TY - JOUR A1 - Bauer, L.J. A1 - Wieder, Frank A1 - Truong, V. A1 - Förste, F. A1 - Wagener, Y. A1 - Jonas, A. A1 - Praetz, S: A1 - Schlesiger, C. A1 - Kupsch, Andreas A1 - Müller, B.R. A1 - Kanngießer, B. A1 - Zaslansky, P. A1 - Mantouvalou, I. T1 - Absorption Correction for 3D Elemental Distributions of Dental Composite Materials Using Laboratory Confocal Micro-X-ray Fluorescence Spectroscopy JF - Analytical Chemistry N2 - Confocal micro-X-ray fluorescence (micro-XRF) spectroscopy facilitates three-dimensional (3D) elemental imaging of heterogeneous samples in the micrometer range. Laboratory setups using X-ray tube excitation render the method accessible for diverse research fields but interpretation of results and quantification remain challenging. The attenuation of X-rays in composites depends on the photon energy as well as on the composition and density of the material. For confocal micro-XRF, attenuation severely impacts elemental distribution information, as the signal from deeper layers is distorted by superficial layers. Absorption correction and quantification of fluorescence measurements in heterogeneous composite samples have so far not been reported. Here, an absorption correction approach for confocal micro-XRF combining density information from microcomputed tomography (micro-CT) data with laboratory X-ray absorption spectroscopy (XAS) and synchrotron transmission measurements is presented. The energy dependency of the probing volume is considered during the correction. The methodology is demonstrated on a model composite sample consisting of a bovine tooth with a clinically used restoration material. KW - Micro X-ray fluorescence spectroscopy KW - Dental composite materials KW - Computed tomography KW - Absorption correction PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601630 DO - https://doi.org/10.1021/acs.analchem.4c00116 SN - 0003-2700 SN - 1520-6882 VL - 96 IS - 21 SP - 8441 EP - 8449 PB - American Chemical Society Publications CY - Washington, DC AN - OPUS4-60163 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 JF - Nanomaterials 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 - Wolff, M. A1 - Wonneberger, R. A1 - Freiberg, K.E. A1 - Hertwig, Andreas A1 - Bonse, Jörn A1 - Giebeler, L. A1 - Koitzsch, A. A1 - Kunz, C. A1 - Weber, H. A1 - Hufenbach, J.K. A1 - Müller, F.A. A1 - Gräf, S. T1 - Formation of laser-induced periodic surface structures on Zr-based bulk metallic glasses with different chemical composition JF - Surfaces and Interfaces N2 - Bulk metallic glasses (BMG) are amorphous metal alloys known for their unique physical and mechanical properties. In the present study, the formation of femtosecond (fs) laser-induced periodic surface structures (LIPSS) on the Zr-based BMGs Zr46Cu46Al8, Zr61Cu25Al12Ti2, Zr52.5Cu17.9Al10Ni14.6Ti5 (Vit105) and Zr57Cu15.4Al10Ni12.6Nb5 (Vit106) was investigated as a function of their different chemical composition. For this purpose, LIPSS were generated on the sample surfaces in an air environment by fs-laser irradiation (λ = 1025 nm, τ = 300 fs, frep = 100 kHz). The surface topography was characterized by scanning electron microscopy and atomic force microscopy. Moreover, the impact of LIPSS formation on the structure and chemical surface composition was analyzed before and after fs-laser irradiation by X-ray diffraction and X-ray photoelectron spectroscopy as well as by transmission electron microscopy in combination with energy dispersive X-ray spectroscopy. Despite the different chemical composition of the investigated BMGs, the fs-laser irradiation resulted in almost similar properties of the generated LIPSS patterns. In the case of Zr61Cu25Al12Ti2, Vit105 and Vit106, the surface analysis revealed the preservation of the amorphous state of the materials during fs-laser irradiation. The study demonstrated the presence of a native oxide layer on all pristine BMGs. In addition, fs-laser irradiation results in the formation of laser-induced oxide layers of larger thickness consisting of an amorphous ZrAlCu-oxide. The precise laser-structuring of BMG surfaces on the nanoscale provides a versatile alternative to thermoplastic forming of BMG surfaces and is of particular interest for the engineering of functional material surfaces. KW - Bulk metallic glasses KW - Femtosecond laser KW - Laser-induced periodic surface structures (LIPSS) KW - Chemical analysis KW - Oxidation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-581799 DO - https://doi.org/10.1016/j.surfin.2023.103305 SN - 2468-0230 VL - 42 SP - 1 EP - 11 PB - Elsevier B.V. AN - OPUS4-58179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lackmann, C. A1 - Velki, M. A1 - Šimić, A. A1 - Müller, Axel A1 - Braun, U. A1 - Ečimović, S. A1 - Hollert, H. T1 - Two types of microplastics (polystyrene-HBCD and car tire abrasion) affect oxidative stress-related biomarkers in earthworm Eisenia andrei in a time-dependent manner JF - Environment International N2 - Microplastics are small plastic fragments that are widely distributed in marine and terrestrial environments. While the soil ecosystem represents a large reservoir for plastic, research so far has focused mainly on the impact on aquatic ecosystems and there is a lack of information on the potentially adverse effects of microplastics on soil biota. Earthworms are key organisms of the soil ecosystem and are due to their crucial role in soil quality and fertility a suitable and popular model organism in soil ecotoxicology. Therefore, the aim of this study was to gain insight into the effects of environmentally relevant concentrations of microplastics on the earthworm Eisenia andrei on multiple levels of biological organization after different exposure periods. Earthworms were exposed to two types of microplastics: (1) polystyrene-HBCD and (2) car tire abrasion in natural soil for 2, 7, 14 and 28 d. Acute and chronic toxicity and all subcellular investigations were conducted for all exposure times, avoidance behavior assessed after 48 h and reproduction after 28 d. Subcellular endpoints included enzymatic biomarker responses, namely, carboxylesterase, glutathione peroxidase, acetylcholinesterase, glutathione reductase, glutathione S-transferase and catalase activities, as well as fluorescence-based measurements of oxidative stress-related markers and multixenobiotic resistance activity. Multiple biomarkers showed significant changes in activity, but a recovery of most enzymatic activities could be observed after 28 d. Overall, only minor effects could be observed on a subcellular level, showing that in this exposure scenario with environmentally relevant concentrations based on German pollution levels the threat to soil biota is minimal. However, in areas with higher concentrations of microplastics in the environment, these results can be interpreted as an early warning signal for more adverse effects. In conclusion, these findings provide new insights regarding the ecotoxicological effects of environmentally relevant concentrations of microplastics on soil organisms. KW - Microplastics KW - Earthworms KW - Toxicity KW - Biomarker KW - oxidative stress PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545423 DO - https://doi.org/10.1016/j.envint.2022.107190 VL - 163 SP - 1 EP - 12 PB - Elsevier Ltd. AN - OPUS4-54542 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Thieme-Hack, M. A1 - Berghaus, U. A1 - Brümmer, F. A1 - Elsner, U. A1 - Färber, C. A1 - Frank, D. A1 - Illgas, M. A1 - Kalbe, Ute A1 - Kathage, J. A1 - Leers, A. A1 - Müller, B. A1 - Röger-Göpfert, C. A1 - Russland, H.-J. A1 - Schnabel, B. A1 - Schneider, O. A1 - Schockmann, D. A1 - Schomakers, H. A1 - Schwalbe, D. A1 - Stegemann, D. A1 - van den Berg, T. A1 - Kramps, S. T1 - Fachbericht Kunststoffsportböden - Nachhaltige Kunststoffbelagsauswahl für Sportfreianlagen N2 - Kunststoff- und Kunststoffrasenflächen kommt bei intensiv genutzten Flächen als Allwetterbeläge eine große Bedeutung zu. Sie leisten einen wichtigen Beitrag zur Absicherung eines ganzjähriger Sportangebote. Gerade Kunststoffrasen ist aber in den letzten Jahren häufig in die Kritik geraten, insbesondere durch gefährliche Inhaltsstoffe und andere negative Einflüsse auf die Umwelt. Dies hat bei Bauherren zu einer Verunsicherung geführt und Fragen aufgeworfen, die erst teilweise beantwortet sind. Die Diskussionen rund um diesen Allwetterbelag haben bereits dazu geführt, dass von Seiten der Industrie viel verändert wurde und neue innovative Lösungen gefunden werden. Der Fachbericht stellt eine Handreichung für Fachleute und interessierte Laien dar, um mehr Klarheit besonders hinsichtlich der Umweltanforderungen zu erzielen. KW - Kunststoffsportbeläge KW - Kunstrasen KW - Umweltverträglichkeit KW - Schadstofftransfer KW - Mikroplastik PY - 2022 UR - https://shop.fll.de/de/fachbericht-kunststoffsportboeden-broschuere.html SP - 1 EP - 70 PB - Forschungsgesellschaft Landschaftsentwicklung Landschaftsbau (FLL) CY - Bonn AN - OPUS4-54390 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tielemann, Christopher A1 - Busch, R. A1 - Reinsch, Stefan A1 - Patzig, C. A1 - Höche, T. A1 - Avramov, I. A1 - Müller, Ralf T1 - Oriented surface nucleation in diopside glass JF - Journal of Non-Crystalline Solids N2 - Es wird die Texturbildung in kristallisierendem Diopsidglas im Zusammenhang mit der Oberflächenbeschaffenheit der unbehandelten Probe untersucht. Zudem wird der diskutiert, dass es sich bei der Texturbildung in Gläsern höchstwahrscheinlich um ein Nukleationsphänomen handelt welches auf die richtungsabhängige Grenzflächenenergie der kristallisierenden Phase zurückzuführen ist. N2 - Oriented surface crystallization on polished diopside glass surfaces has been studied with scanning electron microscopy, electron backscatter diffraction, transmission electron microscopy and laser scanning microscopy. An orientation preference of [001] parallel to the glass surface was detected for separately growing diopside crystals even as small as 700 nm in size. This finding shows that crystal orientation occurs in the outermost surface layer without crystal-crystal interaction and indicates that the crystal orientation is a result of oriented nucleation. Depending on surface preparation, monomodal crystal orientation distributions with [100] perpendicular to the surface or bimodal distributions with [100] and [010] perpendicular to the glass Surface were detected. It was also shown that the degree of crystal orientation increases with decreasing Surface roughness. The observed orientation of diopside crystals could be explained in terms of the interfacial energies of different crystal faces. KW - Surface energy KW - Glass ceramic KW - Glass KW - EBSD KW - Diopsid PY - 2021 UR - https://www.sciencedirect.com/science/article/pii/S002230932100020X DO - https://doi.org/10.1016/j.jnoncrysol.2021.120661 SN - 0022-3093 VL - 562 PB - Elsevier B.V. AN - OPUS4-53073 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cant, D. J. H. A1 - Müller, Anja A1 - Clifford, C. A. A1 - Unger, Wolfgang A1 - Shard, A. G. T1 - Summary of ISO/TC 201 Technical Report 23173—Surface chemical analysis—Electron spectroscopies—Measurement of the thickness and composition of nanoparticle coatings JF - Surface and Interface Analysis N2 - ISO Technical Report 23173 describes methods by which electron spectroscopies, including X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES) and synchrotron techniques, can be employed to calculate the Coating thicknesses and compositions of nanoparticles. The document has been developed to review and outline the current state-of-the-art for such measurements. Such analyses of core–shell nanoparticles are common within the literature, however the methods employed are varied; the relative advantages and disadvantages of These methods, and the optimal usage of each may not be clear to the general analyst. ISO Technical Report 23173 aims to clarify the methods that are available, describe them in clear terms, exhibit examples of their use, and highlight potential issues users may face. The information provided should allow analysts of electron spectroscopy data to make clear choices regarding the appropriate analysis of electron spectroscopy data from coated nanoparticle systems and provide a basis for understanding and comparing results from different methods and systems. KW - Electron spectroscopy KW - Core-shell KW - Nanoparticles KW - ISO 23173 KW - XPS KW - Thickness KW - Composition PY - 2021 DO - https://doi.org/10.1002/sia.6987 SN - 0142-2421 VL - 53 IS - 10 SP - 893 EP - 899 PB - John Wiley & Sons Ltd AN - OPUS4-52976 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Busch, R. A1 - Tielemann, Christopher A1 - Reinsch, Stefan A1 - Müller, Ralf A1 - Patzig, C. A1 - Krause, M. A1 - Höche, T. T1 - Sample preparation for analytical scanning electron microscopy using initial notch sectioning JF - Micron N2 - A novel method for broad ion beam based sample sectioning using the concept of initial notches is presented. An adapted sample geometry is utilized in order to create terraces with a well-define d step in erosion depth from the surface. The method consists of milling a notch into the surface, followed by glancing-angle ion beam erosion, which leads to preferential erosion at the notch due to increased local surface elevation. The process of terrace formation can be utilized in sample preparation for analytical scanning electron microscopy in order to get efficient access to the depth-dependent microstructure of a material. It is demonstrated that the method can be applied to both conducting and non-conducting specimens. Furthermore, experimental parameters influencing the preparation success are determined. Finally, as a proof-of-concept, an electron backscatter diffraction study on a surface crystallized diopside glass ceramic is performed, where the method is used to analyze orientation dependent crystal growth phenomena occurring during growth of surface crystals into the bulk. KW - 3D etching KW - Ion beam erosion Sectioning KW - EBSD KW - Sample preparation KW - Analytical scanning electron microscopy KW - SEM KW - Glass Ceramic KW - Glass KW - Diopsid PY - 2021 DO - https://doi.org/10.1016/j.micron.2021.103090 SN - 0968-4328 VL - 150 PB - Elsevier B.V. AN - OPUS4-53075 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Müller, R. A1 - Brechbühl, Y. A1 - Lutzenberger, S. A1 - Said, Samir A1 - Auersch, Lutz A1 - Guigou-Carter, C. A1 - Villot, M. A1 - Müller, R. ED - Degrande, G. ED - al., et T1 - Vibration Excitation at Turnouts, Mechanism, Measurements and Mitigation Measures T2 - Noise and Vibration Mitigation for Rail Transportation Systems, Proceedings of the 13th International Workshop on Railway Noise, Notes on Numerical Fluid Mechanics and Multidisciplinary Design 150 N2 - There is a strong need for cost-effective mitigation measures for turnouts. SBB has initiated a series of examinations using different methodologies to gain a deeper understanding of the excitation mechanisms at low frequencies, in addition to that obtained in the RIVAS project. To date it is not yet clear what constitutes a complete measurement data set that would enable understanding most of the vibration excitation mechanisms in turnouts. Increasing vibration at turnouts in comparison to normal track is observed for all measured frequencies. The different methodologies are presented in the paper. Under-sleeper pads (USP) are a cost-effective method to reduce vibration at frequencies above 63 Hz (1/3 octave), but there is probably no improvement for frequencies below 63 Hz. A first test of new frog geometry did not show relevant improvements in Vibration emission in comparison to a reference frog geometry. Axle box acceleration measurements are an interesting method to identify defects in a turnout. A specialized measurement system of rail roughness could identify certain geometry Problem areas for some frogs. Noise increases also are observed at turnouts for frequencies ranging between 80 to 1000 Hz. The use of railway source models to calculate contact forces for ballasted track and turnouts seems promising, in particular for understanding the influence of ground. KW - Turnout KW - Switch KW - Vibration excitation KW - Vibration measurements PY - 2021 SN - 978-3-030-70288-5 DO - https://doi.org/10.1007/978-3-030-70289-2_42 SN - 1612-2909 VL - 150 SP - 403 EP - 410 PB - Springer Nature Switzerland AG CY - Cham AN - OPUS4-52612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Faghani, A. A1 - Gholami, M. F. A1 - Trunk, M. A1 - Müller, J. A1 - Pachfule, P. A1 - Vogl, S. A1 - Donskyi, Ievgen A1 - Li, M. A1 - Nickl, Philip A1 - Shao, J. A1 - Huang, M. R. S. A1 - Unger, Wolfgang A1 - Arenal, R. A1 - Koch, C. T. A1 - Paulus, B. A1 - Rabe, J. P. A1 - Thomas, A. A1 - Haag, R. A1 - Adeli, M. T1 - Metal-Assisted and Solvent-Mediated Synthesis of Two-Dimensional Triazine Structures on Gram Scale JF - Journal of the American Chemical Society N2 - Covalent triazine frameworks are an emerging material class that have shown promising performance for a range of applications. In this work, we report on a metal-assisted and solvent-mediated reaction between calcium carbide and cyanuric chloride, as cheap and commercially available precursors, to synthesize two-dimensional triazine structures (2DTSs). The reaction between the solvent, dimethylformamide, and cyanuric chloride was promoted by calcium carbide and resulted in dimethylamino-s-triazine intermediates, which in turn undergo nucleophilic substitutions. This reaction was directed into two dimensions by calcium ions derived from calcium carbide and induced the formation of 2DTSs. The role of calcium ions to direct the two-dimensionality of the final structure was simulated using DFT and further proven by synthesizing molecular intermediates. The water content of the reaction medium was found to be a crucial factor that affected the structure of the products dramatically. While 2DTSs were obtained under anhydrous conditions, a mixture of graphitic material/2DTSs or only graphitic material (GM) was obtained in aqueous solutions. Due to the straightforward and gram-scale synthesis of 2DTSs, as well as their photothermal and photodynamic properties, they are promising materials for a wide range of future applications, including bacteria and virus incapacitation. KW - XPS KW - Triazine KW - 2D PY - 2020 DO - https://doi.org/10.1021/jacs.0c02399 VL - 142 IS - 30 SP - 12976 EP - 12986 PB - ACS American Chemical Society AN - OPUS4-51203 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller-Vahl, H. F. A1 - Strangfeld, Christoph A1 - Nayeri, C. N. A1 - Paschereit, C. O. A1 - Greenblatt, D. T1 - Dynamic Stall Under Combined Pitching and Surging JF - AIAA Journal N2 - Dynamic stall often occurs under conditions of simultaneous unsteady pitching and surging (e.g., rotorcraft and wind turbines), butmanymodels employ a dimensionless time base that implicitly assumes that surging is superimposed, in a quasi-steady manner, on dynamic pitching. An unsteady wind tunnel was used to examine this assumption, where a technique was developed to quantify the unsteady effects of surging on a pitching NACA 0018 airfoil. The technique involved performing multiple harmonic pitching experiments under nominally steady freestream conditions that bracketed a corresponding 50% surging amplitude (1.25 ⋅ 105 ≤ Re ≤ 3.75 ⋅ 105). By interpolating these data, unsteady-pitching/quasi-steady-surging data sets were constructed and compared with de facto synchronous pitch and surging experiments, thereby isolating the unsteady effects of surging on a pitching airfoil. Both large and small poststall maximum angles of attack (αs + 5° and αs + 15°) were considered at multiple pitch-surge phase differences. During deep dynamic stall (αs � 15°), with large-scale separation, surging was seen to have a secondary effect on the unsteady aerodynamics. However, at small poststall maximum angles of attack (αs + 5°), either light or deep dynamic stall behavior was observed depending upon the pitch-surge phase difference. This was attributed to Reynolds number history effects, exemplified by boundary-layer transition, and thus it can be referred to as “transitional” dynamic stall. KW - Dynamic stall KW - Angle of attack oscillations KW - Free stream velocity osciallations PY - 2020 DO - https://doi.org/10.2514/1.J059153 VL - 58 IS - 12 SP - 5134 EP - 5145 PB - American Institute of Aeronautics and Astronautics AN - OPUS4-51037 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cant, D. J. H. A1 - Minelli, C. A1 - Sparnacci, K. A1 - Müller, Anja A1 - Kalbe, H. A1 - Stoger-Pollach, M. A1 - Unger, Wolfgang A1 - Werner, W. S. M. A1 - Shard, A. G. T1 - Surface-Energy Control and Characterization of Nanoparticle Coatings JF - Journal of Physical Chemistry C N2 - Accurate and reproducible measurement of the structure and properties of high-value nanoparticles is extremely important for their commercialization. A significant proportion of engineered nanoparticle systems consist of some form of nominally core-shell structure, whether by design or unintentionally. Often, these do not form an ideal core-shell structure, with typical deviations including polydispersity of the core or shell, uneven or incomplete shells, noncentral cores, and others. Such systems may be created with or without intent, and in either case an understanding of the conditions for formation of such particles is desirable. Precise determination of the structure, composition, size, and shell thickness of such particles can prove challenging without the use of a suitable range of characterization techniques. Here, the authors present two such polymer core-shell nanoparticle systems, consisting of polytetrafluoroethylene cores coated with a range of thicknesses of either polymethylmethacrylate or polystyrene. By consideration of surface energy, it is shown that these particles are expected to possess distinctly differing coating structures, with the polystyrene coating being incomplete. A comprehensive characterization of these systems is demonstrated, using a selection of complementary techniques including scanning electron microscopy, scanning transmission electron microscopy, thermogravimetric analysis, dynamic light scattering, differential centrifugal sedimentation, and X-ray photoelectron spectroscopy. By combining the results provided by these techniques, it is possible to achieve superior characterization and understanding of the particle structure than could be obtained by considering results separately. KW - Nanoparticles KW - Core-shell KW - XPS KW - Size KW - Thickness KW - Damage PY - 2020 DO - https://doi.org/10.1021/acs.jpcc.0c02161 VL - 124 IS - 20 SP - 11200 EP - 11211 PB - ACS CY - Washington DC AN - OPUS4-50899 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kunz, C. A1 - Bonse, Jörn A1 - Spaltmann, Dirk A1 - Neumann, C. A1 - Turchanin, A. A1 - Bartolomé, J. F. A1 - Müller, F. A. A1 - Gräf, S. T1 - Tribological performance of metal-reinforced ceramic composites selectively structured with femtosecond laser-induced periodic surface structures JF - Applied Surface Science N2 - The impact of femtosecond (fs) laser-induced periodic surface structures (LIPSS) on tribological properties was investigated for metal-reinforced ceramic composites (Al2O3-ZrO2-Nb). For this purpose, the metallic niobium (Nb) phase was selectively structured with LIPSS in an air environment with different values of the fs-laser peak fluence by near-infrared fs-laser radiation (λ = 1025 nm, τ = 300 fs, frep = 1 kHz), taking advantage of the different light absorption behavior of ceramic and metal. The tribological performance was evaluated by reciprocating sliding tests in a ball-on-disc configuration using Ringer's solution as lubricant. The surfaces were characterized before and after laser irradiation by optical microscopy, scanning electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, energy dispersive X-ray spectroscopy and by measuring the contact angle with Ringer's solution. The LIPSS formation resulted in an increased wetting of the surface with the lubricant. Moreover, the selectively structured composite surfaces revealed a coefficient of friction significantly reduced by a factor of ~3 when compared to the non-irradiated surface. Furthermore, the formation of a laser-induced oxidation layer was detected with NbO as the most prominent oxidation state. Selectively structured composites with outstanding mechanical properties and enhanced tribological performance are of particular interest for biomedical applications. KW - Laser-induced periodic surface structures (LIPSS) KW - Femtosecond laser ablation KW - Ceramic matrix composites KW - Tribology PY - 2020 DO - https://doi.org/10.1016/j.apsusc.2019.143917 SN - 0169-4332 SN - 1873-5584 VL - 499 IS - 1 SP - 143917 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-49255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, I. A1 - Moll, J. A1 - Kexel, C. A1 - Schubert, L. A1 - Tschöke, K. A1 - Prager, Jens A1 - Lugovtsova, Yevgeniya A1 - Bach, M. A1 - Vogt, T. T1 - SHM using Guided Waves – Recent Activities and Advances in Germany T2 - Proceedings of the 12th International Workshop on Structural Health Monitoring N2 - Issues that prevent Structural Health Monitoring (SHM) based on Guided Waves (GW) from being a part of today’s monitoring solutions in industry are not all obvious to the scientific community. To uncover and overcome these issues, scientists working on SHM and GW problems joined in an expert committee under the patronage of the German Society for Non-Destructive Testing. An initiated online survey among more than 700 experts and users reveals the hurdles hindering the practical application of GWbased SHM. Firstly, methods for proof of reliability of SHM approaches are missing. Secondly, detailed understanding of phenomenological described wave-damage interactions is needed. Additionally, there are significant unsolved implementation issues and unsolved problems of signal processing including handling of environmental influences. To enable substantial proof of reliability without unaffordable experimental effort also efficient simulation tools including realistic damage interaction are needed, enabling the joint use of experimental and simulated data to predict the capabilities of the Monitoring system. Considering these issues, the committee focusses on simulation, signal processing, as well as probability of detection and standardization. In the presented work, recent activities of the expert committee starting with survey results are summarized. An open access data basis of life-like measurements is presented to allow testing and comparison of signal processing and simulation algorithms. Finally, a strategy for efficient proof of reliability increasing the acceptance of SHM in industry and for successful Integration of SHM into real-world engineering structures is proposed. T2 - The 12th International Workshop on Structural Health Monitoring (IWSHM) CY - Stanford, California, USA DA - 10.09.2019 KW - Structural Health Monitoring KW - Ultrasonic Guided Waves KW - Non-Destructive Testing KW - Survey KW - Probability of Detection KW - Reliability PY - 2019 SP - 1 EP - 10 AN - OPUS4-49232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinrich, Thomas A1 - Darlatt, Erik A1 - Lippitz, Andreas A1 - Müller, S. A1 - Schalley, C. A1 - Unger, Wolfgang T1 - Systematic XP and NEXAFS spectroscopy studies of (ter-)pyridineterminated self-assembled monolayers and their addressability for functional molecules JF - Journal of Electron Spectroscopy and Related Phenomena N2 - The chemical composition of surfaces functionalized with self-assembled monolayers (SAMs) is an important parameter that determines their performance in a broad range of applications, from immobilizing molecular machines to initiation and growth control of MOFs (Metal-Organic Frameworks). In this article, a critical Survey of XPS (X-ray photoelectron spectroscopy) and NEXAFS (near edge X-ray absorption fine structure) spectroscopy data for pyridine-functionalized monolayers on gold surfaces is presented to compile correlations that have been indiscernible before. Monolayers with aromatic backbones are compared to monolayers with aliphatic backbones. Monolayers with pyridine end-groups are compared to mixed monolayers formed terpyridine-functionalized by molecules end-groups and non-functionalized molecules. Thiol-oxidation during ageing of the SAMs in air is addressed. And finally, the addressability of the SAMs for the deposition of metal-ions and organic molecules is investigated and compared. This work consequently delivers a comprehensive set of spectroscopic data of (ter-)pyridine-terminated SAMs and their performance as template for the preparation of functional multilayers of macrocycles exhibiting a preferential orientation. KW - (ter-)pyridineterminated self-assembled monolayer KW - X-ray Photoelectron Spectroscopy (XPS) KW - NEXAFS PY - 2019 DO - https://doi.org/10.1016/j.elspec.2019.03.011 VL - 233 SP - 28 EP - 37 PB - Elsevier B.V. AN - OPUS4-48018 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Akatsuka, C. A1 - Honma, T. A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Tanaka, S. A1 - Komatsu, T. T1 - Surface crystallization and gas bubble formation during conventional heat treatment in Na2MnP2O7 glass JF - Journal of Non-Crystalline Solids N2 - The crystallization behavior of sodium ion conductive Na2MnP2O7 glass was examined to clarify the crystallization mechanism. The formation of thermodynamically metastable phase, layered Na2MnP2O7, at the surface of the glass occurred. Heat treatment at 430 °C for 3 h lead to surface crystals of Na2MnP2O7 oriented with the (101) direction perpendicular to the sample surface. As the heat treatment temperature increased, the glass-ceramic samples deformed, and the presence numerous micro bubbles due to dissolved water was detected. KW - Glass-ceramic KW - Crystallization KW - Sodium ion batteries KW - Bubble formation KW - Phosphate PY - 2019 DO - https://doi.org/10.1016/j.jnoncrysol.2019.01.030 VL - 510 SP - 36 EP - 41 PB - Elsevier B.V. AN - OPUS4-49618 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Prewitz, M. A1 - Gaber, M. A1 - Müller, Ralf A1 - Marotzke, C. A1 - Holtappels, Kai T1 - Polymer coated glass capillaries and structures for high-pressure hydrogen storage: Permeability and hydrogen tightness JF - International journal of hydrogen energy N2 - The hydrogen tightness of high-pressure hydrogen storage is a Basic criterion for long-term storage. The H2 permeation coefficients of epoxy resin and a glass lacquer were determined to enable the geometric optimization of a glass capillary storage. It was found that the curing conditions have no significant influence on the H2 permeation coefficient of resin. The H2 permeation coefficient of epoxy resin is only about three orders of Magnitude greater than that of borosilicate glass. This suggests that the initial pressure of 700 bar takes about 2.5 years to be halved in capillary array storage. Therefore, a high-pressure hydrogen storage tank based on glass capillaries is ideally suited for long-term storage in mobile applications. KW - Permeability KW - Glass capillaries KW - Coating KW - Hydrogen storage KW - Long-term calculation KW - Epoxy resin PY - 2018 DO - https://doi.org/10.1016/j.ijhydene.2017.12.092 SN - 0360-3199 VL - 43 IS - 11 SP - 5637 EP - 5644 PB - Elsevier AN - OPUS4-44327 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosemann, Paul A1 - Müller, C. A1 - Kauss, N. A1 - Halle, T. T1 - Einfluss der Wärmebehandlung auf Mikrostruktur und Korrosionsverhalten kohlenstoffhaltiger nichtrostender Stähle T2 - Tagungsband zum 20. Werkstofftechnischen Kolloquium N2 - Das Korrosionsverhalten von kohlenstoffhaltigen martensitischen nichtrostenden Stählen variiert in Abhängigkeit der Wärmebehandlung (WB) und der damit eingestellten Mikrostruktur deutlich stärker als bei kohlenstoffarmen ferritischen und austenitischen nichtrostenden Stählen. Bei erhöhtem Kohlenstoffgehalt bestimmt die diffusionsgesteuerte Bildung und Auflösung von Chromkarbiden die Verteilung von Chrom und Kohlenstoff im Gefüge. Bisher lag der Fokus von Forschungsarbeiten zum Einfluss der WB auf dem Anlassen im allgemein bekannten Sensibilisierungsbereich dieser Werkstoffgruppe zwischen 200 °C und 700 °C und der dort auftretenden Chromverarmung. Mit der gezielten WB des X46Cr13 (1.4034) wird gezeigt, dass Temperatur und Dauer beim Austenitisieren sowie die anschließende Abkühlung beim Härten das Korrosionsverhalten schon vor dem Anlassen signifikant beeinflussen. Auf der Basis von thermodynamischen Berechnungen wurden definierte WB ausgewählt, um gezielt unterschiedliche Volumengehalte von Chromkarbiden im Gefüge und somit auch unterschiedliche Chrom bzw. Kohlenstoffgehalte im Mischkristall zu erzeugen. Anschließend wurden die resultierenden Gefügezustände hinsichtlich Chromkarbidanteil und Härte verglichen und das Korrosionsverhalten mit der elektrochemisch potentiodynamischen Reaktivierung (EPR) sowie durch einen Schnelltest mit der KorroPad-Prüfung untersucht. Dabei konnte ein direkter Zusammenhang zwischen WB, Mikrostrukturänderungen und Korrosionsverhalten festgestellt werden. Mit steigender Austenitisierungstemperatur wird der Anteil an Chromkarbiden reduziert und der Kohlenstoff- und Chromgehalt der Matrix erhöht, bis eine vollständige Auflösung der Chromkarbide gegeben und die chemische Nennzusammensetzung der Legierung im Mischkristall erreicht ist. In der direkten Folge wird die Ausbildung der für nichtrostende Stähle charakteristischen Passivschicht erleichtert und das Lochkorrosionsverhalten verbessert. Die Abkühlrate hat neben den Austenitisierungsparametern ebenfalls einen großen Einfluss auf das Korrosionsverhalten. So führt eine langsame Abkühlung an Luft zu einer Chromverarmung im Gefüge, die eine deutlich erhöhte Lochkorrosionsanfälligkeit zur Folge hat. In Abhängigkeit der WB von kohlenstoffhaltigen nichtrostenden Stählen können Mikrostruktur, Härte und Korrosionsbeständigkeit in einem weiten Bereich variieren. T2 - 20. Werkstofftechnisches Kolloquium CY - Chemnitz, Germany DA - 14.03.2018 KW - Nichtrostender Stahl KW - Wärmebehandlung KW - EPR KW - KorroPad KW - Korrosionsbeständigkeit KW - ThermoCalc KW - Sensibilisierung KW - Martensitischer nichtrostender Stahl KW - Passivschicht PY - 2018 SN - 978-3-00-058901-0 SN - 1439-1597 VL - 72 SP - 711 EP - 720 PB - Eigenverlag CY - Chemnitz AN - OPUS4-44559 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wisniewski, W. A1 - Thieme, C. A1 - Müller, Ralf A1 - Reinsch, Stefan A1 - Groß-Barsnick, S.-M. A1 - Rüssel, C. T1 - Oriented surface nucleation and crystal growth in a 18BaO·22CaO·60SiO2 mol% glass used for SOFC seals JF - CrystEngComm N2 - A glass of the composition 37BaO·16CaO·47SiO2 wt% produced on an industrial scale is crystallized at 970 °C for times ranging from 15 min to 2 h. The crystallization at the immediate surface as well as the crystal growth into the bulk are analyzed using scanning electron microscopy (SEM) including energy dispersive X-ray spectroscopy (EDXS) and electron backscatter diffraction (EBSD) as well as X-ray diffraction in the Θ–2Θ setup (XRD). The immediate surface shows the oriented nucleation of walstromite as well as the formation of wollastonite and an unknown phase of the composition BaCaSi3O8. All three phases also grow into the bulk where walstromite ultimately dominates the kinetic selection and grows throughout the bulk due to a lack of bulk nucleation. Walstromite shows systematic orientation changes as well as twinning during growth. A critical analysis of the XRD-patterns acquired from various crystallized samples indicates that their evaluation is problematic and that phases detected by XRD in this system should be verified by another method such as EDXS. KW - Glass KW - Surface nucleation KW - Orientation KW - EBSD PY - 2018 DO - https://doi.org/10.1039/c7ce02008b VL - 20 IS - 6 SP - 787 EP - 795 PB - Royal Society of Chemistry AN - OPUS4-44405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kunz, C. A1 - Büttner, T.N. A1 - Naumann, B. A1 - Boehm, A.V. A1 - Gnecco, E. A1 - Bonse, Jörn A1 - Neumann, C. A1 - Turchanin, A. A1 - Müller, F.A. A1 - Gräf, S. T1 - Large-area fabrication of low- and high-spatial-frequency laser-induced periodic surface structures on carbon fibers JF - Carbon N2 - The formation and properties of laser-induced periodic surface structures (LIPSS) were investigated on carbon fibers under irradiation of fs-laser pulses characterized by a pulse duration τ = 300 fs and a laser wavelength λ = 1025 nm. The LIPSS were fabricated in an air environment at normal incidence with different values of the laser peak fluence and number of pulses per spot. The morphology of the generated structures was characterized by using scanning electron microscopy, atomic force microscopy and Fast-Fourier transform analyses. Moreover, the material structure and the surface chemistry of the carbon fibers before and after laser irradiation was analyzed by micro Raman spectroscopy and X-ray photoelectron spectroscopy. Large areas in the cm2 range of carbon fiber arrangements were successfully processed with homogenously distributed high- and low-spatial frequency LIPSS. Beyond those distinct nanostructures, hybrid structures were realized for the very first time by a superposition of both types of LIPSS in a two-step process. The findings facilitate the fabrication of tailored LIPSS-based surface structures on carbon fibers that could be of particular interest for e.g. fiber reinforced polymers and concretes. KW - Fs-Laser KW - Laser-induced periodic surface structures (LIPSS) KW - Carbon fibers KW - Large area structuring PY - 2018 UR - https://www.sciencedirect.com/science/article/pii/S0008622318302781 DO - https://doi.org/10.1016/j.carbon.2018.03.035 SN - 0008-6223 SN - 1873-3891 VL - 133 SP - 176 EP - 185 PB - Elsevier Ltd. AN - OPUS4-44625 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -