TY - JOUR A1 - Stein, L. A1 - Wang, Cui A1 - Förster, C. A1 - Resch-Genger, Ute A1 - Heinze, K. T1 - Bulky ligands protect molecular ruby from oxygen quenching N2 - Chromium(III) complexes can show phosphorescence from the spin-flip excited doublet states 2E/2T1 in the near-infrared with high photoluminescence quantum yields and extremely long lifetimes in the absence of dioxygen. The prototype molecular ruby, [Cr(ddpd)2]3+ (ddpd = N,N’-dimethyl-N,N’-dipyridine-2-ylpyridine-2,6-diamine), has a photoluminescence quantum yield and a luminescence lifetime of 13.7% and 1.1 ms in deaerated acetonitrile, respectively. However, its luminescence is strongly quenched by 3O2 via an efficient Dexter-type energy transfer process. To enable luminescence applications of molecular rubies in solution under aerobic conditions, we explored the potential of sterically demanding ddpd ligands to shield the chromium(III) center from O2 using steady state and time-resolved photoluminescence spectroscopy. The structures of the novel complexes with sterically demanding ligands were investigated by single crystal X-ray diffraction and quantum chemically by density functional theory calculations. The O2 sensitivity of the photoluminescence was derived from absolutely measured photoluminescence quantum yields and excited state lifetimes under inert and aerobic conditions and by Stern–Volmer analyses of these data. Optimal sterically shielded chromium(III) complexes revealed photoluminescence quantum yields of up to 5.1% and excited state lifetimes of 518 μs in air-saturated acetonitrile, underlining the large potential of this ligand design approach to broaden the applicability of highly emissive chromium(III) complexes. KW - Fluorescence KW - Synthesis KW - Production KW - Optical spectroscopy KW - Ligand KW - Photophysics KW - Cr(III) KW - Mechanism KW - NIR KW - Sensor KW - Oxygen PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570807 DO - https://doi.org/10.1039/d2dt02950b VL - 51 IS - 46 SP - 17664 EP - 17670 PB - The Royal Society of Chemistry CY - Berlin AN - OPUS4-57080 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epping, Ruben A1 - Koch, Matthias T1 - On-Site Detection of Volatile Organic Compounds (VOCs) N2 - Volatile organic compounds (VOCs) are of interest in many different fields. Among them are food and fragrance analysis, environmental and atmospheric research, industrial applications, security or medical and life science. In the past, the characterization of these compounds was mostly performed via sample collection and off-site analysis with gas chromatography coupled to mass spectrometry (GC-MS) as the gold standard. While powerful, this method also has several drawbacks such as being slow, expensive, and demanding on the user. For decades, intense research has been dedicated to find methods for fast VOC analysis on-site with time and spatial resolution. We present the working principles of the most important, utilized, and researched technologies for this purpose and highlight important publications from the last five years. In this overview, non-selective gas sensors, electronic noses, spectroscopic methods, miniaturized gas chromatography, ion mobility spectrometry and direct injection mass spectrometry are covered. The advantages and limitations of the different methods are compared. Finally, we give our outlook into the future progression of this field of research. KW - Volatile organic compounds KW - On-site detection KW - Mobile analytics KW - Sensors PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570885 DO - https://doi.org/10.3390/molecules28041598 VL - 28 IS - 4 SP - 1 EP - 19 PB - MDPI CY - Basel, Switzerland AN - OPUS4-57088 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nehring, Grzegorz A1 - Girard, Solène A1 - Rabin, Ira T1 - Conservation and Technical Evaluation of an Early Medieval Papyrus Codex N2 - In 2005, a team of Polish archaeologists discovered three Coptic codices, two on papyrus and one on parchment, in the rubbish dump of a hermitage at Sheik Abd el-Gurna, Egypt. While the parchment codex and the remains of the bindings of the papyrus ones have been conserved, the text blocks of the papyrus codices were opened and disassembled and after being disinfected remained untouched for nearly 15 years, until the current project started. Currently, all three books are stored in the collection of the Coptic Museum in Cairo. Our team undertook the conservation of and archaeometric research on the papyrus codices. The first of the books contains the Canons of Pseudo-Basil, while the second is an Encomium of St. Pisenthios. Both codices have been palaeographically dated to the seventh-eighth centuries CE. In this paper, we describe our project and present the results of the work carried out on the Canons of Pseudo-Basil. Our work involved photography in transmitted light, measurements of the thickness of the papyrus leaves, and digital microscopy under three-light illumination. These measurements allowed us to determine the types of the inks and characterize the papyrus writing substrate. For conservation, we used a novel method developed in the Egyptian Museum in Berlin that comprises suspending papyrus folios on a translucent, extremely thin Japanese paper inside glass frames without the use of adhesives.In 2005, a team of Polish archaeologists discovered three Coptic codices, two on papyrus and one on parchment, in the rubbish dump of a hermitage at Sheik Abd el-Gurna, Egypt. While the parchment codex and the remains of the bindings of the papyrus ones have been conserved, the text blocks of the papyrus codices were opened and disassembled and after being disinfected remained untouched for nearly 15 years, until the current project started. Currently, all three books are stored in the collection of the Coptic Museum in Cairo. Our team undertook the conservation of and archaeometric research on the papyrus codices. The first of the books contains the Canons of Pseudo-Basil, while the second is an Encomium of St. Pisenthios. Both codices have been palaeographically dated to the seventh-eighth centuries CE. In this paper, we describe our project and present the results of the work carried out on the Canons of Pseudo-Basil. Our work involved photography in transmitted light, measurements of the thickness of the papyrus leaves, and digital microscopy under three-light illumination. These measurements allowed us to determine the types of the inks and characterize the papyrus writing substrate. For conservation, we used a novel method developed in the Egyptian Museum in Berlin that comprises suspending papyrus folios on a translucent, extremely thin Japanese paper inside glass frames without the use of adhesives. KW - Papyrus KW - Codex KW - Conservation KW - Iron gall ink KW - Coptic PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570998 DO - https://doi.org/10.1080/00393630.2023.2183554 SN - 0039-3630 SP - 1 EP - 12 PB - Taylor & Francis AN - OPUS4-57099 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cappella, Brunero A1 - Spaltmann, Dirk A1 - Gee, M. T1 - Editorial: Tribology and Atomic Force Microscopy - Towards Single Asperity Contact N2 - The concept behind this Research Topic (RT) was to collect works, in which Atomic Force Microscopy (AFM) techniques are employed to study tribological phenomena and to push the resolution of measurements towards single asperity contact. Thanks to the direct determination of sample height with sub-nanometer resolution and the possibility of measuring local friction, AFM can be employed after a tribotest to detect topography and friction changes at the nanometer scale. Recently, efforts are being expended to use AFM cantilevers as tribometers, i.e., as probes altering the volume of suitable samples, thereby measuring tip and/or sample wear and friction at the nano/microscale. Thus, single asperity contact, friction, and wear can be investigated. Since friction and wear at the macroscale are the result of asperities interactions, such experiments are of great importance for better understanding of tribological processes. KW - Nanotribology KW - Friction KW - Wear KW - Single asperity KW - AFM PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571037 DO - https://doi.org/10.3389/fmech.2022.853934 SN - 2297-3079 VL - 8 SP - 1 EP - 2 PB - Frontiers Media CY - Lausanne AN - OPUS4-57103 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neuhold, S. A1 - Algermissen, D. A1 - Drissen, P. A1 - Adamczyk, Burkart A1 - Presoly, P. A1 - Sedlazeck, K. P. A1 - Schenk, J. A1 - Raith, J. G. A1 - Pomberger, R. A1 - Vollprecht, D. T1 - Tailoring the FeO/SiO2 Ratio in Electric Arc Furnace Slags to Minimize the Leaching of Vanadium and Chromium N2 - Based on recently published research on leaching control mechanisms in electric arc furnace (EAF) slags, it is assumed that a FeO/SiO2 ratio of around one leads to low leached V and Cr concentrations. This ratio influences the mineral phase composition of the slag toward higher amounts of spinel and a lower solubility of calcium silicate phases by suppressing the formation of magnesiowuestite and highly soluble calcium silicate phases. To evaluate this hypothesis, laboratory and scaled up tests in an EAF pilot plant were performed on slag samples characterized by elevated V and Cr leaching and a high FeO/SiO2 ratio. Prior to the melting experiments, the optimum FeO/SiO2 ratio was calculated via FactSageTM. In the melting experiments, the ratio was adjusted by adding quartz sand, which also decreased the basicity (CaO/SiO2) of the slag. As a reference, remelting experiments without quartz sand addition were conducted and additionally, the influence of the cooling rate of the slag was examined. The remelted (without quartz sand) and the remelted modified slags (with quartz sand) were analyzed chemically and mineralogically and the leaching behavior was investigated. The modification of the slags yielded a minimized release of V and Cr, supporting the hypothesis that the FeO/SiO2 ratio influences the mineralogy and the leaching behavior. KW - Electric arc furnace (EAF) slags KW - FactSageTM calculations KW - Leaching control mechanisms KW - Melting experiments PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571517 DO - https://doi.org/10.3390/app10072549 VL - 10 IS - 7 SP - 1 EP - 18 PB - MDPI AN - OPUS4-57151 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brüngel, R. A1 - Rückert, J. A1 - Müller, P. A1 - Babick, F. A1 - Friedrich, C. M. A1 - Ghanem, A. A1 - Hodoroaba, Vasile-Dan A1 - Mech, A. A1 - Weigel, S. A1 - Wohlleben, W. A1 - Rauscher, H. T1 - NanoDefiner Framework and e-Tool Revisited According to the European Commission’s Nanomaterial Definition 2022/C 229/01 N2 - The new recommended definition of a nanomaterial, 2022/C 229/01, adopted by the European Commission in 2022, will have a considerable impact on European Union legislation addressing chemicals, and therefore tools to implement this new definition are urgently needed. The updated NanoDefiner framework and its e-tool implementation presented here are such instruments, which help stakeholders to find out in a straightforward way whether a material is a nanomaterial or not. They are two major outcomes of the NanoDefine project, which is explicitly referred to in the new definition. This work revisits the framework and e-tool, and elaborates necessary adjustments to make these outcomes applicable for the updated recommendation. A broad set of case studies on representative materials confirms the validity of these adjustments. To further foster the sustainability and applicability of the framework and e-tool, measures for the FAIRification of expert knowledge within the e-tool’s knowledge base are elaborated as well. The updated framework and e-tool are now ready to be used in line with the updated recommendation. The presented approach may serve as an example for reviewing existing guidance and tools developed for the previous definition 2011/696/EU, particularly those adopting NanoDefine project outcomes. KW - Nanomaterial definition KW - Nanomaterial categorisation KW - Nanomaterial regulation KW - Nanomaterial legislation KW - Decision support KW - FAIRification PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571618 DO - https://doi.org/10.3390/nano13060990 SN - 2079-4991 VL - 13 IS - 6 - Special Issue "Identification and Quantification of Nanomaterials" SP - 1 EP - 16 PB - MDPI CY - Basel, CH AN - OPUS4-57161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eissel, A. A1 - Engelking, Lorenz A1 - Gustus, R. A1 - Treutler, K. A1 - Wesling, V. A1 - Schröpfer, Dirk A1 - Kannengießer, Thomas T1 - Alloy modification for additive manufactured Ni alloy components—part I: effect on microstructure and hardness of Invar alloy N2 - Alloy 36 (1.3912), also known as “Invar,” is an alloy with 36% nickel. The alloy has a remarkably low thermal expansion coefficient in certain temperature ranges. This peculiarity is called the invar effect, which was discovered in 1896 by the Swiss physicist Charles Édouard Guillaume. Therefore, it is used in applications in which dimensional stability is critical, such as molding tools for composite materials in aerospace, automotive applications, or liquified natural gas (LNG) cargo tanks. Moreover, increasingly complex structures and the optimization of resource efficiency also require additive manufacturing steps for the production or repair of components. Additively manufactured components have a heterogeneous microstructure and anisotropic mechanical properties. In addition, the manufactured components require subsequent machining surface finishing, like finish milling, to achieve their final contour. Nickel iron alloys are difficult to machine. Additionally, inhomogeneous microstructure may lead to unstable cutting forces and conditions. In part I of this investigation, the initial alloy 36 is modified with the elements Ti, Zr, and Hf up to a maximum of 0.33 wt.-%. The influence of the modification elements on the microstructure as well as on the hardness of the AM components is examined. Furthermore, one modification is applied to metal arc welding process and investigated. Part II focuses on the effect of the alloy modifications on machinability as well as on the surface integrity of plasma-transferred-arc-welded (PTA) and finish milled invar components. T2 - 75th IIW Annual Assembly CY - Tokyo, Japan DA - 17.07.2022 KW - Alloy modification KW - Alloy 36 KW - Plasma-transferred arc welding PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571777 DO - https://doi.org/10.1007/s40194-023-01510-w SN - 0043-2288 SP - 1 EP - 9 PB - Springer CY - Heidelberg AN - OPUS4-57177 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Machado Ferreira de Araujo, F. A1 - Duarte-Ruiz, D. A1 - Saßnick, H.-D. A1 - Gentzmann, Marie C. A1 - Huthwelker, T. A1 - Cocchi, C. T1 - Electronic Structure and Core Spectroscopy of Scandium Fluoride Polymorphs N2 - Microscopic knowledge of the structural, energetic, and electronic properties of scandium fluoride is still incomplete despite the relevance of this material as an intermediate for the manufacturing of Al−Sc alloys. In a work based on first-principles calculations and X-ray spectroscopy, we assess the stability and electronic structure of six computationally predicted ScF3 polymorphs, two of which correspond to experimentally resolved single-crystal phases. In the theoretical analysis based on density functional theory (DFT), we identify similarities among the polymorphs based on their formation energies, chargedensity distribution, and electronic properties (band gaps and density of states). We find striking analogies between the results obtained for the ow- and high-temperature phases of the material, indirectly confirming that the transition occurring between them mainly consists of a rigid rotation of the lattice. With this knowledge, we examine the X-ray absorption spectra from the Sc and F K-edge contrasting firstprinciples results obtained from the solution of the Bethe−Salpeter equation on top of all-electron DFT with high-energy-resolution fluorescence detection measurements. Analysis of the computational results sheds light on the electronic origin of the absorption maxima and provides information on the prominent excitonic effects that characterize all spectra. A comparison with measurements confirms that the sample is mainly composed of the high- and low-temperature polymorphs of ScF3. However, some fine details in the experimental results suggest that the probed powder sample may contain defects and/or residual traces of metastable polymorphs. KW - Scandium KW - X-ray spectroscopy PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570727 DO - https://doi.org/10.1021/acs.inorgchem.2c04357 SN - 0020-1669 VL - 62 IS - 10 SP - 4238 EP - 4247 PB - ACS Publications CY - Washington DC AN - OPUS4-57072 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Griesche, Axel A1 - Kannengießer, Thomas T1 - Rapid solidification during welding of duplex stainless steels – in situ measurement of the chemical concentration by Laser-Induced Breakdown Spectroscopy (LIBS) N2 - Duplex stainless steels (DSS) are frequently used, especially in applications requiring high strength combined with high corrosion resistance in aggressive media. Examples include power plant components and maritime structures. During welding of these steels, local variations in chemical composition can occur. This results in ferritization of the material and negatively affects the mechanical properties of the components. In this work, tungsten inert gas (TIG) welding experiments were performed with DSS. Chemical composition analysis was realized in situ by using Laser Induced Breakdown Spectroscopy (LIBS). The aim of the work is to quantitatively measure the chemical composition in the weld seam of various DSS and to identify possible influences of welding parameters on the microstructure of the material. The chemical concentrations of the main alloying elements Cr, Ni, Mn on the surface of the sample during the welding process and the cooling process were measured. Mn and Ni are austenite stabilizers and their content increases during welding by using certain high alloyed filler material. Spectra were recorded every 1.3 s at a spacing of approximately 2 mm. During the cooling process the location of the measurement was not changed. The LIBS method is proofed to be suitable for the quantitative representation of the chemical compositions during the welding process. T2 - ICASP-6 CY - Le Bischenberg, France DA - 20.06.2022 KW - LIBS KW - In situ measurement KW - Duplex stainless steel KW - TIG welding KW - Evaporation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571308 DO - https://doi.org/10.1088/1757-899X/1274/1/012018 VL - 1274 SP - 1 EP - 8 PB - IOP Publishing CY - Bristol AN - OPUS4-57130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tsamos, Athanasios A1 - Evsevleev, Sergei A1 - Fioresi, R. A1 - Faglioni, F. A1 - Bruno, Giovanni T1 - Synthetic Data Generation for Automatic Segmentation of X-ray Computed Tomography Reconstructions of Complex Microstructures N2 - The greatest challenge when using deep convolutional neural networks (DCNNs) for automatic segmentation of microstructural X-ray computed tomography (XCT) data is the acquisition of sufficient and relevant data to train the working network. Traditionally, these have been attained by manually annotating a few slices for 2D DCNNs. However, complex multiphase microstructures would presumably be better segmented with 3D networks. However, manual segmentation labeling for 3D problems is prohibitive. In this work, we introduce a method for generating synthetic XCT data for a challenging six-phase Al–Si alloy composite reinforced with ceramic fibers and particles. Moreover, we propose certain data augmentations (brightness, contrast, noise, and blur), a special in-house designed deep convolutional neural network (Triple UNet), and a multi-view forwarding strategy to promote generalized learning from synthetic data and therefore achieve successful segmentations. We obtain an overall Dice score of 0.77. Lastly, we prove the detrimental effects of artifacts in the XCT data on achieving accurate segmentations when synthetic data are employed for training the DCNNs. The methods presented in this work are applicable to other materials and imaging techniques as well. Successful segmentation coupled with neural networks trained with synthetic data will accelerate scientific output. KW - Automatic segmentation KW - 3D deep convolutional neural network (3D DCNN) KW - Dice score KW - Metal matrix composite (MMC) KW - Modified U-Net architectures KW - Multi-phase materials PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571243 DO - https://doi.org/10.3390/jimaging9020022 VL - 9 IS - 2 SP - 1 EP - 23 PB - MDPI AN - OPUS4-57124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mangelsdorf, Axel A1 - Blind, K. T1 - Motives to standardize: Empirical evidence from Germany N2 - In this paper, we identify the strategic motives of German manufacturing companies in the electrical engineering and machinery industry to be involved in standards development organizations. First, we present the general motives for the formation of strategic alliances and relate them to specific standardization motives. Then, we identify pursuing specific company interests, solving technical problems, knowledge seeking, influencing regulation, and facilitating market access as motives to standardize by means of factor analysis. In a second step, we test hypotheses on the relationship between the importance of strategic motives and firm level variables, e.g. R&D intensity, innovation activities, and firm size. The results reveal that firms in electric engineering and machinery have a particularly strong interest in ensuring industry-friendly design of regulations, which can be achieved by standards. Moreover, the results confirm that small firms also from these two sectors are active in standardization alliances to access knowledge from other involved stakeholders. KW - Factor analysis KW - Standardization KW - Strategic alliances KW - Knowledge spillovers KW - Market access KW - Regulation KW - Innovation KW - R&D PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-364586 DO - https://doi.org/10.1016/j.technovation.2016.01.001 SN - 0166-4972 VL - 48-49 SP - 13 EP - 24 PB - Elsevier Science B.V. CY - Amsterdam, Netherlands AN - OPUS4-36458 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cabeza, Sandra A1 - Bruno, Giovanni A1 - Mishurova, Tatiana T1 - Characterization of multiphase metal matrix composites by means of CT and neutron diffraction N2 - The present study examines the relationship between the microstructure of multiphase metal matrix composites and their damage mechanisms. The matrix AlSi12CuMgNi was combined with 15% vol. Al₂O₃ (short fibers), and with 7% vol. Al₂O₃ + 15% vol. SiC (short fibers and whiskers, respectively). The experimental approach encompasses 3D microstructure characterization by means of computed tomography of samples (a) as-cast, (b) after heat treatment, and (c) after compression tests at room temperature. The volume fraction of different phases, their distribution, their orientation, and the presence of defects and damage are studied. The influence of the addition of SiC particles on mechanical properties of composite was investigated. Phase-specific load partition analysis for samples with fiber plane parallel to load was performed by using neutron diffraction (ND) during in-situ compression. ND results show damage in the Si phase, while Al₂O₃ short fibers carry load without damage until failure. The computed tomography observations confirm the load partition analysis. T2 - WCNDT CY - München, Germany DA - 13.06.2016 KW - thermal treatment KW - synchrotron CT KW - neutron diffraction KW - composite KW - aluminum KW - residual stress PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-365499 AN - OPUS4-36549 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Naka, A. A1 - Yasutaka, T. A1 - Sakanakura, H. A1 - Kalbe, Ute A1 - Watanabe, Y. A1 - Inoba, S. A1 - Takeo, M. A1 - Inui, T. A1 - Katsumi, T. A1 - Fujikawa, T. A1 - Sato, K. A1 - Higashinog, K. A1 - Someyaga, M. T1 - Column percolation test for contaminated soils: Key factors for standardization N2 - Column percolation tests may be suitable for prediction of chemical leaching from soil and soil materials. However, compared with batch leaching tests, they are time-consuming. It is therefore important to investigate ways to shorten the tests without affecting the quality of results. In this study, we evaluate the feasibility of decreasing testing time by increasing flow rate and decreasing equilibration time compared to the conditions specified in ISO/TS 21268-3, with equilibration periods of 48 h and flow rate of 12 mL/h. We tested three equilibration periods (0, 12–16, and 48 h) and two flow rates (12 and 36 mL/h)on four different soils and compared the inorganic constituent releases. For soils A and D, we observed similar values for all conditions except for the 0 h–36 mL/h case. For soil B, we observed no appreciable differences between the tested conditions, while for soil C there were no consistent trends probably due to the difference in ongoing oxidation reactions between soil samples. These results suggest that column percolation tests can be shortened from 20 to 30 days to 7–9 days by decreasing the equilibration time to 12–16 h and increasing the flow rate to 36 mL/h for inorganic substances. KW - Contaminated soils KW - Column percolation PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-372038 DO - https://doi.org/10.1016/j.jhazmat.2016.08.046 SN - 0304-3894 VL - 320 SP - 326 EP - 340 PB - Elsevier B.V. AN - OPUS4-37203 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Büchner, T. A1 - Drescher, D. A1 - Merk, V. A1 - Traub, Heike A1 - Guttmann, P. A1 - Werner, St. A1 - Jakubowski, Norbert A1 - Schneider, G. A1 - Kneipp, J. T1 - Biomolecular environment, quantification, and intracellular interaction of multifunctional magnetic SERS nanoprobes N2 - Multifunctional composite nanoprobes consisting of iron oxide nanoparticles linked to silver and gold nanoparticles, Ag–Magnetite and Au–Magnetite, respectively, were introduced by endocytic uptake into cultured fibroblast cells. The cells containing the non-toxic nanoprobes were shown to be displaceable in an external magnetic field and can be manipulated in microfluidic channels. The distribution of the composite nanostructures that are contained in the endosomal system is discussed on the basis of surfaceenhanced Raman scattering (SERS) mapping, quantitative laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) micromapping, and cryo soft X-ray tomography (cryo soft-XRT). Cryo soft-XRT of intact, vitrified cells reveals that the composite nanoprobes form intra-endosomal aggregates. The nanoprobes provide SERS signals from the biomolecular composition of their surface in the endosomal environment. The SERS data indicate the high stability of the nanoprobes and of their plasmonic properties in the harsh environment of endosomes and lysosomes. The spectra point at the molecular composition at the surface of the Ag–Magnetite and Au–Magnetite nanostructures that is very similar to that of other Composite structures, but different from the composition of pure silver and gold SERS nanoprobes used for intracellular investigations. As shown by the LA-ICP-MS data, the uptake efficiency of the magnetite composites is approximately two to three times higher than that of the pure gold and silver nanoparticles. KW - Nanoparticles KW - SERS KW - Cell KW - LA-ICP-MS KW - X-ray tomography PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-371811 DO - https://doi.org/10.1039/c6an00890a SN - 0003-2654 VL - 141 IS - 17 SP - 5096 EP - 5106 PB - Royal Society of Chemistry CY - Cambridge, UK AN - OPUS4-37181 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hsiao, I.-L. A1 - Bierkandt, Frank A1 - Reichardt, Ph. A1 - Luch, A. A1 - Huang, Y.-J. A1 - Jakubowski, Norbert A1 - Tentschert, J. A1 - Haase, A. T1 - Quantification and visualization of cellular uptake of TiO2 and Ag nanoparticles: comparison of different ICP-MS techniques N2 - Safety assessment of nanoparticles (NPs) requires techniques that are suitable to quantify tissue and cellular uptake of NPs. The most commonly applied techniques for this purpose are based on inductively coupled plasma mass spectrometry (ICP-MS). Here we apply and compare three different ICP-MS methods to investigate the cellular uptake of TiO2 (diameter 7 or 20 nm, respectively) and Ag (diameter 50 or 75 nm, respectively) NPs into differentiated mouse neuroblastoma cells (Neuro-2a cells). Cells were incubated with different amounts of the NPs. Thereafter they were either directly analyzed by laser ablation ICP-MS (LA-ICP-MS) or were lysed and lysates were analyzed by ICP-MS and by single particle ICP-MS (SP-ICP-MS). KW - Nanoparticles KW - Single particle ICP-MS KW - Laser ablation ICP-MS KW - Cellular internalization KW - Neurons PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-371620 DO - https://doi.org/10.1186/s12951-016-0203-z SN - 1477-3155 VL - 14 SP - Article 50 AN - OPUS4-37162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Greiser, Sebastian A1 - Benemann, Sigrid A1 - Rademann, K. A1 - Emmerling, Franziska T1 - In Situ Investigation of a Self-Accelerated Cocrystal Formation by Grinding Pyrazinamide with Oxalic Acid N2 - A new cocrystal of pyrazinamide with oxalic acid was prepared mechanochemically and characterized by PXRD, Raman spectroscopy, solid-state NMR spectroscopy, DTA-TG, and SEM. Based on powder X-ray diffraction data the structure was solved. The formation pathway of the reaction was studied in situ using combined synchrotron PXRD and Raman spectroscopy. Using oxalic acid dihydrate the initially neat grinding turned into a rapid self-accelerated liquid-assisted grinding process by the release of crystallization water. Under these conditions, the cocrystal was formed directly within two minutes. KW - in situ KW - cocrystal KW - mechanochemistry KW - pyrazinamide KW - hydrate PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-372357 DO - https://doi.org/10.3390/molecules21070917 SN - 1420-3049 VL - 21 IS - 7 SP - Article 917, 1 EP - 9 AN - OPUS4-37235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlick-Hasper, Eva A1 - Seidler, Oliver A1 - Goedecke, Thomas A1 - Kraume, M. T1 - Helium leak testing of dangerous goods packagings N2 - The International Dangerous Goods Regulations prescribe the immersion under water method (“bubble test”) as standard method for the leakproofness test of dangerous goods packagings. But this test procedure acts as a test method for leak localisation, not for quantitative leakage rates measurement. Additionally, the sensitivity in detecting leaks of small diameters is restricted, depending on the test liquid and the test pressure. The bubble test is not suitable for a comparison with quantitative limit leakage rates based on realistic transport conditions. This is especially important when estimating the risk of the formation of an explosive atmosphere during the intercontinental carriage of dangerous goods packagings in freight containers. To compare measured leakage rates with limit leakage rates, a quantitative leak testing procedure is required. Therefore a new approach for dangerous goods packagings is implemented: The pressure technique by accumulation using Helium as a tracer gas. This work presents the test equipment necessary for the quantitative measurement of Helium leakage rates through closures of different kinds of dangerous goods packagings. The essential steps to achieve good repeatable results are: A controlled Helium filling process to reach a defined test pressure in the test sample, a sufficient homogenisation of the Helium-air-mixture inside the test sample and the ensuring of a constant pressure level of the test sample during the test. The Helium loss rate of the accumulation chamber has to be measured separately to receive a correction factor for the measured leakage rates. Different constructional measures are introduced to prevent a disturbing influence of the Helium leakage rate of the filling valves on the measurement results. Methods to estimate the disturbing effect of Helium permeation through permeable parts of the test sample are also presented. As a supporting method for the experimental investigations the Helium sniffer test can be applied. This practical application-oriented advice can enable other users to establish a pressure technique by accumulation for their own technical field. T2 - 19th World Conference on Non-Destructive Testing CY - Munich, Germany DA - 13.06.2016 KW - Überdruckverfahren KW - Gefahrgutverpackungen KW - Dichtheit KW - Helium KW - Dangerous goods packagings KW - Leakproofness KW - Helium KW - Pressure technique PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-371376 UR - http://ndt.net/?id=19785 SN - 1435-4934 VL - 21 IS - 7 SP - 1 EP - 10 PB - NDT.net CY - Kirchwald AN - OPUS4-37137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel A1 - Gohlke, Dirk A1 - Eisentraut, Mark T1 - Reference block design for high resolution ultrasound immersion tank N2 - In respect of modern approaches in material sciences and highly increased requirements on materials on safety relevant components, quality management and non-destructive testing reclaims a steadily increased meaning. The destructive meaning of measuring the degree of purity is defined in DIN EN 10247 through metallurgical investigations, especially microsections. For and comparable, but non-destructive testing due ultrasonic testing, the material the SEP 1927 is a well-defined industry standard. A novel and alternative way of reference block construction was focused by this work. The proposed amendments, regarding the manufacturing and machining, are less time and cost consuming. Verified by measurements the presented reference block fits the same acoustical characteristics and the requirements of the guideline. T2 - 19th World Conference on Non-Destructive Testing CY - Munich, Germany DA - 13.06.2016 KW - SEP 1927 KW - Degree of purity KW - High resolution ultrasonic testing KW - Immersion tank testing PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-368512 VL - 2016 SP - Paper X15, 1 EP - 4 AN - OPUS4-36851 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wollschläger, Nicole A1 - Tasdemir, Z. A1 - Häusler, Ines A1 - Leblebici, Y. A1 - Österle, Werner A1 - Alaca, B. E. T1 - Determination of the elastic behavior of silicon nanowires within a scanning electron microscope N2 - Three-point bending tests were performed on double-anchored, <110> silicon nanowire samples inside a scanning electron microscope (SEM) via a micromanipulator equipped with a piezo-resistive force sensor. Representing the upper and lower boundaries achievable in a consistent manner, silicon nanowires with widths of 35 nm and 74 nm and a height of 168 nm were fabricated. The nanowires were obtained monolithically along with their 10-m-tall supports through a top-down fabrication approach involving a series of etching processes. Hence, no interface compliance was introduced between supports and nanowires. Exact nanowire dimensions and cross-sectional features were determined by transmission electron microscopy (TEM) following sample preparation through focused ion beam (FIB) machining. Conducting the experiments inside an SEM chamber further raised the opportunity of the direct observation of any deviation from ideal loading conditions such as twisting, which was taken into consideration in simulations. Measured force-displacement behavior was observed to exhibit close resemblance to simulation results obtained by finite element modeling, when the bulk value of 169 GPa was taken as the modulus of elasticity for <110> silicon. Hence, test results show neither any size effect nor evidence of residual stresses for the considered nanoscale objects. The increased effect of the native oxide with reduced nanowire dimensions was captured as well. Thus this very simple in-situ testing method was found to be an alternative to elaborate AFM measurements on geometrically formidable nanostructures. The results demonstrate the applicability of the developed fabrication approach to the incorporation of silicon nanowires in functional micromechanical devices. KW - Silicon nanowire KW - Elastic behavior KW - Scanning electron microscope KW - Mechanical properties PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-370383 DO - https://doi.org/10.1155/2016/4905838 VL - 2016 SP - Article 4905838, 1 EP - 6 PB - Hindawi Publishing Corporation AN - OPUS4-37038 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schneider, Ralf A1 - Weigert, Florian A1 - Lesnyak, V. A1 - Leubner, S. A1 - Lorenz, T. A1 - Behnke, Thomas A1 - Dubavik, A. A1 - Joswig, J.-O. A1 - Resch-Genger, Ute A1 - Gaponik, N. A1 - Eychmüller, A. ED - Resch-Genger, Ute ED - Schneider, Ralf T1 - pH and concentration dependence of the optical properties of thiol-capped CdTe nanocrystals in water and D2O N2 - The optical properties of semiconductor nanocrystals (SC NCs) are largely controlled by their size and surface chemistry, i.e., the chemical composition and thickness of inorganic passivation shells and the chemical nature and number of surface ligands as well as the strength of their bonds to surface atoms. The latter is particularly important for CdTe NCs, which – together with alloyed CdₓHg₁₋ₓTe – are the only SC NCs that can be prepared in water in high quality without the need for an additional inorganic passivation shell. Aiming at a better understanding of the role of stabilizing ligands for the control of the application-relevant fluorescence features of SC NCs, we assessed the influence of two of the most commonly used monodentate thiol ligands, thioglycolic acid (TGA) and mercaptopropionic acid (MPA), on the colloidal stability, photoluminescence (PL) quantum yield (QY), and PL decay behavior of a set of CdTe NC colloids. As an indirect measure for the strength of the coordinative bond of the ligands to SC NC surface atoms, the influence of the pH (pD) and the concentration on the PL properties of these colloids was examined in water and D₂O and compared to the results from previous dilution studies with a set of thiol-capped Cd₁₋ₓHgₓTe SC NCs in D₂O. As a prerequisite for these studies, the number of surface ligands was determined photometrically at different steps of purification after SC NC synthesis with Ellman’s test. Our results demonstrate ligand control of the pH-dependent PL of these SC NCs, with MPA-stabilized CdTe NCs being less prone to luminescence quenching than TGA-capped ones. For both types of CdTe colloids, ligand desorption is more pronounced in H₂O compared to D₂O, underlining also the role of hydrogen bonding and solvent molecules. KW - Quantum dots KW - Fluorescence KW - Ligand analysis KW - Nano particles PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-371253 DO - https://doi.org/10.1039/c6cp03123d VL - 18 IS - 28 SP - 19083 EP - 19092 PB - RSC CY - Cambridge AN - OPUS4-37125 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -