TY - JOUR A1 - Schaupp, Thomas A1 - Schröpfer, Dirk A1 - Kromm, Arne A1 - Kannengießer, Thomas T1 - Welding residual stresses in 960 MPa grade QT and TMCP high-strength steels N2 - High-strength steels with yield strengths ≥ 690 MPa are becoming increasingly significant for modern steel constructions. Both quenched and tempered (QT) high-strength steels and steels produced by the thermo-mechanically controlled process (TMCP) are currently available. TMCP-steels are usually provided with a typical mill scale. Apart from the manufacturing process these steels differ also in their chemical composition. The influence of these differences are investigated here with focus on the residual stresses formed during TIG welding. Bead on plate welds have shown characteristic residual stress distributions depending on the type of steel as well as on the heat input and preheat temperature. The following work demonstrates that the fluid flow, induced by the elements present in the mill scale, leads to a deeper penetration of the material. This can also lead to increased residual stresses in the surface of the weld and the HAZ. Furthermore, higher heat input and preheat temperature can induce higher tensile residual stresses − which are evident in the present study. KW - Residual stresses KW - High-strength steel KW - Welding KW - Mill scale KW - Phase transformation PY - 2017 DO - https://doi.org/10.1016/j.jmapro.2017.05.006 SN - 1526-6125 VL - 27 SP - 226 EP - 232 PB - ELSEVIER AN - OPUS4-40312 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steppan, Enrico A1 - Mantzke, Philipp A1 - Steffens, Benjamin A1 - Rhode, Michael A1 - Kannengießer, Thomas T1 - Thermal desorption analysis for hydrogen trapping in microalloyed high-strength steels N2 - Hydrogen can have an extreme degradation effects in steels, particularly concerning the mechanical properties. These effects can lead to hydrogen-assisted cracking in microalloyed high-strength steels during fabrication and/or operation in industrial applications. In order to study these effects, electrochemically charged tensile specimens were tested to elucidate the degradation of their properties. The carrier gas hot extraction (CGHE) method, which functionally combines a mass spectrometer with a thermal desorption analysis (TDA) process, was used for the detection of ultra-low diffusible hydrogen concentrations in the material specimens. The mass spectrometer provided rapid and automatic determination of hydrogen concentration, whereas the TDA presented the activation energy within the respective test specimen at the specific temperature. Additionally, specimen temperature was carefully monitored to reduce the evaluation error for local effusion peaks. A quenching and deformation dilatometer was used for the analysis of typical heat-affected zones during the welding process for a high reproducibility of the homogenous microstructures that were studied. The present work shows the interaction between hydrogen and lattice defects in different microalloyed materials and heat-affected zones of weldable fine-grained steels. These steels were prepared in a quenched and tempered condition and in a thermo-mechanically rolled condition. These preparations were made according to German standard DIN EN 10025-6 and to DIN EN 10149-2, respectively. The trapping characteristics of two steel grades, S690QL and S700MC, were studied with respect to the activation energy dependent on carbon content and microalloying elements such as Ti, Nb, Mo, Cr, and V. The two steel grades exhibited several types of traps: carbide formations, dislocations, and/or grain boundaries were common, which can influence activation energy and hydrogen solubility. The type and dimension of inclusions or particles also affected the hydrogen trapping behavior. A decrease of carbon and specific alloying elements in thermo-mechanically hot rolled steels led to a change in the activation energy binding the trapped hydrogen. This thermo-mechanically hot rolled steel revealed an increased interaction between hydrogen and precipitations. The higher carbon content in the quenched and tempered steel led to a higher interaction between hydrogen and iron carbide, specifically in the martensitic phase. Furthermore, the trapping behavior in heat-affected zones showed a significant increase in activation energy, especially in the coarse-grained microstructure. These previously mentioned various effects were studied to better understand the degradation of mechanical properties in these two steels. KW - Microalloyed steels KW - Hydrogen embrittlement KW - Heating KW - Chemical analysis KW - Microstructure KW - Heat-affected zone PY - 2017 DO - https://doi.org/10.1007/s40194-017-0451-z SN - 0043-2288 SN - 1878-6669 VL - 61 IS - 4 SP - 637 EP - 648 PB - Springer CY - Berlin Heidelberg AN - OPUS4-40190 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - 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 - 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 - 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 - 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 - 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 - 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 - 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 - 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 - 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 - 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 - Adel-Khattab, D. A1 - Giacomini, F. A1 - Gildenhaar, R. A1 - Berger, G. A1 - Gomes, Cynthia A1 - Linow, Ulf A1 - Hardt, M. A1 - Peleska, B. A1 - Günster, Jens A1 - Stiller, M. A1 - Houshmand, A. A1 - Ghaffar, K. A1 - Gamal, A. A1 - El-Mofty, M. A1 - Knabe, C. T1 - Development of a synthetic tissue engineered three- dimensional printed bioceramic-based bone graft with homogenously distributed osteoblasts and mineralizing bone matrix in vitro N2 - Over the last decade there have been increasing efforts to develop three-dimensional (3D) scaffolds for bone tissue Engineering from bioactive ceramics with 3D printing emerging as a promising technology. The overall objective of the present study was to generate a tissue engineered synthetic bone graft with homogenously distributed osteoblasts and mineralizing bone Matrix in vitro, thereby mimicking the advantageous properties of autogenous bone grafts and facilitating usage for reconstructing segmental discontinuity defects in vivo . To this end, 3D scaffolds were developed from a silica-containing calcium alkali orthophosphate, using, fi rst, a replica technique – the Schwartzwalder – Somers method – and, second, 3D printing, (i.e. rapid prototyping). The mechanical and physical scaffold properties and their potential to facilitate homogenous colonization by osteogenic cells and extracellular bone matrix formation throughout the porous scaffold architecture were examined. Osteoblastic cells were dynamically cultured for 7 days on both scaffold types with two different concentrations of 1.5 and 3 × 10⁹ cells/l. The amount of cells and bone matrix formed and osteogenic marker expression were evaluated using hard tissue histology, immunohistochemical and histomorphometric analysis. 3D-printed scaffolds (RPS) exhibited more micropores, greater compressive strength and silica release. RPS seeded with 3 × 10⁹ cells/l displayed greatest cell and extracellular Matrix formation, mineralization and osteocalcin expression. In conclusion, RPS displayed superior mechanical and biological properties and facilitated generating a tissue engineered synthetic bone graft in vitro, which mimics the advantageous properties of autogenous bone grafts, by containing homogenously distributed terminally differentiated osteoblasts and mineralizing bone matrix and therefore is suitable for subsequent in vivo implantation for regenerating segmental discontinuity bone defects. KW - Bone tissue engineering KW - Calcium alkali orthophosphate KW - Rapid prototyping KW - Scaffold KW - Mandible PY - 2017 DO - https://doi.org/10.1002/term.2362 SN - 1932-6254 SN - 1932-7005 VL - 12 IS - 1 SP - 44 EP - 58 PB - Wiley Online Library AN - OPUS4-40745 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Erdmann, Maren A1 - Trappe, Volker A1 - Sturm, Heinz A1 - Braun, Ulrike A1 - Dümichen, Erik T1 - Cure conversion of structural epoxies by cure state analysis and in situ cure kinetics using nondestructive NIR spectroscopy N2 - Non-isothermal heating rate kinetics was applied to two epoxy resin systems. In situ near-infrared (NIR) measurements were taken with a heatable NIR cell which allowed the cure to be monitored by characteristic absorption bands. An autocatalyzed reaction of the nth order was shown to describe the epoxy conversion curves. Differential Scanning Calorimetry (DSC) was used as a complementary method. The kinetic models developed by both NIR and DSC are in good accordance with experimental epoxy conversion in the in situ NIR setup for single and multiple cure temperature ramps. A linear calibration curve of the characteristic absorption bands of epoxy normalized to aromatic vibrations was introduced. The curing degree of structural epoxies that were cured according to an industrial temperature cure profile was determined by NIR using the calibration curve. The epoxy conversions of the structural components showed good agreement with the experimental in situ NIR. Several degrees of cure for structural specimens were evaluated by NIR and residual reaction enthalpy by DSC. We present the non-destructive NIR spectroscopy as an alternative to determine fast and non-destructive epoxy conversion, particularly suitable for high degrees of cure on structural components. KW - Epoxy resin KW - Curing kinetics KW - In situ near-infrared (NIR) spectroscopy KW - Differential scanning calorimetry (DSC) PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S0040603117300205 DO - https://doi.org/10.1016/j.tca.2017.01.010 SN - 0040-6031 SN - 1872-762X VL - 650 SP - 8 EP - 17 PB - Elsevier B.V. AN - OPUS4-39123 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zocca, Andrea A1 - Lima, Pedro A1 - Günster, Jens T1 - LSD-based 3D printing of alumina ceramics N2 - An improved method of powder 3D printing leading to dense ceramic parts is presented. The application of powder-based binder jetting 3D printing technologies to technical ceramics is generally limited by the low packing density of the powder and by the need to use a flowable powder. With layer-wise slurry deposition, it is, however, possible to deposit powder beds with high particle packing and furthermore using submicron powders. This method was combined with the binder jetting technology to develop a novel process, named LSD-print. By means of LSD-print, a submicron Al2O3 powder could be processed to produce samples with a density comparable with that of standard pressed samples, both in the green state and after sintering. KW - Additive manufacturing KW - Layer-wise slurry deposition KW - Dense alumina KW - 3D printing PY - 2017 DO - https://doi.org/10.4416/JCST2016-00103 SN - 2190-9385 VL - 8 IS - 1, SI SP - 141 EP - 147 PB - Göller Verlag GmbH CY - Baden Baden AN - OPUS4-39672 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Kricheldorf, H. R. T1 - The Role of Transesterification in SnOct 2 - Catalyzed Polymerizations of Lactides N2 - l-lactide or meso-lactide are polymerized either at 120 °C where the polymerization process of l-lactide is accompanied by crystallization, or at 180 °C where poly(l-lactide) remains in the molten state. Polymerizations at 120 °C initially yield even-numbered chains (with respect to lactic acid units) having relatively low dispersity, but the fraction of odd-numbered chains increases with time and the entire molecular weight distribution changes. Traces of cyclics are only formed after 7 d. Polymerizations at 180 °C yield equilibrium of even and odd-numbered chains from the beginning, but at low monomer/initiator ratios and short reaction times (<4 h) cyclics are again not formed. They appear at longer reaction times and entail higher dispersities. The results are discussed in terms of five different transesterification mechanisms. KW - Polylactides KW - MALDI KW - Transesterification KW - Sn catalysts PY - 2017 DO - https://doi.org/10.1002/macp.201600331 SN - 1022-1352 VL - 218 IS - 3 SP - 1600331 PB - Wiley AN - OPUS4-39753 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kirner, Sabrina A1 - Wirth, Thomas A1 - Sturm, Heinz A1 - Krüger, Jörg A1 - Bonse, Jörn T1 - Nanometer-resolved chemical analyses of femtosecond laser-induced periodic surface structures on titanium N2 - The chemical characteristics of two different types of laser-induced periodic surface structures (LIPSS), so-called high and low spatial frequency LIPSS (HSFL and LSFL), formed upon irradiation of titanium surfaces by multiple femtosecond laser pulses in air (30 fs, 790 nm, 1 kHz), are analyzed by various optical and electron beam based surface analytical techniques, including micro-Raman spectroscopy, energy dispersive X-ray analysis, X-ray photoelectron spectroscopy, and Auger electron spectroscopy. The latter method was employed in a high-resolution mode being capable of spatially resolving even the smallest HSFL structures featuring spatial periods below 100 nm. In combination with an ion sputtering technique, depths-resolved chemical information of superficial oxidation processes was obtained, revealing characteristic differences between the two different types of LIPSS. Our results indicate that a few tens of nanometer shallow HSFL are formed on top of a ∼150 nm thick graded superficial oxide layer without sharp interfaces, consisting of amorphous TiO2 and partially crystallized Ti2O3. The larger LSFL structures with periods close to the irradiation wavelength originate from the laser-interaction with metallic titanium. They are covered by a ∼200 nm thick amorphous oxide layer, which consists mainly of TiO2 (at the surface) and other titanium oxide species of lower oxidation states underneath. KW - Laser-induced periodic surface structures (LIPSS) KW - Femtosecond laser KW - Oxidation KW - Titanium KW - Auger electron spectroscopy PY - 2017 DO - https://doi.org/10.1063/1.4993128 SN - 0021-8979 VL - 122 IS - 10 SP - 104901, 1 EP - 9 PB - AIP Publishing CY - Melville, NY, USA AN - OPUS4-41905 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 - Breitenbach, Romy A1 - Silbernagl, Dorothee A1 - Toepel, J. A1 - Sturm, Heinz A1 - Broughton, William J. A1 - Sassaki, G. L. A1 - Gorbushina, Anna T1 - Corrosive extracellular polysaccharides of the rock-inhabiting model fungus Knufia petricola N2 - Melanised cell walls and extracellular polymeric matrices protect rock-inhabiting microcolonial fungi from hostile environmental conditions. How extracellular polymeric substances (EPS) perform this protective role was investigated by following development of the model microcolonial black fungus Knufia petricola A95 grown as a sub-aerial biofilm. Extracellular substances were extracted with NaOH/formaldehyde and the structures of two excreted polymers studied by methylation as well as NMR analyses. The main polysaccharide (~ 80%) was pullulan, also known as α-1,4-; α-1,6-glucan, with different degrees of polymerisation. Αlpha-(1,4)-linked-Glcp and α-(1,6)-linked-Glcp were present in the molar ratios of 2:1. A branched galactofuromannan with an α-(1,2)-linked Manp main chain and a β-(1,6)-linked Galf side chain formed a minor fraction (~ 20%). To further understand the roles of EPS in the weathering of minerals and rocks, viscosity along with corrosive properties were studied using atomic force microscopy (AFM). The kinetic viscosity of extracellular K. petricola A95 polysaccharides (≈ 0.97 × 10-6 m2 s-1) ranged from the equivalent of 2% (w/v) to 5% glycerine, and could thus profoundly affect diffusion-dominated processes. The corrosive nature of rock-inhabiting fungal EPS was also demonstrated by its effects on the aluminium coating of the AFM cantilever and the silicon layer below. KW - Corrosion KW - EPS KW - Melanised microcolonial fungi (MCF) KW - Pullulan KW - Sub-aerial biofilms (SAB) KW - α-1,4- and α-1,6-glucans KW - AFM cantilever vibration KW - Nanoviscosity KW - Nanocorrosion of aluminium and silicon PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-435910 DO - https://doi.org/10.1007/s00792-017-0984-5 SN - 1433-4909 SN - 1431-0651 VL - 22 IS - 2 SP - 165 EP - 175 PB - Springer CY - Berlin AN - OPUS4-43591 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröter, Maria-Astrid A1 - Meyer, Susann A1 - Hahn, Marc Benjamin A1 - Solomun, Tihomir A1 - Sturm, Heinz A1 - Kunte, Hans-Jörg T1 - Ectoine protects DNA from damage by ionizing radiation N2 - Ectoine plays an important role in protecting biomolecules and entire cells against environmental stressors such as salinity, freezing, drying and high temperatures. Recent studies revealed that ectoine also provides effective protection for human skin cells from damage caused by UV-A radiation. These protective properties make ectoine a valuable compound and it is applied as an active ingredient in numerous pharmaceutical devices and cosmetics. Interestingly, the underlying mechanism resulting in protecting cells from radiation is not yet fully understood. Here we present a study on ectoine and its protective influence on DNA during electron irradiation. Applying gel electrophoresis and atomic force microscopy, we demonstrate for the first time that ectoine prevents DNA strand breaks caused by ionizing electron radiation. The results presented here point to future applications of ectoine for instance in cancer radiation therapy. KW - Plasmid DNA pUC19 KW - Electron irradiation 30 [kV] KW - Effective irradiation dose 0.2-16 [Gy] KW - Gel electrophoresis KW - AFM intermittent contact KW - Radioprotector ectoine KW - Compatible solute PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-428287 DO - https://doi.org/10.1038/s41598-017-15512-4 SN - 2045-2322 VL - 7 IS - 1 SP - 15272, 1 EP - 15272, 7 PB - Nature AN - OPUS4-42828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zeegers, G. P. A1 - Steinhoff, R. F. A1 - Weidner, Steffen A1 - Zenobi, R. T1 - Evidence for laser-induced redox reactions in matrix-assisted laserdesorption/ionization between cationizing agents and target plate material: a study with polystyrene and trifluoroacetate salts N2 - Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is often applied to assess the dispersity and the end groups of synthetic polymers through the addition of cationizing agents. Here weaddress how these cation adducts are formed using polystyrene (PS) as a model polymer. We analyzed PSby MALDI-MS with a 2-[(2E)-3-(4-tert-butylphenyl)-2-methylprop-2-enylidene]malononitrile (DCTB) as the matrix and a range of trifluoroacetate (TFA) salts as cationizing agents on a range of different targetplate materials (copper, 1.4301 stainless steel, aluminum, Inconel 625, Ti90/Al6/V4 and chromium-, gold-and silver-plated stainless steel). It was found that on a stainless steel substrate the metal cations Al+,Li+, Na+, Cu+and Ag+formed polystyrene adducts, whereas K+, Cs+, Ba2+, Cr3+, Pd2+, In3+, or their lower oxidation states, did not. For the copper and silver substrates, PS and DCTB adduct formation with cations liberated from these target plate materials was observed upon addition of a cationizing agent, which indicates the occurrence of redox reactions between the added TFA salts and the target plate material. Judging from their standard electrode potentials, these redox reactions would not normally occur, i.e.,they require an additional energy input, strongly suggesting that the observed redox reactions are laser-induced. Furthermore, copper granules were found to successfully sequester PS from a tetrahydrofuran(THF) solution, consistent with the view complex formation with the copper target plate can take place prior to the MALDI-MS measurement. KW - Polymer MALDI KW - Cationization KW - Polystyrene KW - Laser-induced redox reactions KW - Target plate material PY - 2017 DO - https://doi.org/10.1016/j.ijms.2016.10.007 SN - 1387-3806 SN - 1873-2798 VL - 416 SP - 80 EP - 89 PB - Elsevier B.V. AN - OPUS4-41146 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -