.org/10.1016/j.jcsr.2016.08.020 SN - 0143-974X SN - 1873-5983 VL - 128 SP - 193 EP - 200 PB - Elsevier Ltd. AN - OPUS4-37276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gook, S. A1 - Gumenyuk, Andrey A1 - Rethmeier, Michael T1 - Hybrid laser arc welding of high grade X80 and X120 pipeline steels N2 - The aim of the present work was to investigate the possibilities of hybrid laser arc welding regarding reliable production of longitudinal welds of high strength pipe steels X80 and X120 and to evaluate achievable mechanical properties of laser hybrid welds. The study focused on weld toughness examination in low temperature range up to -60 °C. SЮТЭКЛХО ПТХХОЫ ЦКЭОЫТКХЬ were identified in the context of this task. It could be shown that metal cored electrodes guaranteed sufficient Charpy impact toughness at low temperature for both investigated materials. Modern arc welding technologies such as modified pulsed spray arc were used to promote deeper Penetration of the filler material into the narrow laser welding gap. Edge preparation with a 14 mm deep root face was considered as optimum, because no penetration of the filler material could be detected beyond this depth limit and therefore any metallurgical influences on the weld metal properties through the welding wire could be excluded. KW - High strength steel KW - Longitudinal weld KW - Modified spray arc KW - Pipeline KW - Hybrid laser arc welding PY - 2017 SN - 2499-9733 SN - 2305-414Х VL - 1 IS - 22 SP - 21 EP - 35 AN - OPUS4-44343 LA - rus AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Marko, A. A1 - Graf, B. A1 - Gook, S. A1 - Rethmeier, Michael T1 - Application of D-optimum experimental designs in consideration of restrictions for laser metal deposition N2 - The process of laser metal deposition can be applied in many ways. Mostly, it is relevant to coating, for repair welding and for additive manufacturing. To increase the effectiveness and the productiveness, a good process understanding is necessary. Statistical test planning is effectual and often used for this purpose. For financial and temporal reasons, a restriction of the test space is reasonable. In this case, it is recommended to use a D-optimal experimental design which is practically applied to extend existing test plans or if process Limits are known. This paper investigates the applicability of a D-optimum experimental design for the laser metal deposition. The results are compared to the current results of a full factorial test plan. Known restrictions are used for the limitation of the test space. Ti6Al4 is utilized as Substrate material and powder. Comparable results of the D-optimal experimental design and of the full factorial test plan can be demonstrated. However, 80 % of time can be saved by the experimental procedure. For this reason, the application of D-optimal experimental design for laser metal deposition is recommend. KW - Design of experiments KW - Repair welding KW - Additive manufacturing KW - Cladding parameter KW - Laser metal deposition KW - Laser cladding PY - 2017 SN - 2499-9733 SN - 2305-414Х VL - 3 IS - 24 SP - 46 EP - 60 AN - OPUS4-44344 LA - rus AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rethmeier, Michael A1 - Finkbeiner, M. T1 - Licht ist grüner als Strom N2 - Laserschweißen gegen Widerstandspunktschweißen: Die Die Entscheidung fällt am Flansch. Beide Verfahren sind sehr schnell und hoch automatisierbar. KW - Laserschweißen KW - Widerstandspunktschweißen PY - 2017 VL - 24 SP - 6 EP - 6 AN - OPUS4-40413 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bakir, Nasim A1 - Gumenyuk, Andrey A1 - Rethmeier, Michael T1 - Investigation of solidification cracking susceptibility during laser beam welding using an in-situ observation technique N2 - Using the novel optical measurement technique together with the optical flow algorithm, a twodimensional deformation analysis during welding has been conducted. This technique provides for the first time a measurement of the strain field locally in the immediate vicinity of the assumed solidification front. The described procedure of the opticalmeasurement allows to determine the real martial-dependent values of critical strain and strain rate characterising transition to the hot cracking during laser welding processes. The local critical strain that obtained in the assumed solidification showed that the local critical strain decreases as the strain rate increases. Moreover, this phenomenon has also been shown with results from the CTW-test, since the global strain decreases with an increase in the external strain rate. KW - Novel optical measurement KW - Local critical strain KW - Solidification cracking KW - Laser beam Welding PY - 2017 DO - https://doi.org/10.1080/13621718.2017.1367550 SN - 1362-1718 SP - 1 EP - 7 PB - Taylor & Francis AN - OPUS4-42918 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mushtaq, S. A1 - Steers, E.B.M. A1 - Barnhart, D. A1 - Churchill, G. A1 - Kasik, M. A1 - Richter, Silke A1 - Pfeifer, Jens A1 - Putyera, K. T1 - The production of doubly charged sample ions by “charge transfer and ionization” (CTI) in analytical GD-MS N2 - Normally, in analytical GD-MS, the doubly charged metallic ion signals from the sample are several orders of magnitude less than the corresponding singly charged signals. However, we have observed that using a neon plasma, the M++ signals of some elements, which have double ionization energies close to the first ionization energy of neon, are of the same order as the M+ signal. Doubly charged ions may be produced directly in the discharge cell by electron ionization (EI), and also by two electron Penning ionization (TEP), but these processes cannot explain the above effect. In this paper, we suggest that an additional process named as ‘Charge Transfer and Ionization’ (CTI) produces such ions either in their ionic ground state or in an excited state. To confirm that this process is typical of the discharges used in GD-MS and not an artefact of any particular form of cell and ion extraction system, we have carried out comprehensive experimental measurements using three different GD-MS instruments, viz., Nu Astrum, VG9000 and ELEMENT GD and our results provide clear evidence for CTI. This is the first time the process has been identified as an ionization process in analytical GD-MS. CTI must be differentiated from Asymmetric Charge Transfer (ACT), which is a “selective” process and requires a close energy match (e.g. ΔE < 0.5 eV for a strong effect). On the other hand, CTI is “non-selective” in the sense that a close energy match is not required (e.g. a strong effect is observed with ΔE ∼ 2 eV), although the process only occurs for a limited number of elements, depending on the plasma gas used and the total energy required to doubly ionize the metallic atom. KW - Titanium KW - Glow discharge processes KW - Doubly charged ions KW - The charge transfer and ionization process (CTI) KW - Krypton KW - Neon PY - 2017 DO - https://doi.org/10.1039/C6JA00415F SN - 0267-9477 SN - 1364-5544 VL - 32 IS - 9 SP - 1721 EP - 1729 PB - Royal Society of Chemistry AN - OPUS4-41108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wachtendorf, Volker A1 - Kalbe, Ute A1 - Krüger, O. A1 - Bandow, Nicole ED - Brown, R. ED - Gedde, U.W. ED - Hedenqvist, M.S. T1 - Influence of weathering on the leaching behaviour of zinc and PAH from synthetic sports surfaces N2 - Synthetic materials used for outdoor sports grounds consist of a mix of inorganic, organic and polymeric compounds that show ageing due to weathering and a complex leaching behaviour by percolation of rainwater, which can limit its lifetime. Additionally, weathering exposure induces degradation processes in the polymers, which leads to the formation of new surfaces allowing water to access additional reservoirs of leachable compounds. A laboratory test comprising artificial weathering, ozonisation and subsequent leaching was developed to investigate this behaviour in a reproducible and controllable way. The experiments showed a general decline of Zn, polycyclic aromatic hydrocarbons (PAH) and total organic carbon (TOC) concentrations after an initial increase. Within this general trend, the course of concentration over exposure duration is very specific for individual sample materials and the analyte under investigation. The results indicate that weathering and degradation behaviour cannot be predicted from initial material conditions. Thus, weathering experiments are recommended to fill this gap of knowledge. KW - Athletic tracks KW - Artificial turf KW - Ageing KW - Artificial weathering KW - Polymer degradation KW - Rubber granules KW - Leaching KW - Contamination PY - 2017 DO - https://doi.org/10.1016/j.polymertesting.2017.09.021 SN - 0142-9418 SN - 1873-2348 VL - 63 IS - October SP - 621 EP - 631 PB - Elsevier Ltd. CY - Amsterdam, The Netherlands AN - OPUS4-42205 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friedrich, Jörg A1 - Altmann, Korinna A1 - Wettmarshausen, Sascha A1 - Hidde, Gundula T1 - Coating of carbon fibers with adhesion-promoting thin polymer layers using plasma polymerization or electrospray ionization technique—A comparison N2 - Plasma polymers and electrospray-ionization (ESI) polymer layers are compared for most efficient adhesion promotion in carbon fiber-epoxy resin composites. The ultra-thin ESI layers (2–30 nm) of commercial poly(acrylic acid) and poly-(hydroxyethylmethacrylate) produce an significant increase of adhesion measured by single-fiber pull out tests. However, plasma Treatment has also advantages, such as simultaneous activation of the fiber substrate. Chemical structure and composition are rather far from the regular structure of commercial polymers as deposited by ESI processing. KW - Plasma polymers KW - Electrospray ionization polymers KW - Poly(acrylic acid) KW - Poly- (hydroxyethylmethacrylate) PY - 2017 DO - https://doi.org/10.1002/ppap.201600074 SN - 1612-8869 SN - 1612-8850 VL - 14 IS - 3 SP - e1600074-1 EP - 14 AN - OPUS4-40510 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Launert, B. A1 - Szczerba, R. A1 - Gajewski, M. A1 - Rhode, Michael A1 - Pasternak, H. A1 - Gizejowski, M. T1 - The buckling resistance of welded plate girders taking into account the influence of post-welding imperfections - Part 1: Parameter study N2 - Welding is the most important joining technique and offers the advantage of customizable plate thicknesses. On the other hand, welding causes residual stresses and deformations influencing the load carrying capacity. Their consideration in the design requires simple and fast models. Though welding simulation has contributed to accurately access to these values nowadays, their application to large components remains still in a less practicable range. Nevertheless, many studies emphasized the need to make corrections in recently available simplified models. Especially the influence of residual stresses seems somewhat overestimated in many cases if comparing conventional structural steel S355 and high-strength steel S690. In the age of computer-aided design, an improved procedure to implement weld-inducted imperfections appears overdue. This will be presented in two parts. The first part illustrates the potential influence of post-welding imperfections exemplified for weak axis buckling in comparison with the general method in accordance with Eurocode 3. Residual stresses and initial crookedness were varied systematically in order to produce a scatter band of capacities. An approach to characterize the borders of these imperfections was untertaken before that. The excessive scattering of reduction factors for the load bearing capacity demonstrates the importance of these variables. Results were finally evaluated against advanced simulation models which will be further detailed in part two of this contribution. KW - Welded Plate Girders KW - Stability KW - Post-welding Imperfections KW - Residual Stresses KW - Parameter Study PY - 2017 DO - https://doi.org/10.3139/120.110964 SN - 0025-5300 SN - 2195-8572 VL - 59 IS - 1 SP - 47 EP - 56 PB - Carl Hanser Verlag CY - München AN - OPUS4-38922 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scheuerlein, C. A1 - Uhlemann, Patrick A1 - Finn, Monika A1 - Lackner, F. A1 - Savary, F. T1 - Mechanical properties of the HL-LHC 11 T Nb3Sn magnet constituent materials N2 - A test campaign was launched to determine the mechanical properties of the High Luminosity-Large HadronCollider (HL-LHC) 11 T Nb3Sn magnet components. The results can be used to accurately represent the mechanical properties in finite elementmodels that predict the stress and strain distribution in these magnets. Particular attention is paid to anisotropic mechanical behavior of the different magnet materials. Static and dynamic test methods have been applied for determining elastic materials’ behavior, and highly accurate Young’s moduli are obtained with the nondestructive dynamic methods resonance and impulse excitation at ambient temperature and during in situ heat cycles. KW - Superconducting magnets KW - Young’s modulus KW - Resonance testing KW - Stress-strain behavior PY - 2017 DO - https://doi.org/10.1109/TASC.2016.2638046 SN - 1051-8223 SN - 1558-2515 VL - 27 IS - 4 SP - 1 EP - 7 PB - IEEE AN - OPUS4-39219 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vollert, J. A1 - Dixneit, Jonny A1 - Kromm, Arne A1 - Buslaps, Th. A1 - Kannengießer, Thomas T1 - In situ EDXRD study of MAG-welding using LTT weld filler materials under structural restraint N2 - Welding using low transformation temperature (LTT) filler materials is an innovative approach to mitigate detrimental welding residual stresses without cost-intensive post weldtreatments. Due to the local Generation of compressive residual stresses in the weld line by means of a delayed martensite transformation a significant enhancement of the cold cracking resistance of highly stressed welded components can be expected. For the effective usage of These materials a deeper understanding of the microstructural evolution inside the weld material is necessary to determine the complex processes that cause the residual stress formation during welding. Solid-state phase transformation kinetics and the evolution of strain in LTT weld filler materials are monitored in-situ at the instrument ID15A at the ESRF in Grenoble, France. The transferability to real components is implemented by using a realistic MAG welding process under consideration of structural restraint. During welding of multilayer joints, the phase Transformation and phase specific strain evolution of each individual layer is investigated in transmission geometry by means of energy-dispersive X-ray diffraction EDXRD using high energy synchrotron Radiation with a counting rate of 2.5 Hz. The measurement results of a 10% Cr / 10% Ni LTT weld filler are compared to data monitored for the conventional weld filler material G89. The in-situ data clearly indicate a strong effect on the local strain evolution and the formation of compressive strain. This results from the restraint volume expansion during the postponed austenite to martensite transformation of the LTT weld filler, which counteracts the thermal shrinkage. In contrast, for the conventional weld filler material the thermal contraction strains lead to tensile residual strain during welding. Furthermore, the results of in-situ observation during welding Show that the transformation kinetic is dependent on the welding sequence. KW - High energy synchrotron diffraction KW - Low transformation temperature KW - Weld filler KW - Residual stress KW - Welding PY - 2017 DO - https://doi.org/10.4028/www.scientific.net/MSF.905.107 SN - 1662-9752 VL - 905 SP - 107 EP - 113 PB - Trans Tech Publications CY - Switzerland AN - OPUS4-41806 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epping, Ruben A1 - Panne, Ulrich A1 - Falkenhagen, Jana T1 - Critical conditions for liquid chromatography of statistical copolymers: Functionality type and composition distribution characterization by UP-LCCC/ESI-MS N2 - Statistical ethylene oxide (EO) and propylene oxide (PO) copolymers of different monomer compositions and different average molar masses additionally containing two kinds of end groups (FTD) were investigated by ultra high pressure liquid chromatography under critical conditions (UP-LCCC) combined with electrospray ionization time-of flight mass spectrometry (ESI-TOFMS). Theoretical predictions of the existence of a critical adsorption point (CPA) for statistical copolymers with a given chemical and sequence distribution1 could be studied and confirmed. A fundamentally new approach to determine these critical conditions in a copolymer, alongside the inevitable chemical composition distribution (CCD), with mass spectrometric detection, is described. The shift of the critical eluent composition with the monomer composition of the polymers was determined. Due to the broad molar mass distribution (MMD) and the presumed existence of different end group functionalities as well as monomer sequence distribution (MSD), Gradient separation only by CCD was not possible. Therefore, isocratic separation conditions at the CPA of definite CCD fractions were developed. Although the various present distributions partly superimposed the separation process, the goal of separation by end group functionality was still achieved on the basis of the additional dimension of ESI-TOF-MS. The existence of HO-H besides the desired allylO-H end group functionalities was confirmed and their amount estimated. Furthermore, indications for a MSD were found by UPLC/MS/MS measurements. This approach offers for the first time the possibility to obtain a fingerprint of a broad distributed statistical copolymer including MMD, FTD, CCD, and MSD. KW - Polymer KW - Liquid chromatography at critical conditions KW - ESI-TOF-MS PY - 2017 DO - https://doi.org/10.1021/acs.analchem.6b04064 SN - 0003-2700 SN - 1520-6882 VL - 89 IS - 3 SP - 1778 EP - 1786 AN - OPUS4-39240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Greiser, Sebastian A1 - Benemann, Sigrid A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Knowing When To Stop-Trapping Metastable Polymorphs in Mechanochemical Reactions N2 - The cocrystal formation of pyrazinamide (PZA) with malonic acid (MA) was studied in situ. The mechanochemical reaction proceeds via conversion of a crystalline intermediate (PZA:MA II) into the thermodynamically more stable form (PZA:MA I) upon further grinding. The information derived from in situ powder X-ray diffraction (PXRD) enabled the isolation of this new metastable polymorph. On the basis of the PXRD data, the crystal structure of the 1:1 cocrystal PZA:MA II was solved. The polymorphs were further characterized and compared by Raman spectroscopy, solid-state NMR spectroscopy, differential thermal analysis/thermogravimetric analysis, and scanning electron microscopy. Our study demonstrates how monitoring mechanochemical reactions by in situ PXRD can direct the discovery and isolation of even short-lived intermediates not yet accessed by conventional methods. KW - Mechanochemistry KW - Polymorphs KW - Metastable KW - In situ PXRD KW - Cocrystal KW - Pyrazinamide PY - 2017 DO - https://doi.org/10.1021/acs.cgd.6b01572 SN - 1528-7483 SN - 1528-7505 VL - 17 IS - 3 SP - 1190 EP - 1196 AN - OPUS4-39420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dixneit, Jonny A1 - Kromm, Arne A1 - Boin, M. A1 - Wimpory, Robert A1 - Kannengießer, Thomas A1 - Gibmeier, J. A1 - Schröpfer, Dirk T1 - Residual stresses of LTT welds in large-scale components N2 - Residual stresses of welds become more and more important influencing cold cracking as well as the fatigue life of welded components. Low transformation temperature (LTT) filler materials offer the opportunity to alter the residual stresses already during the welding process by means of ad- justed martensite phase transformation temperature (MS). In the current paper, welding residual stresses are studied putting the focus on MS while joining heavy steel sections with a thickness of 20 and 25 mm, respectively. The residual stress state was determined at the top surface using X-ray diffraction as well as in the bulk by neutron diffraction. The results com- pare the residual stresses present in a conventional weld and LTT welds when multi-pass welding of large-scale compo- nents was applied. Repeated phase transformation in the case of the LTT weld is more vital for the residual stresses present in the real-life-like joints. This accounts for the top surface in longitudinal direction but is most pronounced for the bulk of the welds. Detrimental tensile residual stresses are mainly re- duced in the bulk in comparison to a conventional filler wire even in multi-pass welds of thick steel sections. T2 - IIW AA 2016 CY - Melbourne, Australia DA - 10.07.2016 KW - LTT KW - Welding residual stress KW - Phase transformation KW - Interpass temperature PY - 2017 DO - https://doi.org/10.1007/s40194-017-0502-5 SN - 0043-2288 SN - 1878-6669 VL - 61 IS - 6 SP - 1089 EP - 1097 PB - Springer CY - Heidelberg AN - OPUS4-41169 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geißler, Daniel A1 - Würth, Christian A1 - Wolter, C. A1 - Weller, H. A1 - Resch-Genger, Ute T1 - Excitation wavelength dependence of the photoluminescence quantum yield and decay behavior of CdSe/CdS quantum dot/quantum rods with different aspect ratios N2 - The excitation wavelength (lexc) dependence of the photoluminescence (PL) quantum yield (FPL) and decay behavior (tPL) of a series of CdSe/CdS quantum dot/Quantum rods (QDQRs), consisting of the same spherical CdSe core and rod-shaped CdS shells, with aspect ratios ranging from 2 to 20 was characterized. lexc between 400–565 nm were chosen to cover the first excitonic absorption band of the CdSe core material, the onset of absorption of the CDs shell, and the region of predominant shell absorption. A strong lexc dependence of relative and absolutely measured FPL and tPL was found particularly for the longer QDQRs with higher aspect ratios. This is attributed to combined contributions from a length-dependent shell-to-core exciton localization efficiency, an increasing number of defect states within the shell for the longest QDQRs, and probably also the presence of absorbing, yet non-emitting shell material. Although the FPL values of the QDQRs decrease at shorter wavelength, the extremely high extinction coefficients introduced by the shell outweigh this effect, leading to significantly higher brightness values at wavelengths below the absorption onset of the CdS Shell compared with direct excitation of the CdSe cores. Moreover, our results present also an interesting example for the comparability of absolutely measured FPL using an integrating sphere setup and FPL values measured relative to common FPL standards, and underline the Need for a correction for particle scattering for QDQRs with high aspect ratios. KW - Quantum dot KW - Quantum rod KW - Quantum yield KW - Integrating sphere KW - Decay time PY - 2017 DO - https://doi.org/10.1039/C7CP02142A SN - 1463-9076 SN - 1463-9084 VL - 19 IS - 19 SP - 12509 EP - 12516 PB - Royal Society of Chemistry (RSC) AN - OPUS4-40814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Würth, Christian A1 - Kaiser, Martin A1 - Wilhelm, Stefan A1 - Grauel, Bettina A1 - Hirsch, Th. A1 - Resch-Genger, Ute T1 - Excitation power dependent population pathways and absolute quantum yields of upconversion nanoparticles in different solvents N2 - The rational design of brighter upconversion nanoparticles (UCNPs) requires a better understanding of the radiationless deactivation pathways in these materials. Here, we demonstrate the potential of excitation power density (P)-dependent studies of upconversion (UC) luminescence intensities, slope factors, and absolute quantum yields (ΦUC) of popular β-NaYF4:20% Yb3+,2% Er3+ UCNPs of different surface chemistries in organic solvents, D2O, and water as a tool to gain deeper insight into the UC mechanism including population and deactivation pathways particularly of the red emission. Our measurements, covering a P regime of three orders of magnitude, reveal a strong difference of the P-dependence of the ratio of the green and red luminescence bands (Ig/r) in water and organic solvents and P-dependent population pathways of the different emissive energy levels of Er3+. In summary, we provide experimental evidence for three photon processes in UCNPs, particularly for the red emission. Moreover, we demonstrate changes in the excited population dynamics via bi- and triphotonic processes dependent on the environment, surface chemistry, and P, and validate our findings theoretically KW - Upconverion KW - Quantum Yield KW - Photo physics PY - 2017 UR - http://pubs.rsc.org/en/content/articlepdf/2017/nr/c7nr00092h DO - https://doi.org/10.1039/c7nr00092h SN - 2040-3364 SN - 2040-3372 VL - 9 IS - 12 SP - 4283 EP - 4294 PB - The Royal Society of Chemistry AN - OPUS4-39849 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radunz, Sebastian A1 - Tschiche, Harald Rune A1 - Moldenhauer, Daniel A1 - Resch-Genger, Ute T1 - Broad range ON/OFF pH sensors based on pKa tunable fluorescent BODIPYs N2 - A set of highly fluorescent, pH-responsive boron dipyrromethene dyes covering the pH range of 5-12 is presented for broad range pH measurements in mixed aqueous-organic median and polymer matrices. Readout in the intensity Domain with low cost and miniaturized Instrumentation utilizes reversible protonation induced switching ON of their initially completely quenched flourescence mediated by photoinduced electron Transfer. All dyes, rationally designed to reveal closely matching Absorption and Emission properties, are accessible via facile two-step reactions in Overall yields of up to 20%. By modifying the Substitution pattern of the meso-Aryl substiuent, the pKa values could be fine-tuned from 6 to 11. Integration of these molecules into polymeric films by a simple mixing procedure yielded reversible and longterm stable pH sensors for naked eye detection. KW - Fluorescence KW - Sensor KW - PH KW - Dye KW - BODIPY KW - Synthesis KW - Quantification KW - Film KW - Quantum yield KW - Lifetime KW - PET PY - 2017 DO - https://doi.org/10.1016/j.snb.2017.05.080 SN - 0925-4005 VL - 251 SP - 490 EP - 494 PB - Elsevier AN - OPUS4-41782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Pilch, A. A1 - Würth, Christian A1 - Kaiser, Martin A1 - Wawrzynczyk, D. A1 - Kurnatowska, M. A1 - Arabasz, S. A1 - Prorok, K. A1 - Samoc, M. A1 - Strek, W. A1 - Bednarkiewicz, A. T1 - Shaping luminescent properties of Yb3+ and Ho3+ co-doped upconverting core-shell ß-NaYF4 nanoparticles by dopant distribution and spacing N2 - At the core of luminescence color and lifetime Tuning of rare earth doped upconverting nanoparticles (UCNPs), is the understanding of the Impact of the particle architecture for commonly used sensitizer (S) and activator (A) Ions. In this respect, a series of core@Shell NaYF4 UCNPs doped with Yb3+ and Ho3+ ions are presented here, where the same dopant concentrations are distributed in different particle architectures following the scheme: YbHo core and YbHo@..., ...@YbHo, Yb@Ho, Ho@Yb, YbHo@Yb, and Yb@YbHo core-Shell NPs. As refealed by quantitative steady-state and time-resolved luminescence studies, the relative spatial Distribution of the A and S ions in the UCNPs and their protection from surface quenching has a critical Impact on ther luminescence characteristics. Although the increased amount of Yb3+ Ions boosts UCNP Performance by amplifying the Absorption, the Yb3+ ions can also efficiently dissipate the energy stored in the material through energy Migration to the surface, thereby reducing the Overall energy Transfer Efficiency to the activator ions. The results provide yet another proof that UC Phosphor chemistry combined with materials Engineering through intentional core@shell structures may help to fine-tune the luminescence Features of UCNPs for their specific future applications in biosensing, bioimaging, photovoltaics, and Display technologies. KW - Fluorescence KW - Upconversion KW - NIR KW - Nonlinear KW - Nanoparticle KW - Surface chemistry KW - Quantum yield KW - Liftetime KW - Nanocrystal KW - Lanthanide KW - Ho(III) KW - Yb(III) KW - Mechanism KW - Absolute flourescence KW - Excitation power density dependence PY - 2017 DO - https://doi.org/10.1002/smll.201701635 SN - 1613-6810 VL - 13 IS - 47 SP - 1701635, 1 EP - 13 PB - WILEY-VCH Verlag GmbH & co. KGaA CY - Weinheim AN - OPUS4-43629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauli, Jutta A1 - Hoffmann, Katrin A1 - Würth, Christian A1 - Behnke, Thomas A1 - Resch-Genger, Ute T1 - Standardization of fluorescence measurements in the UV/vis/NIR/IR N2 - Photoluminescence techniques are amongst the most widely used Tools in the life sciences, with new and exciting applications in medical diagnostics and molecular Imaging continuously emerging. Advantages include their comparative ease of use, unique sensitivity, non-invasive character, and potential for Multiplexing, remote sensing, and miniaturization. General drawbacks are, however, signals, that contain unwanted wavelength- and polarization contributions from Instrument-dependent effects, which are also time-dependent due to aging of Instrument-components, and difficulties to measure absolute flourescence entensities. Moreover, scattering Systems require Special measurement geometries and the interest in new optical Reporters with Emission > 1000 nm strategies for reliable measurements in the second diagnostic for the comparison of material Performance and the rational designg of new flourophores with improved properties. Here, we present strategies to versatile method-adaptable liquid and solid flourescence Standards for different flourescence paramters including traceable Instrument calibration procedures and the design of integrating spere setups for the absolute measurements of emission spectra and Quantum yields in the wavelength Region of 350 to 1600 nm. Examples are multi-Emitter glasses, spectral flourescence Standards, and quantum yield Standards for the UV/vis/NIR. T2 - Conference on Molecular-Guided Surgery - Molecules, Devices, and Applications III CY - San Francisco, CA, USA DA - 28.01.2017 KW - Fluorescence KW - Reference material KW - Standard KW - Calibration KW - Nanoparticle KW - Absolute flourometry KW - Integrating sphere spectroscopy KW - NIR KW - IR KW - Quantum yield standard KW - Emission standards PY - 2017 SN - 978-1-5106-0539-8 DO - https://doi.org/10.1117/12.2255728 SN - 0277-786X VL - 10049 SP - 1 PB - Proceedings of SPIE AN - OPUS4-41783 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Agudo Jácome, Leonardo A1 - Göbenli, G. A1 - Eggeler, G. ED - Göken, M. T1 - Transmission electron microscopy study of the microstructural evolution during high-temperature and low-stress (011) [01-1] shear creep deformation of the superalloy single crystal LEK 94 N2 - The present work describes the shear creep behavior of the superalloy LEK 94 at temperatures between 980 and 1050 °C and shear stresses between 50 and 140 MPa for loading on the macroscopic crystallographic shear system (MCSS) (011)[01-1]. The strain rate versus strain curves show short primary and extended secondary creep regimes. We find an apparent activation energy for creep of Qapp = 466 kJ/mol and a Norton-law stress exponent of n = 6. With scanning transmission electron microscopy, we characterize three material states that differ in temperature, applied stress, and accumulated strain/time. Rafting develops perpendicular to the maximum principal stress direction, gamma channels fill with dislocations, superdislocations cut gamma' particles, and dislocation networks form at gamma/gamma' interfaces. Our findings are in agreement with previous results for high-temperature and low-stress [001] and [110] tensile creep testing, and for shear creep testing of the superalloys CMSX-4 and CMSX-6 on the MCSSs (111)[01-1] and (001)[100]. The parameters that characterize the evolving gamma/gamma' microstructure and the evolving dislocation substructures depend on creep temperature, stress, strain, and time. KW - Dislocations KW - Microstructure KW - Scanning transmission electron microscopy (STEM) KW - Creep KW - Shear test PY - 2017 DO - https://doi.org/10.1557/jmr.2017.336 SN - 0884-2914 SN - 2044-5326 VL - 32 IS - 24 SP - 4491 EP - 4502 PB - Cambridge University Press CY - Cambrigde AN - OPUS4-43756 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute ED - Otto, S. ED - Scholz, Norman ED - Behnke, Thomas ED - Heinze, K. T1 - Thermo-Chromium: A Contactless Optical Molecular Thermometer N2 - The unparalleled excited-state potential-energy landscape of the chromium(III)-based dye [1]3+ ([Cr(ddpd)2]3+; ddpd=N,N’-dimethyl-N,N’-dipyridin-2-ylpyridin-2,6-diamine) enables a strong dual emission in the near infrared region. The temperature dependence of this dual emission allows the use of [1]3+ as an unprecedented molecular ratiometric thermometer in the 210–373 K temperature range in organic and in aqueous media. Incorporation of [1]3+ in biocompatible nanocarriers, such as 100 nm-sized polystyrene nanoparticles and solutol micelles, provides nanodimensional thermometers operating under physiological conditions. KW - Temperature KW - Sensor KW - Dual emission KW - Fluorescence KW - Cr complex KW - Nano KW - Particle KW - Micelle KW - Probe KW - Environment PY - 2017 DO - https://doi.org/10.1002/chem.201701726 SN - 0947-6539 VL - 23 IS - 50 SP - 12131 EP - 12135 PB - Wiley-VCH AN - OPUS4-42539 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 - Resch-Genger, Ute A1 - Gorris, H.H. T1 - Perspectives and challenges of photon-upconversion nanoparticles - Part I: routes to brighter particles and quantitative spectroscopic studies N2 - Lanthanide-doped photon-upconversion nanoparticles (UCNPs) have been the Focus of many Research activities in materials and life sciences in the last 15 years because of their potential to convert light between different spectral regions and their unique photophysical properties. To fully exploit the application potential of These facinating nanomaterials, a number of challenges have to be overcome, such as the low brightness, particularly of small UCNPs, and the reliable quantification of the excitation-power-density-dependent upconversion luminescence. In this series of critical Reviews, recent developments in the design, Synthesis, optical-spectroscopic characterization, and application of UCNPs are presented with Special Focus on bioanalysis and the life sciences. Here we guide the reader from the Synthesis of UCNPs to different concepts to enhance their luminescence, including the required optical-spectroscopic assessment to quantify material Performance; surface modification strategies and bioanalytical applications as well as selected examples of the use of UCNPs as reporters in different Assay formats are addressed in part II. Future Trends and challenges in the field of upconversion are discussed with Special emphasis on UCNP Synthesis and material characterization, particularly quantitative luminescence studies. KW - Fluorescence KW - Lanthanide KW - Upconversion KW - Brightness KW - Quantification KW - Nanoparticle KW - Absolute fluorometry KW - NIR KW - IR KW - Quantum yield PY - 2017 DO - https://doi.org/10.1007/s00216-017-0499-z SN - 1618-2650 SN - 1618-2642 VL - 409 IS - 25 SP - 5855 EP - 5874 PB - Springer AN - OPUS4-41665 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute ED - Mousavi, M. ED - Thomasson, B. ED - Li, M. ED - Kraft, Marco ED - Würth, Christian ED - Andersson-Engels, S. T1 - Beam-profile-compensated quantum yield measurements of upconverting nanoparticles N2 - The quantum yield is a critically important parameter in the development of lanthanide-based upconverting nanoparticles (UCNPs) for use as novel contrast agents in biological imaging and optical reporters in assays. The present work focuses on the influence of the beam Profile in measuring the quantum yield (f) of nonscattering dispersions of nonlinear upconverting probes, by establishing a relation between f and excitation light power density from a rate equation analysis. A resulting 60% correction in the measured f due to the beam profile utilized for excitation underlines the significance of the beam profile in such measurements, and its impact when comparing results from different Setups and groups across the world. KW - Fluorescence KW - Lanthanide KW - Upconversion KW - Brithtness KW - Quantification KW - Nanoparticle KW - Absolute fluoreometry KW - NIR KW - IR KW - Quantum yield KW - Integrating sphere spectroscopy KW - Method PY - 2017 DO - https://doi.org/10.1039/c7cp03785f SN - 1463-9076 SN - 1463-9084 VL - 19 IS - 33 SP - 22016 EP - 22022 PB - Royal Society of Chemistry AN - OPUS4-42583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Huang, K. A1 - Liu, H. A1 - Kraft, Marco A1 - Shikha, S. A1 - Zheng, X. A1 - Agren, H. A1 - Würth, Christian A1 - Resch-Genger, Ute A1 - Zhang, Y. T1 - A protected excitation-energy reservoir for efficient upconversion luminescence N2 - Lanthanide-doped upconversion nanoparticles (UCNPs) are of great interest for biomedical applications. Currently, the applicability of UCNP bionanotechnology is hampered by the generally low luminescence intensity of UCNPs and inefficient energy Transfer from UCNPs to surface-bound chromophores used e.g. for photodynamic therapy or analyte sensing. In this work, we address the low-Efficiency issue by developing versatile core-Shell nanostructures, where high-concentration sensitizers and activators are confined in the core and Shell Region of representative hexagonal NaYF2:Yb,Er UCNPs. After Doping concentration optimization, the sensitizer-rich core is able to harvest/accumulate more excitation energy and generate almost one order of Magnitude higher luminescence intesity than conventional homogeneously doped nanostructures. At the same time, the activator Ions located in the Shell enable a ~6 times more efficient resonant energy Transfer from UCNPs to surface-bound acceptor dye molecules due to the short distance between donor-acceptor pairs. Our work provides new insights into the rational design of UCNPs and will greatly encrease the General applicability of upconversion nanotechnologies. KW - Fluorescence KW - Lanthanide KW - Upconversion KW - Brightness KW - Quantification KW - Nanoparticle KW - Absolute fluorometry KW - NIR KW - IR KW - Quantum yield KW - Integrating sphere spectroscopy KW - Method KW - Energy transfer KW - Shell KW - Particle architecture PY - 2017 DO - https://doi.org/10.1039/c7nr06900f SN - 2040-3372 SN - 2040-3364 VL - 10 IS - 1 SP - 250 EP - 259 PB - The Royal Society of Chemistry AN - OPUS4-43893 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Otto, S. A1 - Moll, J. A1 - Förster, C. A1 - Geißler, Daniel A1 - Wang, Cui A1 - Resch-Genger, Ute A1 - Heinze, K. T1 - Three-in-One Crystal: The Coordination Diversity of Zinc Polypyridine Complexes N2 - The syntheses, structures, and photophysical properties of two new zinc(II) complexes bearing the tridentate N,N′-dimethyl-N,N′-dipyridin-2-ylpyridine-2,6-diamine (ddpd) ligand are presented. Structural investigations through single-crystal X-ray diffractometry, NMR spectroscopy, and density functional theory calculations revealed a diverse coordination behavior that depends on the counterion. Spectroscopic (UV/Vis and emission spectroscopy) and theoretical techniques (DFT and time-dependent DFT calculations) were employed to explore the photophysical properties of the complexes. KW - Zinc(II) complexes KW - X-ray diffractometry (XRD) KW - NMR spectroscopy KW - Density functional theory (DFT) KW - UV/Vis and emission spectroscopy PY - 2017 DO - https://doi.org/10.1002/ejic.201700948 SN - 1434-1948 SN - 1099-0682 VL - 43 SP - 5033 EP - 5040 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-43274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute ED - Martynenko, Irina ED - Baimuratov, A. S. ED - Osipova, V. A. ED - Kuznetsova, V. A. ED - Purcell-Milton, F. ED - Rukhlenko, I. D. ED - Fedorov, A. V. ED - Gun'ko, Y. K. ED - Baranov, A. V. T1 - Excitation energy dependence of the photoluminescence quantum yield of core/shell CdSe/CdS quantum dots and correlation with circular dichroism N2 - Quantum dot (QD) based nanomaterials are very promising materials for the fabrication of optoelectronic devices like solar cells, light emitting diodes (LEDs), and photodetectors as well as as reporters for chemo- and biosensing and bioimaging. Many of These applications involve the monitoring of changes in photoluminescence intensity and energy transfer processes which can strongly depend on excitation wavelength or energy. In this work, we analyzed the excitation energy dependence (EED) of the photoluminescence quantum yields (PL QYs) and decay kinetics and the circular dichroism (CD) spectra of CdSe/CdS core/shell QDs with different thicknesses of the surface passivation shell. Our results demonstrate a strong correlation between the spectral position of local maxima observed in the EED of PL QY and the zero-crossing points of the CD profiles. Theoretical analysis of the energy band structure of the QDs with effective mass approximation suggests that these structures could correspond to exciton energy levels. This underlines the potential of CD spectroscopy for the study of electronic energy structure of chiroptically active nanocrystals which reveal quantum confinement effects. KW - Fluorescence KW - Semiconductor KW - Nanoparticle KW - Surface chemistry KW - Quantum yield KW - Lifetime KW - Nanocrystal KW - Cysteine KW - Thiol KW - Ligand KW - Quantum dot KW - CdSe KW - Exciton KW - Circular dichroism KW - Theory KW - Excitation spectra KW - Excitation energy dependence PY - 2017 DO - https://doi.org/10.1021/acs.chemmater.7b04478 SN - 0897-4756 SN - 1520-5002 VL - 30 IS - 2 SP - 465 EP - 471 PB - ACS Publications AN - OPUS4-44034 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Seuthe, T. A1 - Mermillod-Blondin, A. A1 - Grehn, M. A1 - Bonse, Jörn A1 - Wondraczek, L. A1 - Eberstein, M. T1 - Structural relaxation phenomena in silicate glasses modifed by irradiation with femtosecond laser pulses N2 - Structural relaxation phenomena in binary and multicomponent lithium silicate glasses were studied upon irradiation with femtosecond (fs) laser pulses (800 nm central wavelength, 130 fs pulse duration) and subsequent thermal annealing experiments. Depending on the annealing temperature, micro-Raman spectroscopy analyses evidenced different relaxation behaviours, associated to bridging and non-bridging oxygen structures present in the glass network. The results indicate that the mobility of lithium ions is an important factor during the glass modification with fs-laser pulses. Quantitative phase contrast imaging (spatial light interference microscopy) revealed that these fs-laser induced structural modifications are closely related to local changes in the refractive index of the material. The results establish a promising strategy for tailoring fs-laser sensitivity of glasses through structural mobility. KW - Femtosecond laser KW - Silicate glasses KW - Raman spectroscopy KW - Structural relaxation KW - Refractive index PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-393045 DO - https://doi.org/10.1038/srep43815 SN - 2045-2322 VL - 7 SP - 43815, 1 EP - 43815, 10 PB - Nature Publishing Group CY - London, UK AN - OPUS4-39304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mull, Birte A1 - Möhlmann, L. A1 - Wilke, Olaf T1 - Photocatalytic degradation of toluene, butyl acetate and limonene under UV and visible light with titanium dioxide-graphene oxide as photocatalyst N2 - Photocatalysis is a promising technique to reduce volatile organic compounds indoors. Titanium dioxide (TiO2) is a frequently-used UV active photocatalyst. Because of the lack of UV light indoors, TiO2 has to be modified to get its working range shifted into the visible light spectrum. In this study, the photocatalytic degradation of toluene, butyl acetate and limonene was investigated under UV LED light and blue LED light in emission test chambers with catalysts either made of pure TiO2 or TiO2 modified with graphene oxide (GO). TiO2 coated with different GO amounts (0.75%–14%) were investigated to find an optimum ratio for the photocatalytic degradation of VOC in real indoor air concentrations. Most experiments were performed at a relative humidity of 0% in 20 L emission test chambers. Experiments at 40% relative humidity were done in a 1 m³ emission test chamber to determine potential byproducts. Degradation under UV LED light could be achieved for all three compounds with almost all tested catalyst samples up to more than 95%. Limonene had the highest degradation of the three selected volatile organic compounds under blue LED light with all investigated catalyst samples. KW - Photocatalysis KW - Emission test chamber KW - Volatile organic compound KW - VOC KW - Degradation PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-402955 DO - https://doi.org/10.3390/environments4010009 SN - 2076-3298 VL - 4 IS - 1 SP - Article 9, 1 EP - 9 PB - MDPI CY - Basel AN - OPUS4-40295 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pavlovic, Mato A1 - Zoëga, Andreas A1 - Kurz, J. H. A1 - Zanotelli, Christina T1 - Investigations to introduce the probability of detection method for ultrasonic inspection of hollow axles at Deutsche Bahn N2 - The vast experience with the automated, ultrasonic system for the inspection of hollow railway axles used by Deutsche Bahn shows that much smaller flaws are detectable than required. This results in a number of false calls. False calls lead to unnecessary demounting and disassembling of wheelsets, which generates unnecessary additional costs. In order to adjust the sensitivity of the inspection system to reduce the number of false calls without compromising safety, the capability of the system to detect cracks needs to be comprehensively established. This capability can be quantified by using probability of detection (POD) curves for the system. The multi-parameter POD model makes it possible to include several factors that influence the crack detection in the analysis. The analysis presented in this paper shows that crack position, orientation, depth extension, and shape as well as the geometry of the axle all have influence on the ultrasonic response amplitude. For future work, calculation of the POD using multi-parameter POD model with these parameters is planned. T2 - ESIS TC24 Workshop "Integrity of Railway Structures" CY - Leoben, Austria DA - 24.10.2016 KW - Crack KW - Reliability KW - POD KW - Axle KW - Ultrasonic PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-415201 DO - https://doi.org/10.1016/j.prostr.2017.07.002 SN - 2452-3216 VL - 4 SP - 79 EP - 86 PB - Elsevier, B.V. AN - OPUS4-41520 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tuma, Dirk A1 - Kumbhar, V. S. A1 - Lee, Y. R. A1 - Ra, C. S. A1 - Min, B.-K. A1 - Shim, J.-J. T1 - Modified chemical synthesis of MnS nanoclusters on nickel foam for high performance all-solid-state asymmetric supercapacitors N2 - Novel MnS nanoclusters were synthesized on nickel foam (NF) using a successive ionic layer adsorption and reaction (SILAR) method. MnS nanoclusters with different sizes were obtained by varying the number of deposition cycles. The crystal structure, chemical composition, and surface microstructure of the electrodes were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, field Emission scanning electron microscopy, and high-resolution transmission electron microscopy. The electrochemical behavior of the MnS nanoclusters was examined by cyclic voltammetry, galvanostatic charge–discharge, cycling test, and electrochemical impedance spectroscopy. The MnS nanoclusters prepared with 90 SILAR cycles showed the best supercapacitance in a 6 M KOH aqueous electrolyte with a specific capacitance of 828 F/g at a scan rate of 5 mV/s and cycling stability of 85.2 % after 5000 charge–discharge cycles. Moreover, an asymmetric supercapacitor (ASC) was assembled with the as-prepared MnS electrode on NF as the positive electrode, hydrothermally prepared reduced graphene oxide (rGO) on NF as the negative electrode, and PVA–KOH gel as the electrolyte. The MnS@NF//rGO@NF ASC showed excellent electrochemical performance with maximum energy and power densities of 34.1 Wh/kg and 12.8 kW/kg, respectively. The ASC also showed a capacitive retention of 86.5 % after 2000 charge–discharge cycles, highlighting its practical application for energy storage. KW - Nanocluster KW - Electrochemical behavior KW - Asymmetric supercapacitor KW - Graphene oxide PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-403147 DO - https://doi.org/10.1039/c7ra00772h SN - 2046-2069 VL - 7 IS - 27 SP - 16348 EP - 16359 PB - The Royal Society of Chemistry CY - London AN - OPUS4-40314 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lichtenstein, D. A1 - Ebmeyer, J. A1 - Meyer, T. A1 - Behr, A.-C. A1 - Kästner, Claudia A1 - Böhmert, L. A1 - Juling, J. A1 - Niemann, B. A1 - Fahrenson, C. A1 - Selve, S. A1 - Thünemann, Andreas A1 - Meijer, J. A1 - Estrela-Lopis, I. A1 - Bräuning, A. A1 - Lampen, A. T1 - It takes more than a coating to get nanoparticles through the intestinal barrier in vitro N2 - Size and shape are crucial parameters which have impact on the potential of nanoparticles to penetrate cell membranes and epithelial barriers. Current research in nanotoxicology additionally focuses on particle coating. To distinguish between core- and coating-related effects in nanoparticle uptake and translocation, two nanoparticles equal in size, coating and charge but different in core material were investigated. Silver and iron oxide nanoparticles coated with poly(acrylic acid) were chosen and extensively characterized by small-angle x-ray scattering, nanoparticle tracing analysis and transmission electron microscopy (TEM). Uptake and transport were studied in the intestinal Caco-2 model in a Transwell System with subsequent elemental analysis. TEM and ion beam microscopy were conducted for particle visualization. Although equal in size, charge and coating, the behavior of the two particles in Caco-2 cells was different: while the internalized amount was comparable, only iron oxide nanoparticles additionally passed the epithelium. Our findings suggest that the coating material influenced only the uptake of the nanoparticles whereas the translocation was determined by the core material. Knowledge about the different roles of the particle coating and core materials in crossing biological barriers will facilitate toxicological risk assessment of nanoparticles and contribute to the optimization of pharmacokinetic properties of nano-scaled pharmaceuticals. KW - Silver KW - Nanoparticle KW - Polymer KW - Polyacrylic acid PY - 2017 DO - https://doi.org/10.1016/j.ejpb.2016.12.004 SN - 0939-6411 SN - 1873-3441 VL - 118 SP - 21 EP - 29 PB - Elsevier AN - OPUS4-41170 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sieg, H. A1 - Kästner, Claudia A1 - Krause, B. A1 - Meyer, T. A1 - Burel, A. A1 - Böhmert, L. A1 - Lichtenstein, D. A1 - Jungnickel, H. A1 - Tentschert, J. A1 - Laux, P. A1 - Braeuning, A. A1 - Estreal-Lopis, I. A1 - Gauffre, F. A1 - Fessard, V. A1 - Meijer, J. A1 - Luch, A. A1 - Thünemann, Andreas A1 - Lampen, A. T1 - Impact of an artificial digestion procedure on aluminum-containing nanomaterials N2 - Aluminum has gathered toxicological Attention based on relevant human exposure and its suspected hazardous potential. Nanoparticles from food supplements or Food contact materials may reach the human gastrointestinal tract. Here, we monitored the physicochemical fate of aluminum containing nanoparticles and aluminum ions when passaging an in vitro model of the human gastrointestinal tract. Smallangle X-ray scattering (SAXS), transmission electron microscopy (TEM), ion beam microscopy (IBM), secondary ion beam mass spectrometry (TOF-SIMS), and inductively coupled plasma mass spectrometry (ICP-MS) in the singleparticle mode were employed to characterize two aluminumcontaining nanomaterials with different particle core materials (Al0, γAl2O3) and soluble AlCl3. Particle size and shape remained unchanged in saliva, whereas strong Agglomeration of both aluminum nanoparticle species was observed at low pH in gastric fluid together with an increased ion release. The levels of free aluminum ions decreased in intestinal fluid and the particles deagglomerated, thus liberating primary particles again. Dissolution of nanoparticles was limited and substantial changes of their shape and size were not detected. The amounts of particle-associated phosphorus, chlorine, potassium, and calcium increased in intestinal fluid, as compared to nanoparticles in standard dispersion. Interestingly, nanoparticles were found in the intestinal fluid after addition of ionic aluminum. We provide a comprehensive characterization of the fate of aluminum nanoparticles in simulated gastrointestinal fluids, demonstrating that orally ingested nanoparticles probably reach the intestinal epithelium. The balance between dissolution and de novo complex formation should be considered when evaluating nanotoxicological experiments. KW - Small-angle X-ray scattering KW - SAXS KW - Nanoparticle PY - 2017 DO - https://doi.org/10.1021/acs.langmuir.7b02729 SN - 1520-5827 SN - 0743-7463 VL - 33 IS - 40 SP - 10726 EP - 10735 PB - Americal Chemical Society AN - OPUS4-42438 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 - Leng, Jing A1 - Kang, Nianjun A1 - Wang, De-Yi A1 - Falkenhagen, Jana A1 - Thünemann, Andreas A1 - Schönhals, Andreas T1 - Structure–Property Relationships of Nanocomposites Based on Polylactide and Layered Double Hydroxides – Comparison of MgAl and NiAl LDH as Nanofiller N2 - Nanocomposites based on poly(L-lactide) (PLA) and organically modified Ni/Al layered double hydroxides (NiAl/LDHs) are prepared by melt blending and investigated by a combination of size exclusion chromatography, differential scanning calorimetry (DSC), small-angle X-ray scattering (SAXS), wide-angle X-ray scattering, and broadband dielectric spectroscopy. A detailed comparison to the behavior of the corresponding MgAl/LDH–PLA nanocomposites is made. SAXS investigations show that the morphology of the NiAl/LDH–PLA nanocomposites is more intercalated compared to the MgAl/LDH based PLA nanocomposite, which is more exfoliated. The DSC investigation gives a different dependence of the degree of crystallization on the concentration of LDH for NiAl/LDH–PLA than for MgAl/LDH–PLA nanocomposite system. These differences are discussed taking the differences of the morphologies of both systems into account. Broadband dielectric spectroscopy reveals information about the molecular dynamics where essential differences are observed for all relaxation processes taking place in both systems which were related to the different morphologies. KW - Nanocomposites KW - Polylactide PY - 2017 DO - https://doi.org/10.1002/macp.201700232 SN - 1022-1352 SN - 1521-3935 VL - 218 IS - 20 SP - Article 1700232, 1 EP - 12 PB - Wiley-VCH Verlag AN - OPUS4-42597 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 - Silverstein, R. A1 - Sobol, Oded A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang A1 - Eliezer, D. T1 - Hydrogen behavior in SAF 2205 duplex stainless steel N2 - This paper describes austenitic-ferritic duplex stainless steels, SAF 2205, in the presence of hydrogen. The duplex stainless steels (DSS) properties include excellent resistance to stress corrosion cracking, high strength and good weldability. Those steels are preferably used in industries combining hydrogen and loads. Hydrogen location in addition to hydrogen binding energy with the steel's defects are of great importance for the analysis of hydrogen embrittlement model in that steel. It is known from previously published works that the susceptibility to hydrogen embrittlement will depend on the competition between reversible and irreversible traps; meaning a direct relation to the hydrogen's state and position in the steel. In this work, we examine the local hydrogen concentration, trapping and distribution by two modern and advanced techniques: thermal desorption spectrometry (TDS) and we support it by time of flight-secondary ion mass spectrometer (ToF-SIMS). In this paper, we support and give for the first time new insights and better understanding to the hydrogen embrittlement mechanism in SAF 2205. The trapping energies levels were calculated using TDS and Lee and Lee's model. This model revealed reversible in addition to irreversible trapping sites. Also the trapping controlling mechanism was found to be a combination of detrapping controlled mechanism and diffusion controlled mechanism. The use of ToF-SIMS for local imaging the distribution of hydrogen species supports the discussion of the different hydrogen traps in this type of steel. The hydrogen embrittlemet phenomenon in SAF 2205 will be discussed in details in that paper. KW - Hydrogen trapping KW - Duplex stainless steel KW - Thermal desorption spectrometry (TDS) KW - ToF-SIMS PY - 2017 DO - https://doi.org/10.1016/j.jallcom.2016.11.184 SN - 0925-8388 SN - 1873-4669 VL - 695 SP - 2689 EP - 2695 PB - Elsevier B.V. AN - OPUS4-38856 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 - Sobol, Oded A1 - Nolze, Gert A1 - Saliwan Neumann, Romeo A1 - Eliezer, D. A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - Novel approach to image hydrogen distribution and related phase transformation in duplex stainless steels at the sub-micron scale N2 - The effect of electrochemical charging of hydrogen on the structure of a lean duplex stainless steel LDX 2101® (EN 1.4162, UNS S32101) was examined by both Time-of-Flight secondary ion mass spectrometry and electron back-scatter diffraction. The goal is to correlate hydrogen concentration and induced structural changes. Chemical and structural characterizations were done for the same region at the sample's surface with sub-micron spatial resolution. Regions of interest were varying in size between 50 × 50 μm and 100 × 100 μm. The results show a phase transformation of austenite to mainly a defect-rich BCC and scarcely a HCP phase. The phase transformation occurred in deuterium rich regions in the austenite. KW - Time-of-flight secondary ion mass spectrometry KW - ToF-SIMS KW - Electron backscatter diffraction KW - EBSD KW - Hydrogen-assisted cracking KW - Data fusion KW - Lean duplex stainless steel PY - 2017 DO - https://doi.org/10.1016/j.ijhydene.2017.08.016 SN - 0360-3199 VL - 42 IS - 39 SP - 25114 EP - 25120 AN - OPUS4-42022 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Haferkamp, Sebastian A1 - Fischer, Franziska A1 - Kraus, Werner A1 - Emmerling, Franziska T1 - Mechanochemical Knoevenagel condensation investigated in situ N2 - The mechanochemical Knoevenagel condensation of malononitrile with p-nitrobenzaldehyde was studied in situ using a tandem approach. X-ray diffraction and Raman spectroscopy were combined to yield time-resolved information on the milling process. Under solvent-free conditions, the reaction leads to a quantitative conversion to p-nitrobenzylidenemalononitrile within 50 minutes. The in situ data indicate that the process is fast and proceeds under a direct conversion. After stopping the milling process, the reaction continues until complete conversion. The continuous and the stopped milling process both result in crystalline products suitable for single crystal X-ray diffraction. KW - Mechanochemistry KW - Ball milling KW - C–C coupling KW - In situ KW - Knoevenagel condensation PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-425388 DO - https://doi.org/10.3762/bjoc.13.197 VL - 13 SP - 2010 EP - 2014 PB - Beilstein-Institut AN - OPUS4-42538 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szczerba, Wojciech A1 - Schneider, M. A1 - Żukrowski, J. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Riesemeier, Heinrich A1 - Sikora, M. A1 - Mandel, K. T1 - Spectroscopic Study of the Role of Metal Ions in the Adsorption Process of Phosphate in Nanoscaled Adsorbers Based on Metal (Zn/ Fe/Zr) Oxyhydroxides N2 - Currently great effort is made to find materials and technologies for the recycling of phosphate from wastewater. Herein, we present an in-depth study of the Phosphate adsorption mechanism of a promising adsorber material, a Zn−Fe−Zr oxyhydroxide-based nanostructured precipitate. The behavior of the multicomponent nanomaterial, consisting of both crystalline and amorphous parts, is investigated via X-ray absorption fine structure spectroscopy and Mössbauer spectroscopy, revealing the importance of the nanostructured composition for the phosphate adsorption. We found evidence that adsorption takes place especially in the vicinity of iron sites in the amorphous part of the material. KW - Zn-Fe-Zr nanoparticles KW - Adsorption of phosphate KW - XAFS KW - Catalysis PY - 2017 DO - https://doi.org/10.1021/acs.jpcc.7b04773 SN - 1932-7447 VL - 121 IS - 45 SP - 25033 EP - 25042 PB - ACS Publications AN - OPUS4-43348 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Rui A1 - Russo, Patrícia A. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Jeon, Taeyeol A1 - Pinna, Nicola T1 - Hybrid organic–inorganic transition-metal phosphonates as precursors for water oxidation electrocatalysts N2 - Efficient water oxidation catalysts are required for the development of water splitting technologies. Herein, the synthesis of layered hybrid NiFephenylphosphonate compounds from metal acetylacetonate precursors and phenylphosphonic acid in benzyl alcohol, and their Oxygen evolution reaction performance in alkaline medium, are reported. The hybrid particles are formed by inorganic layers of NiO6 and FeO6 distorted octahedra separated by bilayers of the organic group, and template the Formation in situ of NiFe hydroxide nanosheets of sizes between 5 and 25 nm and thicknesses between 3 and 10 nm. X-ray absorption spectroscopy measurements suggest that the hybrid also acts as a template for the local structure of the metal sites in the active catalyst, which remain distorted after the transformation. Optimum electrocatalytic activity is achieved with the hybrid compound with a Fe content of 16%. The combination of the synergistic effect between Ni and Fe with the structural properties of the hybrid results in an efficient catalyst that generates a current density of 10 mA cm−2 at an overpotential of 240 mV, and also in a stable catalyst that operates continuously at low overpotentials for 160 h. KW - Water oxydation catalysis KW - EXAFS PY - 2017 DO - https://doi.org/10.1002/adfm.201703158 SN - 1616-301X SN - 1616-3028 VL - 27 IS - 40 SP - Article 1703158, 1 EP - 11 PB - WILEY-VCH Verlag CY - Weinheim AN - OPUS4-42783 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pasternak, H. A1 - Launert, B. A1 - Kannengießer, Thomas A1 - Rhode, Michael T1 - Advanced residual stress assessment of plate girders through welding simulation N2 - This article provides an impression on potentials in applying nowadays welding simulation tools in construction design. This is carried out exemplary on plate girders from two structural steel grades. The calculated residual stresses are compared with measurements by sectioning method. It has been repeatedly stated that present Eurocode models fail to approximate the residual stresses. Especially for high strength steel (HSS) only limited information is available on realistic occurring residual stresses in typical I-girders. The investigations are aimed to give further guidance on these values. A few proposals on advanced models are discussed. T2 - MBST 2016 - Modern Building Materials, Structures and Techniques CY - Vilnius, Litunia DA - 26.05.2016 KW - Residual stresses KW - Plate girders KW - I-shape sections KW - High-strength steel KW - Welding simulation PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-392177 UR - http://www.sciencedirect.com/science/article/pii/S1877705817305192 DO - https://doi.org/10.1016/j.proeng.2017.02.013 SN - 1877-7058 IS - 172 SP - 23 EP - 30 PB - Elsevier CY - Amsterdam, Niederlande AN - OPUS4-39217 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Omara, Shereen Shabaan A1 - Turky, G. A1 - Ghoneim, A. A1 - Thünemann, Andreas A1 - Abdel Rehim, M. H. A1 - Schönhals, Andreas T1 - Hyperbranched poly(amidoamine)/kaolinite nanocomposites: Structure and charge carrier dynamics N2 - An ex-situ approach was applied to prepare nanocomposites from hyperbranched poly(amidoamine) and modified kaolinite (Ka-DCA). The structure of the polymer and the corresponding nanocomposites was investigated by FTIR, DSC, SAXS and TEM. SAXS might suggest a partly exfoliated structure of the nanocomposites, which was supported by TEM. The molecular dynamics was studied by means of broadband dielectric spectroscopy (BDS). The dielectric spectra are dominated by a conductivity contribution at higher temperatures for all samples investigated. The obtained results further indicated that DC conductivity is increased by 4 orders of magnitude with increasing concentration of Ka-DCA nanofiller. Further, a significant separation between the conductivity relaxation time and that of segmental dynamics was observed. The decoupling phenomenon and the conductivity mechanism were discussed in detail. This study provides insights about the influence of the nanofiller on the structure and the conductivity contribution of nanocomposites of hyperbranched polymers including the decoupling phenomenon and fragility. KW - Hyperbranched polymers KW - Nanocomposites KW - Conductivity PY - 2017 DO - https://doi.org/10.1016/j.polymer.2017.06.017 SN - 0032-3861 VL - 121 SP - 64 EP - 74 PB - Elsevier Ltd. AN - OPUS4-40648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Juling, S. A1 - Niedzwiecka, A. A1 - Böhmert, L. A1 - Lichtenstein, D. A1 - Selve, S. A1 - Braeuning, A. A1 - Thünemann, Andreas A1 - Krause, E. A1 - Lampen, A. T1 - Protein Corona Analysis of Silver Nanoparticles Links to Their Cellular Effects N2 - The breadth of applications of nanoparticles and the access to food-associated consumer products containing nanosized materials lead to oral human exposure to such particles. In biological fluids nanoparticles dynamically interact with biomolecules and form a protein corona. Knowledge about the protein corona is of great interest for understanding the molecular effects of particles as well as their fate inside the human body. We used a mass spectrometry-based toxicoproteomics approach to elucidate mechanisms of toxicity of silver nanoparticles and to comprehensively characterize the protein corona formed around silver nanoparticles in Caco-2 human intestinal epithelial cells. Results were compared with respect to the cellular function of proteins either affected by exposure to nanoparticles or present in the protein corona. A transcriptomic data set was included in the analyses in order to obtain a combined multiomics view of nanoparticle-affected cellular processes. A relationship between corona proteins and the proteomic or transcriptomic responses was revealed, showing that differentially regulated proteins or transcripts were engaged in the same cellular signaling pathways. Protein corona analyses of nanoparticles in cells might therefore help in obtaining information about the molecular consequences of nanoparticle treatment. KW - Silver nanoparticles KW - Protein KW - Small-angle X-ray scattering KW - SAXS PY - 2017 DO - https://doi.org/10.1021/acs.jproteome.7b00412 SN - 1535-3893 SN - 1535-3907 VL - 16 IS - 11 SP - 4020 EP - 4034 PB - Americal Chemical Society AN - OPUS4-42688 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 - Mirtschin, Nikolaus A1 - Pretsch, T. T1 - Programming of one- and two-step stress recovery in a poly(ester urethane) N2 - This work demonstrates that phase-segregated poly(ester urethane) (PEU) with switching segments of crystallizable poly(1,4-butylene adipate) (PBA) can be programmed to generate two separate stress recovery events upon heating under constant strain conditions. For programming, two elongations are applied at different temperatures, followed by unloading and cooling. During the adjacent heating, two-step stress recovery is triggered. The results indicate that the magnitude of the stress recovery signals corresponds to the recovery of the two deformation stresses in reverse order. As demonstrated by further experiments, twofold stress recovery can be detected as long as the elongation at higher temperature exceeds the strain level of the deformation at lower temperature. Another finding includes that varying the lower deformation temperature enables a control over the stress recovery temperature and thus the implementation of so-called “temperature-memory effects”. Moreover, exerting only one elongation during programming enables a heating-initiated one-step stress recovery close to the deformation temperature. Based on these findings, such polymers may offer new technological opportunities in the fields of active assembly when used as fastening elements and in functional clothing when utilized for compression stockings. KW - DSC KW - Mechanical properties PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-393585 DO - https://doi.org/10.3390/polym9030098 SN - 2073-4360 VL - 9 IS - 3 SP - Article 98, 1 EP - 12 PB - MDPI CY - Basel AN - OPUS4-39358 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauw, Brian Richard A1 - Smith, A. J. A1 - Snow, T. A1 - Terril, N. J. A1 - Thünemann, Andreas T1 - The modular small-angle X-ray scattering data correction sequence N2 - Data correction is probably the least favourite activity amongst users experimenting with small-angle X-ray scattering: if it is not done sufficiently well, this may become evident only during the data analysis stage, necessitating the repetition of the data corrections from scratch. A recommended comprehensive sequence of elementary data correction steps is presented here to alleviate the difficulties associated with data correction, both in the laboratory and at the synchrotron. When applied in the proposed order to the raw signals, the resulting absolute scattering cross section will provide a high degree of accuracy for a very wide range of samples, with its values accompanied by uncertainty estimates. The method can be applied without modification to any pinhole-collimated instruments with photon-counting direct-detection area detectors. KW - Small-angle X-ray scattering KW - SAXS KW - Accuracy KW - Methodology KW - Data correction PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-432114 DO - https://doi.org/10.1107/S1600576717015096 SN - 1600-5767 VL - 50 IS - 6 SP - 1800 EP - 1811 PB - International Union of Crystallography AN - OPUS4-43211 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauw, Brian Richard A1 - Kästner, Claudia A1 - Thünemann, Andreas T1 - Nanoparticle size distribution quantification: results of a small-angle X-ray scattering inter-laboratory comparison N2 - This paper presents the first worldwide inter-laboratory comparison of small-angle X-ray scattering (SAXS) for nanoparticle sizing. The measurands in this comparison are the mean particle radius, the width of the size distribution and the particle concentration. The investigated sample consists of dispersed silver nanoparticles, surrounded by a stabilizing polymeric shell of poly(acrylic acid). The silver cores dominate the X-ray scattering pattern, leading to the determination of their radius size distribution using (i) the generalized indirect Fourier transformation method, (ii) classical model fitting using SASfit and (iii) a Monte Carlo fitting approach using McSAS. The application of these three methods to the collected data sets from the various laboratories produces consistent mean number- and volume-weighted core radii of Rn = 2.76 (6) nm and Rv = 3.20 (4) nm, respectively. The corresponding widths of the lognormal radius distribution of the particles were σn = 0.65 (1) nm and σv = 0.71 (1) nm. The particle concentration determined using this method was 3.0 (4) g l−1 or 4.2 (7) × 10−6 mol l−1. These results are affected slightly by the choice of data evaluation procedure, but not by the instruments: the participating laboratories at synchrotron SAXS beamlines, commercial and in-house-designed instruments were all able to provide highly consistent data. This demonstrates that SAXS is a suitable method for revealing particle size distributions in the sub-20 nm region (at minimum), out of reach for most other analytical methods. KW - SAXS KW - Small-angle X-ray scattering KW - Silver nanoparticles PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-422800 DO - https://doi.org/10.1107/S160057671701010X SN - 1600-5767 VL - 50 IS - 5 SP - 1280 EP - 1288 PB - (IUCr) International Union of Crystallography AN - OPUS4-42280 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szczerba, Wojciech A1 - Costo, R. A1 - Veintemillas-Verdaguer, S. A1 - del Puerto Morales, M. A1 - Thünemann, Andreas T1 - SAXS analysis of single- and multi-core iron oxide magnetic nanoparticles N2 - This article reports on the characterization of four superparamagnetic iron oxide nanoparticles stabilized with dimercaptosuccinic acid, which are suitable candidates for reference materials for magnetic properties. Particles p1 and p2 are single-core particles, while p3 and p4 are multi-core particles. Small-angle X-ray scattering analysis reveals a lognormal type of size distribution for the iron oxide cores of the particles. Their mean radii are 6.9 nm (p1), 10.6 nm (p2), 5.5 nm (p3) and 4.1 nm (p4), with narrow relative distribution widths of 0.08, 0.13, 0.08 and 0.12. The cores are arranged as a clustered network in the form of dense mass fractals with a fractal dimension of 2.9 in the multi-core particles p3 and p4, but the cores are well separated from each other by a protecting organic shell. The radii of gyration of the mass fractals are 48 and 44 nm, and each network contains 117 and 186 primary particles, respectively. The radius distributions of the primary particle were confirmed with transmission electron microscopy. All particles contain purely maghemite, as shown by X-ray absorption fine structure spectroscopy KW - Superparamagnetic nanoparticles KW - Iron oxide KW - Reference materials KW - SAXS KW - Small-angle x-ray scattering KW - XANES KW - X-ray absorption near-edge structure KW - X-ray absorption fine structure PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-395948 DO - https://doi.org/10.1107/S1600576717002370 SN - 1600-5767 VL - 50 IS - Part 2 SP - 481 EP - 488 PB - (IUCr) International Union of Crystallography AN - OPUS4-39594 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kästner, Claudia A1 - Lichtenstein, Dajana A1 - Lampen, Alfonso A1 - Thünemann, Andreas T1 - Monitoring the fate of small silver nanoparticles during artificial digestion N2 - The report on the results of an in vitro digestion study of silver nanoparticles in presence and absenceof food. The particles were poly(acrylic acid) stabilized ultra-small silver nanoparticles with a radius of 3.1 nm and a relative size distribution width of 0.2. As food components oil, starch, skimmed milk powderand a mixture thereof were chosen. Aggregation of the particles was quantified with small-angle X-rayscattering in terms of log-normal radii distributions. Complete aggregation of the primary particles wasdetermined in the absence of food. In contrast, the presence of oil and starch initiates a disaggregationin the intestine. Only small aggregates of 6 nm radii and aggregation numbers of 7 were found in thepresence of milk powder. It prevents primary particles from etching in the gastric and intestinal juice.Our results indicate that the silver nanoparticles can pass the digestion process in a nanoscale form butundergo a strong and food-dependent transformation in their state of aggregation. KW - Small-angle X-ray scattering KW - SAXS PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-404099 DO - https://doi.org/10.1016/j.colsurfa.2016.08.013 SN - 0927-7757 SN - 1873-4359 VL - 526 SP - 76 EP - 81 PB - Elsevier B.V. AN - OPUS4-40409 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Terkawi, Abdal-Azim A1 - Scholz, G. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinsch, Stefan A1 - Kemnitz, E. A1 - Emmerling, Franziska T1 - Ca- and Sr- tetrafluoroisophthalates: mechanochemical synthesis, characterization, and ab initio structure determination N2 - New fluorinated coordination polymers were prepared mechanochemically by milling the alkaline earth metal hydroxides MII(OH)2·xH2O (MII: Ca, Sr) with tetrafluoroisophthalic acid (H2mBDC-F4). The structures of [{Ca(mBDC-F4)(H2O)2}·H2O] and [{Sr(mBDC-F4)(H2O)2}·H2O] were determined based on ab initio calculations and their powder X-ray diffraction (PXRD) data. The compounds are isomorphous and crystallize in the orthorhombic space group P212121. The determined structures were validated by using extended X-ray absorption (EXAFS) data. The new materials were thoroughly characterized using elemental analysis, thermal analysis, magic angle spinning NMR, and attenuated total reflection-infrared spectroscopy. Further characterization methods such as BET, dynamic vapor sorption, and scanning electron microscopy imaging were also used. Our investigations indicate that mechanochemistry is an efficient method for preparing such materials. KW - Mechanochemistry KW - In situ KW - XRD KW - Coordination polymers PY - 2017 UR - http://pubs.rsc.org/-/content/articlehtml/2017/dt/c7dt00734e DO - https://doi.org/10.1039/c7dt00734e VL - 46 IS - 18 SP - 6003 EP - 6012 AN - OPUS4-41516 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wolf, Marcus A1 - Afanasiev, Roman A1 - Böllinghaus, Thomas A1 - Pfennig, A. T1 - Investigation of Corrosion Fatigue of Duplex Steel X2CrNiMoN22-5 3 Exposed to a Geothermal Environment under Different Electrochemical Conditions and Load Types N2 - Corrosion fatigue (CF) of duplex stainless steel (DSS) X2CrNiMoN22-5-3 was investigated in in-situ geothermal conditions of the Northern German Basin (NGB). The influence of the load type on CF behavior of the alloy was examined by applying push/pull and rotating bending cyclic load to failure. The hour-glass shaped specimens with both polished and precisely turned surface finish were tested in corrosion chambers allowing for the permanent circulation of Northern German Basin electrolyte heated to 369 K. Additionally, the influence of a protective cathodic potential on the CF life expectancy was investigated by employing a potentiostat. The rotating bending cyclic load led to a higher CF life expectancy, which decreased with increasing duration of the experiment due to a higher deterioration rate of the material. The application of a cathodic potential caused a significant increase of the CF lifespan from 4.7 x 105 (open-circuit potential (OCP)) to 107 cycles (preset threshold cycle number) for the potential range from USHE = – 450 to – 900 mV. Microstructural analysis of the CF damage revealed horizontal grain attack within corrosion pit cavities, multiple fatigue cracks and preferable deterioration of the austenitic phase. T2 - 13th International Conference on Greenhouse Gas Control Technologies, GHGT-13 CY - Lausanne, Switzerland DA - 14.11.2016 KW - Different load cases KW - Corrosion fatigue KW - DSS KW - Geothermal environment KW - Different electrochemical conditions PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-439231 DO - https://doi.org/10.1016/j.egypro.2017.03.1657 SN - 1876-6102 VL - 114 SP - 5337 EP - 5345 PB - Elsevier Science AN - OPUS4-43923 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 - Hernández-Nava, E. A1 - Tammas-Williams, S. A1 - Smith, C. A1 - Léonard, Fabien A1 - Withers, P. J. A1 - Todd, I. A1 - Goodall, R. T1 - X-ray tomography characterisation of lattice structures processed by selective electron beam melting N2 - Metallic lattice structures intentionally contain open porosity; however, they can also contain unwanted closed porosity within the structural members. The entrained porosity and defects within three different geometries of Ti-6Al-4V lattices, fabricated by Selective Electron Beam Melting (SEBM), is assessed from X-ray computed tomography (CT) scans. The results suggest that horizontal struts that are built upon loose powder show particularly high (~20 x 10⁻³ vol %) levels of pores, as do nodes at which many (in our case 24) struts meet. On the other hand, for struts more closely aligned (0° to 54°) to the build direction, the fraction of porosity appears to be much lower (~0.17 x 10⁻³%) arising mainly from pores contained within the original atomised powder particles. KW - Cellular solids KW - Aqdditive manufacturing KW - Computed tomography KW - Titanium alloys PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-413689 UR - http://www.mdpi.com/2075-4701/7/8/300 DO - https://doi.org/10.3390/met7080300 SN - 2075-4701 VL - 7 IS - 8 SP - Article 300, 1 EP - 12 PB - MDPI AN - OPUS4-41368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Naresh-Kumar, G. A1 - Vilalta-Clemente, A. A1 - Jussila, H. A1 - Winkelmann, Aimo A1 - Nolze, Gert A1 - Vespucci, S. A1 - Nagarajan, S. A1 - Wilkinson, A. J. A1 - Trager-Cowan, C. T1 - Quantitative imaging of anti-phase domains by polarity sensitive orientation mapping using electron backscatter diffraction N2 - Advanced structural characterisation techniques which are rapid to use, non-destructive and structurally definitive on the nanoscale are in demand, especially for a detailed understanding of extended-defects and their influence on the properties of materials. We have applied the electron backscatter diffraction (EBSD) technique in a scanning electron microscope to non-destructively characterise and quantify antiphase domains (APDs) in GaP thin films grown on different (001)Si substrates with different offcuts. We were able to image and quantify APDs by relating the asymmetrical intensity distributions observed in the EBSD patterns acquired experimentally and comparing the same with the dynamical electron diffraction simulations. Additionally mean angular error maps were also plotted using automated cross-correlation based approaches to image APDs. Samples grown on substrates with a 4° offcut from the [110] do not show any APDs, whereas samples grown on the exactly oriented substrates contain APDs. The procedures described in our work can be adopted for characterising a wide range of other material systems possessing non-centrosymmetric point groups. KW - Polarity KW - Semiconductor KW - Antiphase boundary PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-420167 SN - 2045-2322 VL - 7 SP - Article 10916, 1 EP - 10 AN - OPUS4-42016 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bender, P. A1 - Bogart, L.K. A1 - Posth, O. A1 - Szczerba, Wojciech A1 - Rogers, S.E. A1 - Castro, A. A1 - Nilsson, L. A1 - Zeng, L. J. A1 - Sugunan, A. A1 - Sommertune, J. A1 - Fornara, A. A1 - Gonzales-Alonso, D. A1 - Fernandez Barquin, L. A1 - Johansson, C. T1 - Structural and magnetic properties of multi-core nanoparticles analysed using a generalised numerical inversion method N2 - The structural and magnetic properties of magnetic multi-core particles were determined by numerical inversion of small angle scattering and isothermal magnetisation data. The investigated particles consist of iron oxide nanoparticle cores (9 nm) embedded in poly(styrene) spheres (160 nm). A thorough physical characterisation of the particles included transmission electron microscopy, X-ray diffraction and asymmetrical flow field-flow fractionation. Their structure was ultimately disclosed by an indirect Fourier transform of static light scattering, small angle X-ray scattering and small angle neutron scattering data of the colloidal dispersion. The extracted pair distance distribution functions clearly indicated that the cores were mostly accumulated in the outer surface layers of the poly(styrene) spheres. To investigate the magnetic properties, the isothermal magnetisation curves of the multi-core particles (immobilised and dispersed in water) were analysed. The study stands out by applying the same numerical approach to extract the apparent moment distributions of the particles as for the indirect Fourier transform. It could be shown that the main peak of the apparent moment distributions correlated to the expected intrinsic moment distribution of the cores. Additional peaks were observed which signaled deviations of the isothermal magnetisation behavior from the non-interacting case, indicating weak dipolar interactions. KW - Numerical inversion KW - Magnetic nanoparticles KW - Iron oxides KW - Magnetic properties KW - Structural properties PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-400952 DO - https://doi.org/10.1038/srep45990 SN - 2045-2322 VL - 7 SP - Article 45990, 1 EP - 14 AN - OPUS4-40095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Olejko, Lydia A1 - Bald, Ilko T1 - FRET efficiency and antenna effect in multi-color DNA origami-based light harvesting systems N2 - Artificial light harvesting complexes find applications in artificial photosynthesis, photovoltaics and light harvesting chemical sensors. They are used to enhance the absorption of light of a reaction center which is often represented by a single acceptor. Here, we present different light harvesting systems on DNA origami structures and analyze systematically the light harvesting efficiency. By changing the number and arrangement of different fluorophores (FAM as donor, Cy3 as transmitter and Cy5 as acceptor molecules) the light harvesting efficiency is optimized to create a broadband absorption and to improve the antenna effect 1 (including two energy transfer steps) from 0.02 to 1.58, and the antenna effect 2 (including a single energy transfer step) from 0.04 to 8.7, i.e. the fluorescence emission of the acceptor is significantly higher when the light-harvesting antenna is excited at lower wavelength compared to direct excitation of the acceptor. The channeling of photo energy to the acceptor proceeds by Förster Resonance Energy Transfer (FRET) and we carefully analyze also the FRET efficiency of the different light harvesting systems. Accordingly, the antenna effect can be tuned by modifying the stoichiometry of donor, transmitter and acceptor dyes, whereas the FRET efficiency is mainly governed by the spectroscopic properties of dyes and their distances. KW - DNA origami KW - Light-harvesting KW - FRET KW - Antenna effect PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-405867 UR - http://pubs.rsc.org/en/content/articlelanding/2017/ra/c7ra02114c#!divAbstract DO - https://doi.org/10.1039/C7RA02114C VL - 7 IS - 39 SP - 23924 EP - 23934 PB - The Royal Soc. of Chemistry AN - OPUS4-40586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosemann, Paul A1 - Müller, C. A1 - Baumann, O. A1 - Modersohn, W. A1 - Halle, T. T1 - Influence of the post-weld surface treatment on the corrosion resistance of the duplex stainless steel 1.4062 N2 - The duplex stainless steel 1.4062 (X2CrNiN22-2) is used as alternative material to austenitic stainless steels in the construction industry. The corrosion resistance of welded seams is influenced by the base material, the weld filler material, the welding process and also by the final surface treatment. The scale layer next to the weld seam can be removed by grinding, pickling, electro-polished or blasting depending on the application and the requested corrosion resistance. Blasted surfaces are often used in industrial practice due to the easier and cheaper manufacturing process compared to pickled or electro-polished surfaces. Furthermore blasting with corundum-grain is more effective than blasting with glass-beads which also lower the process costs. In recent years, stainless steel surfaces showed an unusually high susceptibility to pitting corrosion after grinding with corundum. For this reason, it is now also questioned critically whether the corrosion resistance is influenced by the applied blasting agent. This question was specifically investigated by comparing grinded, pickled, corundum-grain- and glass-bead-blasted welding seams. Results of the SEM analyses of the blasting agents and the blasted surfaces will be presented and correlated with the different performed corrosion tests (potential measurement, KorroPad-test and pitting potential) on welding seams with different surface treatments. T2 - 19th Chemnitz Seminar on Materials Engineering – 19. Werkstofftechnisches Kolloquium CY - Chemnitz, Germany DA - 16.03.2017 KW - Corrosion resistance KW - Welding KW - Duplex stainless steels KW - Pitting corrosion KW - Surface treatment PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-395374 DO - https://doi.org/10.1088/1757-899X/181/1/012019 SN - 1757-899X SN - 1757-8981 VL - 181 IS - Conference 1 SP - Article UNSP 012019, 1 EP - 9 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-39537 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Asadujjaman, Asad A1 - Kent, B. A1 - Bertin, Annabelle T1 - Phase transition and aggregation behaviour of an UCST-type copolymer poly(acrylamide-coacrylonitrile) in water: effect of acrylonitrile content, concentration in solution, copolymer chain length and presence of electrolyte N2 - An UCST-type copolymer of acrylamide (AAm) and acrylonitrile (AN) (poly(AAm-co-AN)) was prepared by reversible addition fragmentation chain transfer (RAFT) polymerization and its temperature-induced phase transition and aggregation behaviour studied by turbidimetry, static and dynamic light scattering, small angle neutron scattering (SANS) and cryo-transmission electron microscopy (cryo-TEM) measurements. The phase transition temperature was found to increase with increasing AN content in the copolymer, concentration of the solutions and copolymer chain length. A significant effect was observed onto the phase transition temperature by addition of different electrolytes into the copolymer solution. The copolymer chains were aggregated below the phase transition temperature and disaggregated above it. The size of the aggregates increases with increasing AN contents and concentration of the copolymer solutions below the phase transition temperature. The copolymer chains were expanded and weekly associated in solution above the phase transition temperature. A model is proposed to explain such association–aggregation behaviour of poly(AAm-co-AN) copolymers depending on AN contents and concentration of the copolymer solutions as a function of temperature. KW - Thermoresponsive polymers KW - UCST-type copolymer PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-394636 DO - https://doi.org/10.1039/c6sm02262f SN - 1744-683X SN - 1744-6848 VL - 13 IS - 3 SP - 658 EP - 669 PB - RSC AN - OPUS4-39463 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 - Theiler, Geraldine A1 - Gradt, Thomas T1 - Gleitverhalten von PEEK-Kompositwerkstoffen in Wasserstoffumgebung N2 - Die Reibeigenschaften von PEEK Materialien gegen Stahlscheiben wurden in Luft, Vakuum und Wasserstoffumgebung untersucht. KW - PEEK-Komposite KW - Wasserstoff KW - Vakuum KW - Graphit PY - 2017 SN - 0724-3472 VL - 64 IS - 6 SP - 52 EP - 59 AN - OPUS4-42919 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baer, Wolfram A1 - Wossidlo, Peter T1 - Validation of a low blow specimen technique for R-curve determination using a drop tower N2 - Fracture mechanics based component design requires appropriate fracture mechanics toughness data with respect to both, loading rate as well as test temperature. Taking high-rate loading into account such as with accidental scenarios, different standards such as ASTM E 1820 or BS 7448-3 provide some information on dynamic fracture mechanics testing. Nevertheless, the designations differ so that a validation of the own material specific test method used for dynamic R-curve determination is mandatory. In order to address this for ductile cast iron materials an experimental method for the reliable determination of dynamic J-integral crack resistance curves at -40 °C following the multiple specimen approach has been established and validated. The experimental concept offers some additional valuable features. Single values of dynamic crack initiation toughness can be determined using a single specimen technique based on crack sensors. Furthermore, an experimentally independent method is provided according to which CTOD δ5 R-curves can be established. The focus of the present paper is on the validation of the experimental low blow technique using a drop tower test system. A drop tower test system was developed and set up to perform low blow tests at temperatures down to -40 °C. The system allows for a variation of the impact mass and height and was optimized for testing of ductile cast iron at stress intensity rates from approximately 5∙10⁴ to 3∙10⁵ MPa√ms⁻¹. This range of loading rate is characteristic for instance with crash scenarios of heavy sectioned DCI casks for radioactive materials. In order to address characteristic challenges of impact tests (test duration of microseconds up to milliseconds, inertial effects, signal oscillations), an appropriate full bridge strain gage method for the measurement of force directly on the specimen as well as a non-contact measurement of load line displacement using an optical extensometer have been developed and validated. The low blow test requires either to prevent bouncing strikes of the hammer by using the stop block technique or to catch the hammer after its first strike. Both options are not part of the experimental concept and setup which have been realized here. The paper describes investigations which have been performed in order to make sure that bouncing strikes of the hammer do not cause additional crack extension in the specimen. This is necessary to ensure a unique relation between the work done and the achieved crack extension. The investigations covered the analysis of limit loads of the specimen with respect to the measured force. The measured stiffness of the specimen was assessed and signals of crack sensors were analyzed. Furthermore, an analysis of the mechanical behavior of the loading system and the specimen by optical observation was performed. Corresponding results are discussed in the paper. It had finally been proven that additional crack extension in the specimen due to bouncing strikes of the hammer is not to be expected under the given conditions of test setup, material and loading. It can be seen as a major experimental advantage that the striker does not have to be catched after the low blow test. T2 - XXIV Italian Group of Fracture Conference CY - Urbino, Italy DA - 01.03.2017 KW - Dynamic fracture mechanics KW - R-curve KW - Low blow KW - Ductile cast iron PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-437686 DO - https://doi.org/10.1016/j.prostr.2017.04.005 SN - 2452-3216 VL - 3 SP - 25 EP - 32 AN - OPUS4-43768 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kühn, Hans-Joachim A1 - Rehmer, Birgit A1 - Skrotzki, Birgit T1 - Thermomechanical fatigue of heat-resistant austenitic cast iron EN-GJSA-XNiSiCr35-5-2 (Ni-Resist D-5S) N2 - TMF tests were carried out on EN-GJSA-XNiSiCr35-5-2 at constant minimum temperature (400 °C) and varying maximum temperatures (Tmax = 700 °C, 800 °C, 900 °C) with hold times of 180 s at Tmax and two phase angles (in-phase (IP), 180° out-of-phase (OP)). The results showed a comparable strength under OP- and IP-TMF loading. At Tmax = 700 °C and 900 °C, the lifetime in IP-tests was slightly longer than that of OP-tests, while it is vice versa at Tmax = 800 °C. The IP-tests at Tmax = 900 °C showed a similar lifetime as OP-tests at Tmax = 700 °C and 800 °C, which was unexpected for such a high testing temperature. All IP-tests at Tmax = 900 °C showed a continuous cyclic softening from the beginning on, which was different from all other testing conditions. Complementary metallographic investigations indicated that under this test condition, intergranular creep damage is present in the volume of the test pieces. T2 - 3rd International Workshop on Thermo-Mechanical Fatigue (TMF-Workshop 2016) CY - Berlin, Germany DA - 27.04.2016 KW - Cast iron KW - Cracks KW - Cyclic softening KW - Microscopy KW - Thermomechanical fatigue PY - 2017 DO - https://doi.org/10.1016/j.ijfatigue.2017.01.009 SN - 0142-1123 SN - 1879-3452 VL - 99 IS - 2 (Special issue: Recent developments in thermo-mechanical fatigue) SP - 295 EP - 302 PB - Elsevier CY - Oxford AN - OPUS4-39680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madkour, Sherif A1 - Szymoniak, Paulina A1 - Radnik, Jörg A1 - Schönhals, Andreas T1 - Unraveling the Dynamics of Nanoscopically Confined PVME in Thin Films of a Miscible PVME/PS Blend N2 - Broadband dielectric spectroscopy (BDS) was employed to investigate the glassy dynamics of thin films (7−200 nm) of a poly(vinyl methyl ether) (PVME)/polystyrene (PS) blend (50:50 wt %). For BDS measurements, nanostructured capacitors (NSCs) were employed, where films are allowed a free surface. This method was applied for film thicknesses up to 36 nm. For thicker films, samples were prepared between crossed electrode capacitors (CECs). The relaxation spectra of the films showed multiple processes. The first process was assigned to the α-relaxation of a bulklike layer. For films measured by NSCs, the rates of α-relaxation were higher compared to those of the bulk blend. This behavior was related to the PVME-rich free surface layer at the polymer/air interface. The second process was observed for all films measured by CECs (process X) and the 36 nm film measured by NSCs (process X2). This process was assigned to fluctuations of constraint PVME segments by PS. Its activation energy was found to be thickness-dependent because of the evidenced thickness dependency of the compositional heterogeneity. Finally, a third process with an activated temperature dependence was observed for all films measured by NSCs (process X1). It resembled the molecular fluctuations in an adsorbed layer found for thin films of pure PVME, and thus, it is assigned accordingly. This process undergoes an extra confinement because of frozen adsorbed PS segments at the polymer/substrate interface. To our knowledge, this is the first example where confinement-induced changes were observed by BDS for blend thin films KW - Thin Films KW - Broadband Dielectric Spectroscopy PY - 2017 DO - https://doi.org/10.1021/acsami.7b10572 SN - 1944-8244 VL - 9 IS - 42 SP - 37289 EP - 37299 PB - ACS Publications AN - OPUS4-42652 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 - Fedelich, Bernard A1 - Kühn, Hans-Joachim A1 - Rehmer, Birgit A1 - Skrotzki, Birgit T1 - Experimental and analytical investigation of the TMF-HCF lifetime behavior of two cast iron alloys N2 - The combined loading Thermomechanical Fatigue (TMF) with High Cycle Fatigue (HCF) has been experimentally investigated for two cast iron alloys. Both alloys contain globular graphite nodules but the first one has a ferritic structure while the second one has an austenitic crystal structure. In particular, the influences of the HCF frequency, of the HCF loading amplitude and of the location of the superposed HCF cycles have been investigated. It was observed that the HCF frequency has a limited impact on the fatigue life. On the other side, the HCF-strain amplitude has a highly non-linear influence on the fatigue life. The experimental results can be understood in terms of a fracture mechanics based damage mechanism: Cracks quickly initiate due to the TMF loading and the growth of the cracks up to a few mm controls the fatigue life. If HCF-loading cycles are superposed, cyclic crack propagation dramatically accelerates after a threshold has been reached. This threshold is regarded as controlling the fatigue life reduction. The previous ideas have been expressed in a model that can be very simply applied to estimate the fatigue life reduction ratio due to the superposed HCF cycles. It only contains two adjustable parameters and can be combined with any TMF life assessment model. T2 - 3rd International Workshop on Thermo-Mechanical Fatigue (TMF-Workshop 2016) CY - Berlin, Germany DA - 27.04.2016 KW - Thermomechanical Fatigue (TMF) KW - High Cycle Fatigue (HCF) KW - Cast iron KW - Fatigue assessment PY - 2017 DO - https://doi.org/10.1016/j.ijfatigue.2016.11.013 SN - 0142-1123 SN - 1879-3452 VL - 99 IS - 2 (Special issue: Recent developments in thermo-mechanical fatigue) SP - 266 EP - 278 PB - Elsevier CY - Oxford AN - OPUS4-39810 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Pourmand, P. A1 - Wolff, Dietmar A1 - Gedde, U.W. T1 - Influence of ageing on sealability of elastomeric O-rings N2 - At BAM, which is the federal institute for materials research and testing in Germany, it is one of our tasks to evaluate the safety of casks designed for transport and/or storage of radioactive material. This includes the assessment of the service lifetime of elastomeric seals that are part of the container lid system with regard to the requirements for long-term safety (40 years and more) of the containers. Therefore, we started an accelerated ageing programme with selected rubbers often used for seals (HNBR, EPDM and FKM) which are aged at four different temperatures (75 °C, 100 °C, 125 °C and 150 °C) up to 1.5 years. In order to assess sealability, O-rings are aged in compression by 25 % (corresponding to the compression during service) between plates as well as in flanges that allow leakage rate measurements. For comparison, uncompressed O-rings are aged as well. Further methods characterising seal performance are compression stress relaxation (CSR) reflecting the loss of sealing force of a compressed seal over time, and compression set (CS) which represents the recovery behaviour of a seal after release from compression. Additionally, hardness is measured for information about the change of mechanical properties. The experimental results indicate that while hardness, CSR and CS show considerable degradation effects, the leakage rate stays relatively constant or even decreases until shrinkage combined with the loss of resilience of the aged seal leads to leakage. This demonstrates that static leakage rate, which is the only available direct seal performance criterion, has only limited sensitivity towards the degradation of the seal material. CS data is extrapolated using time-temperature shifts and Arrhenius graphs. An exemplary CS of 50 % would be reached after approx. 1.2, 17 and 29 years at 60 °C for HNBR, EPDM and FKM respectively. T2 - PolymerTec 2016 CY - Merseburg, Germany DA - 15.06.2016 KW - Compression KW - Leakage KW - Degradation KW - Rubber KW - Lifetime PY - 2017 DO - https://doi.org/10.1002/masy.201600157 SN - 1022-1360 SN - 1521-3900 VL - 373 IS - 1 SP - UNSP 1600157, 1 EP - 10 PB - WILEY-V C H VERLAG GMBH CY - Weinheim AN - OPUS4-40958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 - 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 - Mishurova, Tatiana A1 - Cabeza, Sandra A1 - Artzt, Katia A1 - Haubrich, J. A1 - Klaus, M. A1 - Genzel, Ch. A1 - Requena, G. A1 - Bruno, Giovanni T1 - An Assessment of Subsurface Residual Stress Analysis in SLM Ti-6Al-4V N2 - Ti-6Al-4V bridges were additively fabricated by selective laser melting (SLM) under different scanning speed conditions, to compare the effect of process energy density on the residual stress state. Subsurface lattice strain characterization was conducted by means of synchrotron diffraction in energy dispersive mode. High tensile strain gradients were found at the frontal surface for samples in an as-built condition. The geometry of the samples promotes increasing strains towards the pillar of the bridges. We observed that the higher the laser energy density during fabrication, the lower the lattice strains. A relief of lattice strains takes place after heat treatment. KW - Selective laser melting KW - Additive manufacturing KW - Heat treatment KW - Ti-6Al-4V KW - Synchrotron X-ray diffraction KW - Residual stress PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-395759 DO - https://doi.org/10.3390/ma10040348 SN - 1996-1944 VL - 10 IS - 4 SP - Article 348, 1 EP - 14 AN - OPUS4-39575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Obaton, A-F. A1 - Fain, J. A1 - Djemaï, M. A1 - Meinel, Dietmar A1 - Léonard, Fabien A1 - Mahé, E. A1 - Lécuelle, B. A1 - Fouchet, J-J. A1 - Bruno, Giovanni T1 - In vivo XCT bone characterization of lattice structured implants fabricated by additive manufacturing N2 - Several cylindrical specimens and dental implants, presenting diagonal lattice structures with different cell sizes (600, 900 and 1200 µm) were additively manufactured by selective laser melting process. Then they were implanted for two months in a sheep. After removal, they were studied by Archimedes’ method as well as X-ray computed tomography in order to assess the penetration of bone into the lattice. We observed that the additive manufactured parts were geometrically conform to the theoretical specifications. However, several particles were left adhering to the surface of the lattice, thereby partly or entirely obstructing the cells. Nevertheless, bone penetration was clearly visible. We conclude that the 900 µm lattice cell size is more favourable to bone penetration than the 1200 µm lattice cell size, as the bone penetration is 84 % for 900 µm against 54 % for 1200 µm cell structures. The lower bone penetration value for the 1200 µm lattice cell could possibly be attributed to the short residence time in the sheep. Our results lead to the conclusion that lattice implants additively manufactured by selective laser melting enable better bone integration. KW - Biomedical engineering KW - Dentistry KW - Medical imaging KW - X-ray computer tomography PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-418648 DO - https://doi.org/10.1016/j.heliyon.2017.e00374 SN - 2405-8440 IS - 3 SP - Article e00374, 1 EP - 21 PB - Elsevier Limited CY - 125 London Wall London, EC2Y 5AS United Kingdom AN - OPUS4-41864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wollschläger, Nicole A1 - Häusler, Ines A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Palasse, L. A1 - Dirscherl, K. T1 - Characterization of porous, TiO2 nanoparticle films using on-axis TKD in SEM – a new nano-analysis tool for a large-scale application N2 - A combined methodical approach is tested with respect to the characterization of the inner structure of porous TiO2 layers as typically used in modern dye sensitized solar cells (DSSC). Their performance is directly linked to the surface area of the pore network. The micrometer thick layer employed was manufactured by screen-printing of a starting TiO2 powder constituted of shape-controlled, bipyramidal anatase nanoparticles 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). 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 - TiO2 KW - TKD KW - Particle size distribution KW - Nanoparticles KW - Porous film PY - 2017 UR - https://www.cambridge.org/core/services/aop-cambridge-core/content/view/8A8B29335A2F4D0CB6922F6F5A19C5DC/S1431927617003397a.pdf/characterization_of_porous_tio2_nanoparticle_films_using_onaxis_tkd_in_sem_a_new_nanoanalysis_tool_for_a_largescale_application.pdf DO - https://doi.org/10.1017/S1431927617003397 VL - 23 IS - S1 (July) SP - 542 EP - 543 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-41924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rehmer, Birgit A1 - Skrotzki, Birgit A1 - Glaubitz, Steffen T1 - Influence of casting skin on fatigue lifetime of ferritic ductile cast iron N2 - The fatigue behaviour of cast iron is usually investigated on machined specimens. Components of cast iron, however, have a casting skin; therefore the investigation of the influence of the casting skin on the lifetime is of interest. To study this influence isothermal fatigue tests were carried out on heat-resisting spheroidal graphite cast iron EN GJS SiMo 4.05 in 4–point-bending set-up at 400 °C. Specimens with and without casting skin were investigated comparatively. The number of cycles to failure was significantly lower for specimens with casting skin. Metallographic investigations underline the reduction of lifetime caused by casting skin. KW - Cast iron KW - Casting skin KW - Fatigue KW - Lifetime PY - 2017 SN - 0025-5300 VL - 59 IS - 1 SP - 5 EP - 10 PB - Carl Hanser Verlag CY - München AN - OPUS4-38929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stegemann, Robert A1 - Cabeza, Sandra A1 - Lyamkin, V. A1 - Bruno, Giovanni A1 - Pittner, Andreas A1 - Wimpory, Robert A1 - Boin, M. A1 - Kreutzbruck, Marc T1 - Residual stress characterization of steel TIG welds by neutron diffraction and by residual magnetic stray field mappings N2 - The residual stress distribution of tungsten inert gas welded S235JRC+C plates was determined by means of neutron diffraction(ND). Large longitudinal residual stresses with maxima around 600 MPa were found. With these results as reference, the evaluation of residual stress with high spatial resolution GMR (giant magneto resistance) sensors was discussed. The experiments performed indicate a correlation between changes in residual stresses (ND) and the normal component of local residual magnetic stray fields (GMR). Spatial variations in the magnetic field strength perpendicular to the welds are in the order of the magnetic field of the earth. KW - GMR KW - Magnetic stray field KW - Neutron diffraction KW - Residual stress KW - TIG-welding PY - 2017 DO - https://doi.org/10.1016/j.jmmm.2016.11.102 SN - 0304-8853 SN - 1873-4766 VL - 426 SP - 580 EP - 587 PB - Elsevier CY - Amsterdam AN - OPUS4-38678 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 - Klingelhöffer, 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 - Cabeza, Sandra A1 - Mishurova, Tatiana A1 - Garces, G. A1 - Requena, G. A1 - Bruno, Giovanni A1 - Sevostianov, I. T1 - Stress-induced damage evolution in cast AlSi12CuMgNi alloy with one- and two ceramic reinforcements N2 - Two composites, consisting of an as-cast AlSi12CuMgNi alloy reinforced with 15%vol. Al2O3 short fibres and with 7%vol. Al2O3 short fibres + 15%vol. SiC particles were studied. Synchrotron computed tomography disclosed distribution, orientation, and volume fraction of the different phases. In-situ compression tests during neutron diffraction in direction parallel to the fibres plane revealed the load partition between phases. Internal damage (fragmentation) of the Si phase and Al2O3 fibres was directly observed in CT reconstructions. Significant debonding between Al-matrix and SiC particles was also found. Finally, based on the Maxwell scheme, a micro-mechanical model was utilized for the new composite with two ceramic reinforcements; it rationalizes the experimental data, and predicts the evolution of all internal stress components in each phase. KW - Computed tomography KW - Metal matrix composite KW - Load partition KW - Neutron diffraction PY - 2017 DO - https://doi.org/10.1007/s10853-017-1182-7 SN - 0022-2461 SN - 1573-4803 VL - 52 IS - 17 SP - 10198 EP - 10216 PB - Springer AN - OPUS4-40572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shashev, Yury A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Evsevleev, Sergei A1 - Müller, Bernd R. A1 - Osenberg, Markus A1 - Manke, Ingo A1 - Hentschel, Manfred P. A1 - Bruno, Giovanni T1 - Optimizing the visibility of X-ray phase grating interferometry N2 - The performance of grating interferometers coming up now for Imaging interfaces within materials depends on the efficiency (visibility) of their main component, namely the phase grating. Therefore, experiments with monochromatic synchrotron radiation and corresponding simulations are carried out. The visibility of a Phase grating is optimized by different photon energies, varying detector to grating distances and continuous rotation of the phase grating about the grid lines. Such kind of rotation changes the projected grating shapes, and thereby the distribution profiles of phase shifts. This yields higher visibilities than derived from ideal rectangular shapes. By continuous grating rotation and variation of the propagation distance, we achieve 2D visibility maps. Such maps provide the visibility for a certain combination of grating orientation and detector position. Optimum visibilities occur at considerably smaller distances than in the standard setup. KW - Synchrotron, BAMline KW - Talbot-Lau interferometer KW - X-ray imaging KW - X-ray refraction KW - Grating interferometry KW - X-ray phase contrast PY - 2017 DO - https://doi.org/10.3139/120.111097 SN - 0025-5300 VL - 59 IS - 11-12 SP - 974 EP - 980 PB - Hanser Verlag AN - OPUS4-42955 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Lange, Axel A1 - Bruno, Giovanni T1 - Microstructure Characterization of Ceramics via 2D and 3D X-Ray Refraction Techniques N2 - 3D imaging techniques are very fashionable nowadays, and allow enormous progress in understanding ceramic microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this feature article, we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. While the techniques are limited by the X-ray absorption of the material under investigation, we demonstrate showcases of ceramics and composite materials, where understanding of process parameter influence or simply of microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography. KW - X-ray refraction KW - Porosity KW - Specific surface KW - Crack detection KW - Composites PY - 2017 DO - https://doi.org/10.1016/j.jeurceramsoc.2016.12.031 SN - 0955-2219 SN - 1873-619X VL - 37 IS - 5 SP - 1879 EP - 1889 PB - Elsevier CY - Amsterdam AN - OPUS4-39094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Léonard, Fabien A1 - Oesch, Tyler A1 - Meinel, Dietmar A1 - Bruno, Giovanni A1 - Rachmatulin, Natalia A1 - Fontana, Patrick A1 - Sevostianov, I. T1 - Evaluation of fiber orientation in a composite and its effect on material behavior N2 - The reinforcement of concrete with polymer fibers provides resistance to crack formation. The orientation distribution of these fibers has a significant influence on the mechanical behavior of the material. To optimize material performance, micromechanical models that are capable of making accurate predictions of the mechanical behavior of composite materials are needed. These models must be calibrated using experimental results from microstructural characterization. For the fiber orientation distribution analysis in the present study, computed tomography (CT) data were used to evaluate the properties of a fiber-reinforced cement mortar. The results have indicated that the fibers in this material have highly anisotropic orientation characteristics and that there is a clear tendency for the polymer fibers to agglomerate during mixing and casting. The incorporation of this experimental data into micromechanical models will increase the accuracy of those models for material simulation and optimization. T2 - 7th Conference on Industrial Computed Tomography (iCT 2017) CY - Leuven, Belgium DA - 07.02.2017 KW - Orientation distribution KW - Fiber-reinforced concrete KW - Computed tomography PY - 2017 UR - http://www.ndt.net/?id=20818 SN - 1435-4934 VL - 22 IS - 3 SP - 1 EP - 7 PB - NDT.net CY - Kirchwald AN - OPUS4-39338 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosu, Dana-Maria A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Kraehnert, R. A1 - Hertwig, Andreas ED - Hertwig, Andreas ED - Hinrichs, K. ED - Beck, Uwe ED - Esser, N. T1 - Ellipsometric porosimetry on pore-controlled TiO2 layers N2 - The practical performance of surface coatings in applications like catalysis, water splitting or batteries depends critically on the coating materials’ porosity. Determining the porosity in a fast and nondestructive way is still an unsolved problem for industrial thin-films technology. As a contribution to calibrated, non-destructive, optical layer characterisation, we present a multi-method comparison study on porous TiO2 films deposited by sol-gel synthesis on Si wafers. The ellipsometric data were collected on a range of samples with different TiO2 layer thickness and different porosity values. These samples were produced by templated sol-gel synthesis resulting in layers with a well-defined pore size and pore density. The ellipsometry measurement data were analysed by means of a Bruggeman effective medium approximation (BEMA), with the aim to determine the mixture ratio of void and matrix material by a multi-sample analysis strategy. This analysis yielded porosities and layer thicknesses for all samples as well as the dielectric function for the matrix material. Following the idea of multi-method techniques in metrology, the data was referenced to imaging by electron microscopy (SEM) and to a new EPMA (electron probe microanalysis) porosity approach for thin film analysis. This work might lead to a better metrological understanding of optical porosimetry and also to better-qualified characterisation methods for nano-porous layer systems. 1. IntroductionPorous materials, especially porous thin films play an importantrole in chemical and physical technology in every case where thecontact area between two media has to be maximised. From cataly-sis to photochemistry and photovoltaics, the applications of porouslayer materials are diverse and numerous [1–6].The accurate and non-destructive characterisation of porousfilms for layered systems poses a challenge. This applies especiallyfor the key parameter of porous films, their porosity, i.e. the mix-ing ratio between the Matrix of the film (host material) and thepore volume which is empty or filled with a fluid medium (inclu-sions). This parameter influences most of the physical and chemicalproperties of a porous thin film and is therefore essential for theunderstanding as well as the optimisation of this class of materials. T2 - International Conference on Spectroscopic Ellipsometry (ICSE-7) CY - Berlin, Germany DA - 06.06.2016 KW - Spectroscopic ellipsometry KW - Porous materials KW - Porosimetry KW - Multi-sample analysis KW - Thin film metrology PY - 2017 DO - https://doi.org/10.1016/j.apsusc.2016.11.055 SN - 0169-4332 SN - 1873-5584 VL - 421 IS - Part B SP - 487 EP - 493 PB - Elsevier B.V. AN - OPUS4-42517 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 - Mieller, Björn A1 - Rabe, Torsten A1 - Rangelov, V. T1 - In situ shrinkage measurement during pressure-assisted sintering of low temperature co-fired ceramic panels N2 - Shrinkage measurements of miniaturized low temperature co-fired ceramics (LTCC) samples under load typically lead to collapsing of the samples, which hampers the characterization of shrinkage up to full densification. In this paper, a measurement setup is presented, which allows for in situ shrinkage measurements of practical, large LTCC panels during pressure-assisted sintering in a sintering press. The shrinkage behavior of two commercial LTCC systems (GreenTape 951 and Ceramtape GC) has been measured under loads of up to 1 MPa. No crushing of the specimens was observed and reproducible characterization of shrinkage up to full densification has been performed. Based on comparisons to thermomechanical analyzer measurements in this and other studies, it was found that the in situ approach is much better suited for shrinkage characterization of LTCC under load. Reproducibility and accuracy of the method are discussed and practical as well as more academic applications are proposed. KW - Shrinkage KW - Low temperature KW - Sinter/sintering PY - 2017 DO - https://doi.org/10.1111/ijac.12634 SN - 1546-542X SN - 1744-7402 VL - 14 IS - 2 SP - 245 EP - 251 AN - OPUS4-39327 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wessig, P. A1 - Schulze, T. A1 - Pfennig, A. A1 - Weidner, Steffen A1 - Prentzel, S. A1 - Schlaad, H. T1 - Thiol–ene polymerization of oligospiroketal rods N2 - The nucleophilic thiol–ene (thia-Michael) reaction between molecular rods bearing terminal thiols and bis-maleimides was investigated. The molecular rods have oligospiroketal (OSK) and oligospirothioketal (OSTK) backbones. Contrary to the expectations, cyclic oligomers were always obtained instead of linear rigid-rod polymers. Replacing the OS(T)K rods with a flexible chain yielded polymeric products, suggesting that the OS(T)K structure is responsible for the formation of cyclic products. The reason for the preferred formation of cyclic products is due to the presence of folded conformations, which have already been described for articulated rods. KW - Oligospiroketals KW - Polymerization KW - MALDI-TOF MS PY - 2017 DO - https://doi.org/10.1039/C7PY01569K SN - 1759-9954 SN - 1759-9962 VL - 8 IS - 44 SP - 6879 EP - 6885 PB - Royal Society of Chemistry AN - OPUS4-42685 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lauer, Franziska A1 - Seifert, Stephan A1 - Kneipp, Janina A1 - Weidner, Steffen T1 - Simplifying the preparation of pollen grains for MALDI-TOF MS classification N2 - Matrix-assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF MS) is a well-implemented analytical technique for the investigation of complex biological samples. In MS, the sample preparation strategy is decisive for the success of the measurements. Here, sample preparation processes and target materials for the investigation of different pollen grains are compared. A reduced and optimized sample preparation process prior to MALDI-TOF measurement is presented using conductive carbon tape as target. The application of conductive tape yields in enhanced absolute signal intensities and mass spectral pattern information, which leads to a clear separation in subsequent pattern analysis. The results will be used to improve the taxonomic differentiation and identification, and might be useful for the development of a simple routine method to identify pollen based on mass spectrometry. KW - MALDI KW - Conductive carbon tape KW - Pollen KW - Sample pretreatment KW - Principal component analysis PY - 2017 DO - https://doi.org/10.3390/ijms18030543 SN - 1422-0067 SN - 1661-6596 VL - 18 IS - 3 SP - 543-1 EP - 543-11 PB - MDPI AN - OPUS4-41733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lüchtenborg, Jörg A1 - Mühler, T. A1 - Léonard, Fabien A1 - Günster, Jens T1 - Laser-induced slip casting (LIS) – a new additive manufacturing process for dense ceramics demonstrated with Si3N4 N2 - Up to now, there exists a lack of methods for the additive manufacturing of voluminous ceramic parts with properties comparable to those of conventionally manufactured ones. A high density after sintering is needed to reach the superior properties of ceramic materials. We have developed a new additive manufacturing method, Laser-Induced Slip casting (LIS), to generate ceramic green bodies with high particle packing density and with virtually no restriction in the particle size of the feedstock, especially in terms of small particles. This is achieved by laser-induced local drying of slurries, with the process resembling many features of the well-established stereolithography, but without the excessive use of polymeric material. Thus, unlike the stereolithography process, the resulting green bodies can be processed like traditionally produced ceramic parts. This method allows large and dense additive-manufactured parts to be obtained from conventional water-based ceramic slurries. As an example, we will demonstrate the application of this novel technique with Si3N4. KW - Additive manufacturing KW - Ceramics PY - 2017 DO - https://doi.org/10.4416/JCST2017-00091 SN - 2190-9385 VL - 8 IS - 4 SP - 531 EP - 540 PB - Göller Verlag CY - Baden-Baden AN - OPUS4-43738 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 - Maenz, S. A1 - Brinkmann, O. A1 - Kunisch, E. A1 - Horbert, V. A1 - Gunella, F. A1 - Bischoff, S. A1 - Schubert, H. A1 - Sachse, A. A1 - Xin, L. A1 - Günster, Jens A1 - Illerhaus, Bernhard A1 - Jandt, K. D. A1 - Bossert, J. A1 - Kinne, R. W. A1 - Bungartz, M. T1 - Enhanced bone formation in sheep vertebral bodies after minimally invasive treatment with a novel, PLGA fiber-reinforced brushite cement. N2 - Injectable, brushite-forming calcium phosphate cements (CPC) show potential for bone replacement, but they exhibit low mechanical strength. This study tested a CPC reinforced with poly(l-lactide-co-glycolide) acid (PLGA) fibers in a minimally invasive, sheep lumbar vertebroplasty model. The study aimed to test the in vivo biocompatibility and osteogenic potential of a PLGA fiber-reinforced, brushite-forming CPC in a sheep large animal model. KW - µCT KW - Vertebral KW - PLGA cement PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S152994301631066X DO - https://doi.org/10.1016/j.spinee.2016.11.006 SN - 1529-9430 SN - 1878-1632 VL - 17 IS - 5 SP - 709 EP - 719 PB - Elsevier Science direct AN - OPUS4-40462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sun, C. A1 - Tian, X. A1 - Wang, L. A1 - Liu, Y. A1 - Wirth, Cynthia A1 - Günster, Jens A1 - Li, D. A1 - Jin, Z. T1 - Effect of particle size gradation on the performance of glass-ceramic 3D printing process N2 - Particle size gradation is regarded as an effective method for overcoming the contradicting requirements in three-dimensional printing (3DP). In present work, particle size gradation was optimized to obtain both acceptable flowability of the powder material and high-strength 3D-printed glass-ceramic products. The effect of gradation on the printing process, sintering process and performance of the 3D-printed glass-ceramic products was investigated comprehensively. The glass-ceramic powders with three size ranges were mixed in certain proportions and applied to print parts. The result showed parts printed with powder mixed by 60 wt% 45–100 µm and 40 wt% 0–25 µm particles had satisfactory density of 1.60 g/cm³ and bending strength of 13.8 MPa. The flowability decreased with an increasing proportion of fine particles. Part density was determined by the powder bulk density in the powder bed as well as the shrinkage during sintering while strength of part was found to be dependent on the sintering degree. KW - Flowability KW - Glass-ceramic KW - Particle size gradation KW - Three-dimensional printing KW - Mechanical properties PY - 2017 DO - https://doi.org/10.1016/j.ceramint.2016.09.197 SN - 0272-8842 VL - 43 IS - 1 SP - 578 EP - 584 PB - Elsevier AN - OPUS4-39783 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Colombo, P. A1 - Schmidt, J. A1 - Franchin, G. A1 - Zocca, Andrea A1 - Günster, Jens T1 - Additive manufacturing techniques for fabricating complex ceramic components from preceramic polymers N2 - Capsule summary THE MATERIALS Manufacturers can use preceramic polymers to produce ceramic components in a range of compositions using a variety of additive manufacturing technologies. Preceramic polymers even can overcome some of the problems that are intrinsic to additive manufacturing in general. THE APPLICATION Modifying the composition, molecular architecture, and molecular weight of preceramic polymers allows adaptation of these materials to specific processing requirements of individual additive manufacturing technologies. THE OPPORTUNITY Further development of new additive manufacturing technologies, in addition to improvement of existing technologies, will enable manufacturing of advanced ceramic components with enhanced mechanical characteristics and new functional properties. KW - Additive manufacturing KW - Preceramic polymers PY - 2017 VL - 96 IS - 3 SP - 16 EP - 23 AN - OPUS4-40747 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 - Schmidt, Wolfram A1 - Brouwers, H.J.H. A1 - Kühne, Hans-Carsten A1 - Meng, Birgit T1 - Interactions of polysaccharide stabilising agents with early cement hydration without and in the presence of superplasticizers N2 - Polysaccharides are incorporated into cement based Systems in order to modify the rheological properties. Typically, cellulose ethers, sphingan gums, guar gum or starch ethers are applied. Depending upon their chemistry, molecular architecture, and adsorption tendency, polysaccharides interact differently with the entire cementitious system. Some stabilising agents like diutan gum mainly affect the cementitious paste; other stabilising agents like starch tend to interact with the sand fraction and even with the coarse aggregates. Cellulose and guar gum shows more diverse performances. Typically stabilising admixtures like polysaccharides are used, when sophisticated rheological properties are adjusted. Therefore, polysaccharides are often used in combination with superplasticisers, which are added to reduce the yield stress of concrete. This can cause interactions, particularly when the stabilising Agent shows a strong tendency to adsorb on particle surfaces. Adsorptive stabilising agents may reduce the amount of adsorbed superplasticisers, thus affecting both viscosity and yield stress, while non-adsorptive stabilising agents mainly affect the plastic viscosity independently of the superplasticiser. Due to the strong influence of superplasticisers on the yield stress, influences of the stabilising agent on the yield stress retreat into the background, so that their major effect is an increase of the plastic viscosity. The paper provides a comprehensive overview of how different polysaccharide superplasticisers affect cementitious flowable systems and points out the challenges of the combined use of polysaccharides and superplasticisers. Based on rheometric experiments and observations of the hydration process, time dependent effects on the workability as well as of the hydration of cement are presented and discussed. KW - Concrete KW - Polysaccharides KW - Rheology KW - Stabilising agents KW - Starch KW - Sphingan PY - 2017 DO - https://doi.org/10.1016/j.conbuildmat.2016.11.022 SN - 0950-0618 SN - 1879-0526 VL - 139 SP - 584 EP - 593 PB - Elsevier AN - OPUS4-40597 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 - Homberg, U. A1 - Baum, D. A1 - Prohaska, S. A1 - Günster, Jens A1 - Krauss-Schüler, Stefanie T1 - Adapting trabecular structures for 3D printing: an image processing approach based on μCT data N2 - Materials with a trabecular structure notably Combine advantages such as lightweight, reasonable strength, and permeability for fl uids. This combination of advantages is especially interesting for tissue engineering in trauma surgery and orthopedics. Bone-substituting scaffolds for instance are designed with a trabecular structure in order to allow cell migration for bone ingrowth and vascularization. An emerging and recently very popular technology to produce such complex, porous structures is 3D printing. However, several technological aspects regarding the scaffold architecture, the printable resolution, and the feature size have to be considered when fabricating scaffolds for bone tissue replacement and regeneration. Here, we present a strategy to assess and prepare realistic trabecular structures for 3D printing using image analysis with the aim of preserving the structural elements. We discuss critical conditions of the printing system and present a 3-stage approach to adapt a trabecular structure from μ CT data while incorporating knowledge about the printing system. In the first stage, an image-based extraction of solid and void structures is performed, which results in voxel- and graph-based representations of the extracted structures. These representations not only allow us to quantify geometrical properties such as pore size or strut geometry and length. But, since the graph represents the geometry and the topology of the initial structure, it can be used in the second stage to modify and adjust feature size, volume and sample size in an easy and consistent way. In the final reconstruction stage, the graph is then converted into a voxel representation preserving the topology of the initial structure. This stage generates a model with respect to the printing conditions to ensure a stable and controlled voxel placement during the printing process. KW - Additive manufacturing, 3D printing KW - Trabecular structures KW - Image-based analysis PY - 2017 DO - https://doi.org/10.1088/2057-1976/aa7611 SN - 2057-1976 VL - 3 IS - 3 SP - Article 035027, 1 EP - 14 PB - IOP Publishing Ltd AN - OPUS4-40744 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -