TY - JOUR A1 - Linberg, Kevin A1 - Röder, Bettina A1 - Al-Sabbagh, Dominik A1 - Emmerling, Franziska A1 - Michalchuk, Adam T1 - Controlling polymorphism in molecular cocrystals by variable temperature ball milling N2 - Mechanochemistry offers a unique opportunity to modify and manipulate crystal forms, often providing new products as compared with conventional solution methods. While promising, there is little known about how to control the solid form through mechanochemical means, demanding dedicated investigations. Using a model organic cocrystal system (isonicotinamide:glutaric acid), we here demonstrate that with mechanochemistry, polymorphism can be induced in molecular solids under conditions seemingly different to their conventional thermodynamic (thermal) transition point. Whereas Form II converts to Form I upon heating to 363 K, the same transition can be initiated under ball milling conditions at markedly lower temperatures (348 K). Our results indicate that mechanochemical techniques can help to reduce the energy barriers to solid form transitions, offering new insights into controlling polymorphic forms. Moreover, our results suggest that the nature of mechanochemical transformations could make it difficult to interpret mechanochemical solid form landscapes using conventional equilibrium-based tools. KW - Mechanochemistry KW - Polymorphism KW - TRIS PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564728 DO - https://doi.org/10.1039/d2fd00115b SP - 1 EP - 16 PB - Royal Society of Chemistry AN - OPUS4-56472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kazemifard, N. A1 - Dehkohneh, Abolfazl A1 - Baradaran Ghavami, S. T1 - Probiotics and probiotic-based vaccines: A novel approach for improving vaccine efficacy N2 - Vaccination is defined as the stimulation and development of the adaptive immune system by administering specific antigens. Vaccines' efficacy, in inducing immunity, varies in different societies due to economic, social, and biological conditions. One of the influential biological factors is gut microbiota. Cross-talks between gut bacteria and the host immune system are initiated at birth during microbial colonization and directly control the immune responses and protection against pathogen colonization. Imbalances in the gut microbiota composition, termed dysbiosis, can trigger several immune disorders through the activity of the adaptive immune system and impair the adequate response to the vaccination. The bacteria used in probiotics are often members of the gut microbiota, which have health benefits for the host. Probiotics are generally consumed as a component of fermented foods, affect both innate and acquired immune systems, and decrease infections. This review aimed to discuss the gut microbiota's role in regulating immune responses to vaccination and how probiotics can help induce immune responses against pathogens. Finally, probiotic-based oral vaccines and their efficacy have been discussed. KW - Probiotics KW - Gut microbiota KW - Probiotic-based vaccines PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561767 DO - https://doi.org/10.3389/fmed.2022.940454 SN - 2296-858X VL - 9 SP - 1 EP - 15 PB - Frontiers Media CY - Lausanne AN - OPUS4-56176 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lifka, S. A1 - Harsányi, K. A1 - Baumgartner, E. A1 - Pichler, L. A1 - Baiko, D. A1 - Wasmuth, Karsten A1 - Heitz, J. A1 - Meyer, M. A1 - Joel, A.-C. A1 - Bonse, Jörn A1 - Baumgartner, W. ED - Mail, M. T1 - Laser-processed antiadhesive bionic combs for handling nanofibers inspired by nanostructures on the legs of cribellate spiders N2 - Nanofibers are drawing the attention of engineers and scientists because their large surface-to-volume ratio is favorable for applications in medicine, filter technology, textile industry, lithium-air batteries, and optical sensors. However, when transferring nanofibers to a technical product in the form of a random network of fibers, referred to as nonwoven fabric, the stickiness of the freshly produced and thus fragile nanofiber nonwoven remains a problem. This is mainly because nanofibers strongly adhere to any surface because of van der Waals forces. In nature, there are animals that are actually able to efficiently produce, process, and handle nanofibers, namely cribellate spiders. For that, the spiders use the calamistrum, a comb-like structure of modified setae on the metatarsus of the hindmost (fourth) legs, to which the 10–30 nm thick silk nanofibers do not stick due to a special fingerprint-like surface nanostructure. In this work, we present a theoretical model of the interaction of linear nanofibers with a sinusoidally corrugated surface. This model allows for a prediction of the adhesive interaction and, thus, the design of a suitable surface structure to prevent sticking of an artificially nonwoven of nanofibers. According to the theoretical prediction, a technical analogon of the nanoripples was produced by ultrashort pulse laser processing on different technically relevant metal surfaces in the form of so-called laser-induced periodic surface structures (LIPSS). Subsequently, by means of a newly established peel-off test, the adhesion of an electrospun polyamide fiber-based nonwoven was quantified on such LIPSS-covered aluminium alloy, steel, and titanium alloy samples, as well as on polished (flat) control samples as reference and, additionally, on samples with randomly rough surfaces. The latter revealed that the adhesion of electrospun nanofiber nonwoven is significantly lowered on the nanostructured surfaces compared with the polished surfaces. KW - Laser-induced periodic surface structures (LIPSS) KW - Cribellate spiders KW - Calamistrum KW - Electrospinning KW - Nanofibers PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561799 DO - https://doi.org/10.3762/bjnano.13.105 SN - 2190-4286 VL - 13 SP - 1268 EP - 1283 PB - Beilstein-Institut zur Förderung der Chemischen Wissenschaften CY - Frankfurt, M. AN - OPUS4-56179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ewert, U. A1 - Jaenisch, Gerd-Rüdiger A1 - Schumacher, David A1 - Zscherpel, U. A1 - Deresch, A. A1 - Bircher, B. A1 - Meli, F. T1 - Schnelle Messung und tomographische Rekonstruktion von Brennflecken < 5 μm durch Aufnahmen strukturierter Prüfkörper N2 - Im Europäischen EMPIR-Projekt „NanoXSpot“ (Measurement of the focal spot size of Xray tubes with spot sizes down to 100 nm) werden neue Messmethoden für Brennflecke von Röntgenröhren entwickelt. Teil des Projektes ist die Entwicklung eines zur Lochkameramethode äquivalenten Messverfahrens für kleine Brennflecke. ASTM E 1165-20, Annex A, beschreibt die Bestimmung von Brennfleckgrößen aus Kantenprofilen von Lochaufnahmen für Röntgenröhren mit Brennflecken > 50 μm. Es wurde bereits vorgeschlagen über die Analyse der richtungsabhängigen Kantenunschärfe einer Lochblende und anschließender CT-Rekonstruktion die Intensitätsverteilung des Brennflecks äquivalent zur Lochkameraaufnahme zu berechnen. Die Lochkameramethode, wie in EN 12543-2 und ASTM E 1165-20 beschrieben, ist im unteren Größenbereich für Mikrofokusröhren nicht geeignet, da Pinholes < 10 μm schwer zu fertigen sind und lange Belichtungszeiten erwartet werden. Mit Hilfe exakt gefertigter Lochblenden sowie strukturierter Targets mit konvergierenden Strukturen wird der Bereich mit der Single-Shot-CT-Methode auf die Messung von Mikrofokusröhren, alternativ zur Vermessung von Kanten oder Strichgruppenkörpern, erweitert. Die rekonstruierten Brennfleckformen werden mit Kantenund Lochkameraaufnahmen quantitativ verglichen, um die Messgenauigkeit zu bewerten. Außerdem werden CNR und Messzeit bestimmt, um die Wirtschaftlichkeit der Verfahren zu bewerten. T2 - DGZfP-Jahrestagung CY - Online meeting DA - 10.05.2021 KW - Röntgenröhre KW - Brennfleckmessung KW - Prüfkörper KW - Rekonstruktion PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561846 SP - 1 EP - 2 AN - OPUS4-56184 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Loges, A. A1 - Scholz, G. A1 - Amadeu de Sosa, Nader A1 - Jingjing, S. A1 - Emmerling, Franziska A1 - John, T. A1 - Paulus, B. A1 - Braun, T. T1 - Studies on the local structure of the F/OH site in topaz by magic angle spinning nuclear magnetic resonance and Raman spectroscopy N2 - he mutual influence of F and OH groups in neighboring sites in topaz (Al2SiO4(F,OH)2) was investigated using magic angle spinning nuclear magnetic resonance (MAS NMR) and Raman spectroscopy. The splitting of 19F and 1H NMR signals, as well as the OH Raman band, provides evidence for hydrogen bond formation within the crystal structure. Depending on whether a given OH group has another OH group or fluoride as its neighbor, two different hydrogen bond constellations may form: either OH···O···HO or F···H···O. The proton accepting oxygen was determined to be part of the SiO4 tetrahedron using 29Si MAS NMR. Comparison of the MAS NMR data between an OH-bearing and an OH-free topaz sample confirms that the 19F signal at −130 ppm stems from F− ions that take part in H···F bonds with a distance of ∼ 2.4 Å, whereas the main signal at −135 ppm belongs to fluoride ions with no immediate OH group neighbors. The Raman OH sub-band at 3644 cm−1 stems from OH groups neighboring other OH groups, whereas the sub-band at 3650 cm−1 stems from OH groups with fluoride neighbors, which are affected by H···F bridging. The integrated intensities of these two sub-bands do not conform to the expected ratios based on probabilistic calculations from the total OH concentration. This can be explained by a difference in the polarizability of the OH bond between the different hydrogen bond constellations or partial order or unmixing of F and OH, or a combination of both. This has implications for the quantitative interpretation of Raman data on OH bonds in general and their potential use as a probe for structural (dis-)order. No indication of tetrahedrally coordinated Al was found with 27Al MAS NMR, suggesting that the investigated samples likely have nearly ideal Al/Si ratios, making them potentially useful as high-density electron microprobe reference materials for Al and Si, as well as for F. KW - Topas KW - NMR KW - XRD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561863 DO - https://doi.org/10.5194/ejm-34-507-2022 SN - 1617-4011 VL - 34 IS - 5 SP - 507 EP - 521 PB - Copernicus Publications CY - Göttingen AN - OPUS4-56186 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emmerling, Franziska A1 - Hoch, C. T1 - Laudatio Prof. Dr.-Ing. Caroline Röhr N2 - It is a laudatio on the ocations of Prof. Dr.-Ing. Caroline Röhrs 60th birthday. KW - Metal-oxides PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561877 DO - https://doi.org/10.1002/zaac.202200159 SN - 0044-2313 VL - 648 IS - 10 SP - 1 EP - 2 PB - John Wiley & Sons, Ltd AN - OPUS4-56187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ehlers, Henrik A1 - Thewes, R. A1 - Pelkner, Matthias T1 - Online Process Monitoring for Additive Manufacturing Using Eddy Current Testing With Magnetoresistive Sensor Arrays N2 - The rising popularity of additive manufacturing processes leads to an increased interest in possibilities and methods for related process monitoring. Such methods ensure improved process quality and increase the understanding of the manufacturing process, which in turn is the basis for stable component quality, e.g., required in the aerospace industry or in the medical sector. For laser powder bed fusion, a handful of process monitoring tools already exist, such as optical tomography, thermography, pyrometry, imaging, or laser power monitoring. Although these tools provide helpful information about the process, more information is required for an accurate in-depth understanding. In this article, advanced approaches in eddy current testing (ET) are combined, such as single wire excitation, magnetoresistive (MR) sensor arrays, and heterodyning to build up a system that can be used for online process monitoring of laser powder bed fusion. In addition to detailed information about the developed ET system and underlying signal processing, the first results of magnetoresistance-basedonline ET during the laser powder fusion process are presented. While producing a step-shaped cuboid, each layer is tested during recoating. Test results show that not only the contours of the topmost layer are detected but also the contours of previous layers covered by powder. At an excitation frequency of 1 MHz, a penetration depth of approx. 400 μm is obtained. To highlight the possibilities of ET for online process monitoring of laser powder bed fusion, results are compared with postexposure images of the integrated layer control system (LCS). KW - Process monitoring KW - Eddy current testing KW - Giant magneto resistance (GMR) KW - Additive manufacturing KW - Laser powder bed fusion PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560881 DO - https://doi.org/10.1109/JSEN.2022.3205177 VL - 22 IS - 20 SP - 19293 EP - 19300 PB - IEEE CY - New York, NY AN - OPUS4-56088 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eissel, A. A1 - Engelking, Lorenz A1 - Treutler, K. A1 - Schroepfer, Dirk A1 - Wesling, V. A1 - Kannengießer, Thomas T1 - Investigations on influencing the microstructure of additively manufactured Co‑Cr alloys to improve subsequent machining conditions N2 - Co-Cr alloys are frequently used for highly stressed components, especially in turbine and plant construction, due to their high resistance to thermal and mechanical stress, as well as to corrosive and abrasive loads. Furthermore, they are classified as difficult-to-cut materials because of their high strength and toughness as well as their low thermal conductivity. However, for Co, an increased cost and supply risk can be observed in recent years. Therefore, additive manufacturing (AM) offers significant economic advantages due to higher material efficiency regarding repair, modification, and manufacturing of such components. Concerning inhomogeneity and anisotropy of the microstructure and properties as well as manufacturing-related stresses, a lot of knowledge is still necessary for the economic use of additive welding processes in SMEs. In addition, subsequent machining, particularly contour milling, is essential to generate the required complex contours and surfaces. Hence, additive and machining manufacturing processes need to be coordinated in a complementary way, especially due to additional challenges arising in milling of heterogeneous hard-to-cut microstructures. Recently, it has been shown that modern, hybrid cutting processes, such as ultrasonic-assisted milling (US), can improve the cutting situation. In this investigation, the Co-Cr initial alloy is additionally modified with Ti and Zr up to 1 wt% with the aim to enhance the homogeneity of the microstructure and, thus, the machinability. Hence the investigation includes finish milling tests of the AM components and the comparison of US and conventional machining. Both the modifications and the ultrasonic assistance exhibit a significant effect on the machining situation; for example US causes a higher surface integrity of the finish milled surfaces compared to conventional milling. T2 - International Congress on Welding, Additive Manufacturing and associated non-destructive testing CY - Online meeting DA - 08.06.2022 KW - Cobalt-chromium alloy KW - Additive manufacturing KW - Ultrasonic-assisted milling KW - Surface integrity PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560917 DO - https://doi.org/10.1007/s40194-022-01397-z SP - 1 EP - 9 PB - Springer CY - Heidelberg AN - OPUS4-56091 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Auersch, Lutz A1 - Song, Jiaojiao T1 - Dynamic damage detection of slab tracks – finite element models on Winkler soil and finite-element boundary-element models on continuous soil N2 - The train passages over intact or damaged slab tracks on different soils have been calculated by two methods. The finite element method (FEM) uses a Winkler soil under the track model by adding a thin “soil layer”. The combined finite element boundary element method has a continuous soil model which is included by the boundary element method. The basic results are the distributions of the track (rail, track plate, and base layer) displacements along the track for a single axle laod. These solutions are superposed to a complete train load and transformed to time histories. The influence of track and soil parameters has been analysed. The main interest is the influence of the track damage. A gap between track plate and base layer of different lengths has been studied for changes in amplitudes and widths of deflection. A best fit to measured track displacements has been found so that the track damage can be identified and quantified. The FEM model with Winkler soil cannot be fitted to the amplitude and width with the same soil parameters. Therefore, the FEBEM model is preferable for these railway track problems. KW - Track damage quantification KW - Finite element method KW - Combined finite-element boundary-element method PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562207 DO - https://doi.org/10.3390/civileng3040055 SN - 2673-4109 VL - 3 IS - 4 SP - 979 EP - 997 PB - MDPI CY - Basel AN - OPUS4-56220 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiehle, Philipp A1 - Brinkmann, M. T1 - Material behaviour of unstabilised earth block masonry and its components under compression at varying relative humidity N2 - block and mortar types is analysed with particular regard to the influence of varying relative humidity. The uniaxial compressive strength and deformation characteristics of unstabilised earth blocks and mortars as well as of unstabilised earth block masonry are studied in detail and compared to conventional masonry to evaluate whether the structural design can be made accordingly. An increase of 30 % points in relative humidity leads to a reduction of the masonry´s compressive strength between 33 % and 35 % whereas the Young´s modulus is reduced by 24–29 %. However, the ratio between the Young´s modulus and the characteristic compressive strength of earth block masonry ranges between E33/fk = 283–583 but is largely independent of the relative humidity. The results show that the mechanical properties of the investigated unstabilised earth block masonry are sufficient for load-bearing structures, yielding a masonry compressive strength between 2.3 MPa and 3.7 MPa throughout the range of moisture contents investigated. In general, the design concept of conventional masonry can be adapted for unstabilised earth masonry provided that the rather low Young´s modulus as well as the moisture dependence of both, compressive strength and Young´s modulus, are sufficiently taken into account. KW - Compressive strength KW - Earth block masonry KW - Compression tests KW - Stress-strain relation KW - Relative humidity KW - Moisture content PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562417 DO - https://doi.org/10.1016/j.cscm.2022.e01663 SN - 2214-5095 VL - 17 SP - 1 EP - 15 PB - Elsevier B.V. CY - Netherlands AN - OPUS4-56241 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meng, Xiangmeng A1 - Putra, Stephen Nugraha A1 - Bachmann, Marcel A1 - Artinov, Antoni A1 - Rethmeier, Michael T1 - Influence of the free surface reconstruction on the spatial laser energy distribution in high power laser beam welding modeling N2 - An accurate and efficient description of the spatial distribution of laser energy is a crucial factor for the modeling of laser material processing, e.g., laser welding, laser cutting, or laser-based additive manufacturing. In this study, a 3D heat transfer and fluid flow model coupled with the volume-of-fluid algorithm for free surface tracking is developed for the simulation of molten pool dynamics in high-power laser beam welding. The underlying laser-material interactions, i.e., the multiple reflections and Fresnel absorption, are considered by a raytracing method. Two strategies of free surface reconstruction used in the ray-tracing method are investigated: a typical piecewise linear interface calculation (PLIC)-based method and a novel localized level-set method. The PLIC-based method is discrete, resulting in noncontinuous free surface reconstruction. In the localized level-set method, a continuous free surface is reconstructed, and, thus, the exact reflection points can be determined. The calculated spatial laser energy distribution and the corresponding molten pool dynamics from the two methods are analyzed and compared. The obtained numerical results are evaluated with experimental measurements to assure the validity of the proposed model. It is found that distinct patterns of the beam multiple reflections are obtained with the different free surface reconstructions, which shows significant influence not only on the molten pool behaviors but also on the localized keyhole dynamics. KW - Laser beam welding KW - Laser energy distribution KW - Weld pool dynamics KW - Ray teacing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562429 DO - https://doi.org/10.2351/7.0000739 SN - 1042-346X VL - 34 IS - 4 SP - 042023-1 EP - 042023-8 PB - Laser Institute of America CY - Orlando, Fla. AN - OPUS4-56242 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schoknecht, Ute A1 - Kalbe, Ute A1 - Heisterkamp, I. A1 - Kretzschmar, M. A1 - Gartiser, S. A1 - Happel, O. A1 - Ilvonen, O. T1 - Release of substances from joint grouts based on various binder types and their ecotoxic effects N2 - Background: The leaching of substances and the ecotoxic effects of eluates were studied for joint grouts that are based on various types of binders. Eight products, two of them containing either epoxy resin, polybutadiene or polyurethane binders, or modifed cement, were investigated using harmonized leaching tests for construction products in combination with ecotoxicity tests on algae, daphnia, luminescent bacteria, fish eggs and mutagenicity in accordance with CEN/TR 17105. In addition to basic parameters, such as pH, TOC, and inorganic components, organic substances in the eluates were analysed by gas and liquid chromatography in combination with mass spectrometry. Quantitative analyses in combination with ecotoxicity data on selected substances were used to deduce which substances cause the observed ecotoxic effects. Results: Different patterns of ecotoxic effects were observed in joint grouts with different binder types. The most ecotoxic effects were observed in epoxy resin-based products, followed by polybutadiene-based products. Fewer ecotoxic effects were observed in polyurethane-based products and modifed cements. Some of these showed no ecotoxicity. Some of the substances in the eluates were identified and related to ecotoxic effects. 4-Tert-butylphenol and amines probably contributed to the ecotoxic effects of at least one of the epoxy resin-based renders, whereas cobalt is assumed to contribute to the toxic effect on algae of one of the polybutadiene-based products. However, only some of the leached substances could be identifed, and only some of the ecotoxic effects can be explained by the available information on the composition of eluates and known ecotoxic profiles of the identified substances. Conclusions: Ecotoxicity tests on eluates from leaching tests indicate whether environmentally hazardous substances can be leached from construction products. Combined ecotoxicity tests and chemical analysis of eluates from EU-wide harmonized leaching tests for construction products can provide information on substances that cause these effects. This supports the identifcation and development of environmentally friendly construction products. This study confirmed that ecotoxicity tests in accordance with CEN/TR 17105 are a tool well-suited to support the implementation of the European Commission’s zero pollution vision for 2050 and to reduce pollution to levels no longer considered harmful to health and natural ecosystems. KW - Joint grouts KW - Leaching KW - Ecotoxixity PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562392 DO - https://doi.org/10.1186/s12302-022-00686-0 SN - 2190-4707 VL - 34 IS - 1 SP - 1 EP - 16 PB - Springer Nature CY - Berlin AN - OPUS4-56239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Serrano Munoz, Itziar A1 - Magnier, V. A1 - Brunel, F. A1 - Dufrenoy, P. T1 - Influence of the Composition on the Compressive Behaviour of a Semi-Metallic Brake-Pad Material N2 - The contact interface between the rotation and static part of a friction brake is central to the optimal functioning of the brake system due to the occurrence of heat dissipation, mechanical interaction and thermal exchanges. Generally, braking performances are evaluated by the energetic efficiency and wear rates of the contact surface. However, the compressive behaviour of the contact materials has also a significant contribution to the overall performances. In this work, the meso- and microscopic compressive behaviour of a sintered semi-metallic brake-pad material is investigated mainly via compression testing coupled with Digital Image Correlation (DIC) technique, as well as optical and scanning electron microscopy (SEM) analysis. The composition of a reference material (RM) is simplified to a selection of nine components, as opposed to up to thirty components typically used in commercial brake-pad materials. The retained components are considered as the most crucial for safe-operating performances. At the studied stress levels, the RM material is flexible (E = 5330 MPa), deformable (Ezz−plastic = −0.21%), and exhibits hysteresis loops. Subsequently, the contribution to the mechanical response of each individual component is investigated by producing the so-called dissociated materials, where the number of components is, at a time, further reduced. It is observed that the macroscopic behaviour is mainly controlled by the content (i.e., size distribution, shape and nature) of graphite particles, and that the hysteresis is only related to one of the two types of graphite used (G2 particles). Moreover, RM containing 13 wt% of G2 particles embedded in a relatively soft matrix (10.86 GPa) is able to increase the hysteresis (by 35%) when compared to the dissociated material containing 20 wt% of G2 particles which is embedded in a stiffer matrix (E = 106 GPa). KW - Semi-metallic brake-pad material KW - Powder metallurgy KW - Components influence KW - Graphite induced hysteresis KW - Digital image correlation (DIC) KW - Compression testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562003 DO - https://doi.org/10.3390/ma15227911 VL - 15 IS - 22 SP - 7911 PB - MDPI AN - OPUS4-56200 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schoknecht, Ute A1 - Mathies, H. T1 - The Impact of Weather Conditions on Biocides in Paints N2 - Weather conditions affect biocides on exposed outer surfaces on constructions. Contact with water causes hydrolysis and leaching of substances. Ultraviolet radiation may induce photolysis. As a result, a mixture of biocidal active substances and transformation products can be emitted into the environment. In a semi-field study, leaching of the biocidal active substances terbutryn, diuron, octylisothiazolinone, carbendazim, and selected transformation products was observed for two paints containing either a white or a red pigment. Painted test panels were exposed to natural weathering for about 1.5 years. Runoff samples were analyzed during the course of the experiment. At the end of the study, residues of biocidal active substances and transformation products were determined in sections of the test panels. Emissions of substances were mainly observed during the first few months of the experiments. Increased emissions of transformation products were observed during periods of increased global radiation and subsequent periods with relatively high amounts of driving rain. Different patterns of transformation products were observed, especially for terbutryn, both for paints containing different pigments and in experiments that were started in different periods of the year, as well as during different periods of the experiments. KW - Substance release KW - Construction products KW - Biocides KW - Transformation KW - Weathering KW - Driving rain KW - Global radiation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560651 DO - https://doi.org/10.3390/ma15207368 VL - 15 IS - 20 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-56065 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Van Tran, K. A1 - Woracek, R. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Abou-Ras, D. A1 - Puplampu, S. A1 - Förster, C. A1 - Penumadu, D. A1 - Dahlberg, C. F. O. A1 - Banhart, J. A1 - Manke, I. T1 - Torsion of a rectangular bar: Complex phase distribution in 304L steel revealed by neutron tomography N2 - Metastable austenitic stainless steel (304L) samples with a rectangular cross-section were plastically deformed in torsion during which they experienced multiaxial stresses that led to a complex martensitic phase distribution owing to the transformation induced plasticity effect. A three-dimensional characterization of the phase distributions in these cm-sized samples was carried out by wavelength-selective neutron tomography. It was found that quantitatively correct results are obtained as long as the samples do not exhibit any considerable preferential grain orientation. Optical microscopy, electron backscatter diffraction, and finite element modeling were used to verify and explain the results obtained by neutron tomography. Altogether, neutron tomography was shown to extend the range of microstructure characterization methods towards the meso- and macroscale. KW - Neutron tomography KW - Phase distribution KW - Rectangular cross-section KW - Torsion KW - Geometrical effect PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561649 DO - https://doi.org/10.1016/j.matdes.2022.111037 SN - 0264-1275 VL - 222 SP - 111037 PB - Elsevier Ltd. AN - OPUS4-56164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Costabel, S. A1 - Hiller, Thomas A1 - Dlugosch, R. A1 - Kruschwitz, Sabine A1 - Müller Petke, M. T1 - Evaluation of single-sided nuclear magnetic resonance technology for usage in geosciences N2 - Because of its mobility and ability to investigate exposed surfaces, single-sided (SiS) nuclear magnetic resonance (NMR) technology enables new application fields in geosciences. To test and assess its corresponding potential, we compare longitudinal (T1) and transverse (T2) data measured by SiS NMR with those of conventional geoscientific laboratory NMR. We use reference sandstone samples covering a broad range of pore sizes. Our study demonstrates that the lower signal-to-noise ratio of SiS NMR data generally tends to slightly overestimated widths of relaxation time distributions and consequently pore size distributions. While SiS and conventional NMR produce very similar T1 relaxation data, unbiased SiS NMR results for T2 measurements can only be expected for fine material, i.e. clayey or silty sediments and soils with main relaxation times below 0.05s. This limit is given by the diffusion relaxation rate due to the gradient in the primary magnetic field associated with the SiS NMR. Above that limit, i.e. for coarse material, the relaxation data is strongly attenuated. If considering the diffusion relaxation time of 0.2 s in the numerical data inversion process, the information content >0.2s is blurred over a range larger than that of conventional NMR. However, our results show that principle range and magnitudes of the relaxation time distributions are reconstructed to some extent. Regarding these findings, SiS NMR can be helpful to solve geoscientific issues, e.g. to assess the hydro-mechanical properties of the walls of underground facilities or to provide local soil moisture data sets for calibrating indirect remote techniques on the regional scale. The greatest opportunity provided by the SiS NMR technology is the acquisition of profile relaxation data for rocks with significant bedding structures at the µm scale. With this unique feature, SiS NMR can support the understanding and modeling of hydraulic and diffusional anisotropy behavior of sedimentary rocks. KW - Single-sided NMR KW - Geosciences KW - Nuclear magnetic resonance PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561676 DO - https://doi.org/10.1088/1361-6501/ac9800 SN - 0957-0233 VL - 34 IS - 1 SP - 1 EP - 13 PB - IOP Publishing AN - OPUS4-56167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chen, Yue A1 - Schilling, Markus A1 - von Hartrott, P. A1 - Beygi Nasrabadi, Hossein A1 - Skrotzki, Birgit A1 - Olbricht, Jürgen T1 - Ontopanel: A Tool for Domain Experts Facilitating Visual Ontology Development and Mapping for FAIR Data Sharing in Materials Testing N2 - In recent years, the design and development of materials are strongly interconnected with the development of digital technologies. In this respect, efficient data management is the building block of material digitization and, in the field of materials science and engineering (MSE), effective solutions for data standardization and sharing of different digital resources are needed. Therefore, ontologies are applied that represent a map of MSE concepts and relationships between them. Among different ontology development approaches, graphical editing based on standard conceptual modeling languages is increasingly used due to its intuitiveness and simplicity. This approach is also adopted by the Materials-open-Laboratory project (Mat-o-Lab), which aims to develop domain ontologies and method graphs in accordance with testing standards in the field of MSE. To suit the actual demands of domain experts in the project, Ontopanel was created as a plugin for the popular open-source graphical editor diagrams.net to enable graphical ontology editing. It includes a set of pipeline tools to foster ontology development in diagrams.net, comprising imports and reusage of ontologies, converting diagrams to Web Ontology Language (OWL), verifying diagrams using OWL rules, and mapping data. It reduces learning costs by eliminating the need for domain experts to switch between various tools. Brinell hardness testing is chosen in this study as a use case to demonstrate the utilization of Ontopanel. KW - Materials Testing KW - Ontology KW - Visual ontology development KW - Data mapping KW - FAIR PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560339 DO - https://doi.org/10.1007/s40192-022-00279-y SP - 1 EP - 12 PB - Springer AN - OPUS4-56033 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ermilova, Elena A1 - Weise, Matthias A1 - Hertwig, Andreas T1 - Hybrid optical measurement technique for detection of defects in epitaxially grown 4H-SiC layers N2 - Recent developments in power electronics require the use of new wide bandgap compound semiconductor. We demonstrate the use of the ellipsometry and white light interference microscopy to detect defects in epitaxially grown SiC layers on SiC substrates. Such hybrid optical metrology methods can be used to better understand the mechanism of the development of the defects as well as their effects on the material´s optoelectronic properties. T2 - EOS Annual Meeting (EOSAM 2022) CY - Porto, Portugal DA - 12.09.2022 KW - Imaging ellipsometry KW - White light interference microscopy KW - Wide bandgap compound semiconductor KW - Epitaxially grown 4H-SiC layers PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561113 DO - https://doi.org/10.1051/epjconf/202226610001 VL - 266 SP - 1 EP - 2 AN - OPUS4-56111 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shaheen, Sabahat A1 - Hicke, Konstantin T1 - Measurement of Geometric Phase using a φ-OTDR setup N2 - Geometric phase showing sensitivity to changes in polarisation state and intensity of backscattered light is measured using a novel φ-OTDR setup based on coherent heterodyne detection. Principle is demonstrated using a polarisation scrambler inline a fiber-under-test. T2 - Optical Fiber Sensors 2022 CY - Alexandria, Virginia, United States DA - 29.08.2022 KW - Coherent Heterodyne KW - Geometric Phase KW - Distributed Fiber Optic Sensor PY - 2022 SN - 978-1-957171-14-2 SP - W4.72 AN - OPUS4-56116 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sieber, M. J. A1 - Wilke, M. A1 - Appelt, O. A1 - Oelze, Marcus A1 - Koch-Müller, M. T1 - Melting relations of Ca–Mg carbonates and trace element signature of carbonate melts up to 9 GPa – A proxy for melting of carbonated mantle lithologies N2 - The most profound consequences of the presence of Ca–Mg carbonates (CaCO3–MgCO3) in the Earth’s upper mantle may be to lower the melting temperatures of the mantle and control the melt composition. Low-degree partial melting of a carbonate-bearing mantle produces CO2-rich, silica-poor melts compositionally imposed by the melting relations of carbonates. Thus, understanding the melting relations in the CaCO3–MgCO3 system facilitates the interpretation of natural carbonate-bearing silicate systems. We report the melting relations of the CaCO3–MgCO3 system and the partition coefficient of trace elements between carbonates and carbonate melt from experiments at high pressure (6 and 9 GPa) and temperature (1300–1800 ◦C) using a rocking multi-anvil press. In the absence of water, Ca–Mg carbonates are stable along geothermal gradients typical of subducting slabs. Ca–Mg carbonates (∼ Mg0.1–0.9Ca0.9–0.1CO3) partially melt beneath mid-ocean ridges and in plume settings. Ca–Mg carbonates melt incongruently, forming periclase crystals and carbonate melt between 4 and 9 GPa. Furthermore, we show that the rare earth element (REE) signature of Group-I kimberlites, namely strong REE fractionation and depletion of heavy REE relative to the primitive mantle, is resembled by carbonate melt in equilibrium with Ca-bearing magnesite and periclase at 6 and 9 GPa. This suggests that the dolomite–magnesite join of the CaCO3–MgCO3 system might be useful to approximate the REE signature of carbonate-rich melts parental to kimberlites. KW - High pressure experiments KW - Laser Ablation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561197 DO - https://doi.org/10.5194/ejm-34-411-2022 SN - 0935-1221 VL - 34 IS - 5 SP - 411 EP - 424 PB - Copernicus Publications CY - Göttingen AN - OPUS4-56119 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schwarz, W. A1 - Wilsch, Gerd A1 - Katsumi, N. A1 - Ebell, Gino A1 - Völker, Tobias T1 - Ion distribution in concrete overlay, mapped by laser induced breakdown spectroscopy (LIBS), modified by an embedded zinc anode N2 - Galvanic corrosion protection by embedded zinc anodes is an accepted technique for the corrosion protection of reinforcing steel in concrete. Galvanic currents flow between the zinc anode and the steel reinforcement due to the potential difference that is in the range of a few hundred mV. The ion distribution was studied on two steel reinforced concrete specimens admixed with 3 wt.% chloride/wt. cement and galvanically protected by a surface applied EZ-anode. On both specimens, a zinc anode was embedded and glued to the concrete surface by a geo-polymer-based chloride-free binder. At one specimen, the EZ-anode was operated for 2,5 years, the EZ-anode at the other specimen was not electrically connected to the reinforcement, this specimen serves as a reference. Both specimens have been stored under identical conditions. The ion distribution between the anode (EZ-ANODE) and cathode (steel reinforcement) was studied by laser-induced breakdown spectroscopy (LIBS) after 7 months, 12 months, and 2,5 years. Results of the LIBS studies on the specimen with activated EZ-anode after 7 months, 12 months, and 2,5 years and of the reference specimen after 2,5 years are reported. Results show that diffusion of ions contributes to the changes in the ion distribution but migration, especially of chlorides towards the EZ-anode is significant despite the weak electric field – several hundred millivolts - generated by the galvanic current. Results show that chloride ions accumulate near the zinc-anode as in water-insoluble zinc-hydroxy chlorides - Simonkollite. T2 - ICCRRR 2022 CY - Capetown, South Africa KW - Corrosion KW - LIBS KW - Zinc KW - Anode PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560576 DO - https://doi.org/10.1051/matecconf/202236404023 SN - 2261-236X VL - 364 SP - 1 EP - 7 PB - EDP Sciences CY - Les Ulis AN - OPUS4-56057 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ewert, U. A1 - Jaenisch, Gerd-Rüdiger A1 - Schumacher, David A1 - Bircher, B. A1 - Meli, F. A1 - Deresch, A. T1 - EMPIR-Projekt NanoXSpot: Neue Normentwürfe für die Brennfleckmessung an Röntgenröhren im Makro-, Mikro- und Nanometerbereich für Hersteller und Anwender N2 - Im Rahmen des EMPIR-Projektes NanoXSpot (Nanometre X-ray Focal Spot Measurement) werden rückführbare Messverfahren zur Bestimmung der Brennfleckgröße und -form von Röntgenröhren im Bereich von 100 nm bis 10 mm entwickelt, welche die Grundlage für die Erarbeitung mehrerer Normentwürfe bilden. Diese werden 2022 parallel bei ISO TC 135 (NDT) SC 5 (RT) und CEN TC 138 (NDT) WG 1 (RT) eingereicht. Entsprechende Normen werden auch bei ASTM vorgestellt. Die Norm EN 12543-4 (Kantenmethode) wird umgeschrieben für die Messung von Brennflecken von 1 μm – 10 mm durch Auswertung von Loch- oder Scheibenaufnahmen. Der im Rahmen des NanoXSpot-Projektes neu entwickelte NxS-Testkörper ist geeignet für den Bereich von 1 μm – 100 μm. Von 100 μm bis 10 mm können ASTM-Lochtestkörper verwendet werden, die bereits bei ASTM E 1165 beschrieben sind. Neu ist die Anwendung eines CT-Algorithmus zur Rekonstruktion der Brennflecke, um Lochblenden-basierte Brennfleckkameras, insbesondere im Bereich unter 100 μm, zu ersetzen. Ein neuer Normteil, EN 12543-6, wurde entworfen, um die Brennfleckmessung im Bereich 100 nm – 20 μm mit hoher Genauigkeit zu ermöglichen. Verschiedene Strichgruppen-Testkörper kommen hier zum Einsatz. Das sind die JIMAPrüfkörper, ein neuer Hochkontrast-Strichgruppentestkörper von YXLON (HiCo) und der neu entwickelte Testkörper NxS. Diese werden vorgestellt. Die Messprozedur für Röhrenhersteller wird auf einer numerischen Fit-Prozedur basieren, die über einen Ringversuch im Projekt validiert wurde. Beide Normen benötigen numerische Auswertealgorithmen zur korrekten Anwendung, die als kommerzielle Software und Public Domain – Software verfügbar gemacht werden. Es wird über die zu erwartenden Standardprozeduren und die erforderliche Hardware zur Anwendung der Normen informiert. T2 - DGZfP-Jahrestagung CY - Kassel, Germany DA - 23.05.2022 KW - Röntgenröhre KW - Brennfleckmessung KW - Normung PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561029 SP - 1 EP - 10 AN - OPUS4-56102 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schumacher, David A1 - Jaenisch, Gerd-Rüdiger A1 - Ewert, U. A1 - Bircher, B. A1 - Meli, F. A1 - Sofiienko, A. A1 - Steffen, J. P. A1 - Deresch, A. T1 - EMPIR-Projekt NanoXSpot: Ringversuch zur Untersuchung der neu entwickelten Methoden für die Brennfleckmessung an Röntgenröhren im Mikro- und Nanometerbereich N2 - Im Rahmen des EMPIR-Projektes NanoXSpot (Nanometre X-Ray Focal Spot Measurement) werden rückführbare Messverfahren zur Bestimmung der Brennfleckgröße und -form von Röntgenröhren mit Submikrometerauflösung (100 nm – 20 μm) entwickelt, die die Grundlage für die Erarbeitung eines Standardentwurfes bilden. Der Standardentwurf wird bei CEN TC 138 (Non-destructive testing) WG 1 (Radiographic testing) eingereicht und mit ISO und ASTM harmonisiert. Zur Untersuchung der entwickelten Methoden (Brennfleck-CT, Fit-Prozedur für Strichgruppenkörper) und des im Projekt NanoXSpot neu entworfenen Testkörpers, NxS, wurde ein Ringversuch durchgeführt. Dabei wurde sowohl der angestrebte Überlappungsbereich mit EN 12543 Teil 5 (Messung der effektiven Brennfleckgröße von Mini- und Mikrofokus-Röntgenröhren) und ASTM E 2903 (Standard Test Method for Measurement of the Effective Focal Spot Size of Mini and Micro Focus X-ray Tubes) für Brennflecke >5 μm als auch Brennflecke <5 μm untersucht. Im Mittelpunkt standen dabei Stabilität und Wiederholbarkeit der entwickelten Methoden zur Bestimmung der Brennfleckgröße. In diesem Beitrag werden die Ergebnisse des durchgeführten Ringversuches vorgestellt und diskutiert, um Schlussfolgerungen und Empfehlungen für die Vorbereitung eines erweiterten Ringversuchs mit Partnern und Stakeholdern abzuleiten. T2 - DGZfP-Jahrestagung CY - Kassel, Germany DA - 23.05.2022 KW - Brennfleckmessung KW - Computer-Tomografie KW - EMPIR KW - Normung PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561037 SP - 1 EP - 2 AN - OPUS4-56103 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Silveira, A. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Longo, E. A1 - Greving, I. A1 - Lasch, P. A1 - Shahar, R A1 - Zaslansky, P. T1 - Water flow through bone: Neutron tomography reveals differences in water permeability between osteocytic and anosteocytic bone material N2 - Vertebrate bones are made of a nanocomposite consisting of water, mineral and organics. Water helps bone material withstand mechanical stress and participates in sensation of external loads. Water diffusion across vertebrae of medaka (bone material lacking osteocytes) and zebrafish (bone material containing osteocytes) was compared using neutron tomography. Samples were measured both wet and following immersion in deuterated-water (D2O). By quantifying H+ exchange and mutual alignment with X-ray lCT scans, the amount of water expelled from complete vertebra was determined. The findings revealed that anosteocytic bone material is almost twice as amenable to D2O diffusion and H2O exchange, and that unexpectedly, far more water is retained in osteocytic zebrafish bone. Diffusion in osteocytic bones (only 33 % – 39 % water expelled) is therefore restricted as compared to anosteocytic bone (~ 60 % of water expelled), presumably because water flow is confined to the lacunar-canalicular network (LCN) open-pore system. Histology and Raman spectroscopy showed that anosteocytic bone contains less proteoglycans than osteocytic bone. These findings identify a previously unknown functional difference between the two bone materials. Therefore, this study proposes that osteocytic bone retains water, aided by non-collagenous proteins, which contribute to its poroelastic mechano-transduction of water flow confined inside the LCN porosity. KW - Bone porosity KW - Anosteocytic bone KW - Water permeability KW - Neutron tomography KW - Proteoglycans PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564563 DO - https://doi.org/10.1016/j.matdes.2022.111275 VL - 224 SP - 1 EP - 13 PB - Elsevier Ltd. AN - OPUS4-56456 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Z. A1 - Dong, K. A1 - Mazzio, K. A. A1 - Hilger, A. A1 - Markötter, Henning A1 - Wilde, F. A1 - Heinemann, T. A1 - Manke, I. A1 - Adelhelm, P. T1 - Phase transformation and microstructural evolution of CuS electrodes in solid-state batteries probed by in situ 3D X-ray tomography N2 - Copper sulfide shows some unique physico-chemical properties that make it appealing as a cathode active material (CAM) for solid-state batteries (SSBs). The most peculiar feature of the electrode reaction is the reversible formation of μm-sized Cu crystals during cycling, despite its large theoretical volume change (75%). Here, the dynamic microstructural evolution of CuS cathodes in SSBs is studied using in situ synchrotron X-ray tomography. The formation of μm-sized Cu within the CAM particles can be clearly followed. This process is accompanied by crack formation that can be prevented by increasing the stack pressure from 26 to 40 MPa. Both the Cu inclusions and cracks show a preferential orientation perpendicular to the cell stack pressure, which can be a result of a z-oriented expansion of the CAM particles during lithiation. In addition, cycling leads to a z-oriented reversible displacement of the cathode pellet, which is linked to the plating/stripping of the Li counter electrode. The pronounced structural changes cause pressure changes of up to 6 MPa within the cell, as determined by operando stack pressure measurements. Reasons for the reversibility of the electrode reaction are discussed and are attributed to the favorable combination of soft materials. KW - Copper sulfide KW - Crack evolution KW - Digital volume correlation KW - Phase transformation KW - Solid-state batteries PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564577 DO - https://doi.org/10.1002/aenm.202203143 IS - 2203143 SP - 1 EP - 12 PB - Wiley VHC-Verlag AN - OPUS4-56457 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - El-Batahgy, A. A1 - Elkousy, M. A1 - Al-Rahman, A. A1 - Gumenyuk, Andrey A1 - Rethmeier, Michael A1 - Gook, S. T1 - Retaining Mechanical Properties of GMA-Welded Joints of 9%Ni Steel Using Experimentally Produced Matching Ferritic Filler Metal N2 - Motivated by the loss of tensile strength in 9%Ni steel arc-welded joints performed using commercially available Ni-based austenitic filler metals, the viability of retaining tensile strength using an experimentally produced matching ferritic filler metal was confirmed. Compared to the austenitic Ni-based filler metal (685 MPa), higher tensile strength in gas metal arc (GMA) welded joints was achieved using a ferritic filler metal (749 MPa) due to its microstructure being similar to the base metal (645 MPa). The microstructure of hard martensite resulted in an impact energy of 71 J (-196 °C), which was two times higher than the specified minimum value of _>34 J. The tensile and impact strength of the welded joint is affected not only by its microstructure, but also by the degree of its mechanical mismatch depending on the type of filler metal. Welds with a harder microstructure and less mechanical mismatch are important for achieving an adequate combination of tensile strength and notched impact strength. This is achievable with the cost-effective ferritic filler metal. A more desirable combination of mechanical properties is guaranteed by applying low preheating temperature (200 °C), which is a more practicable and economical solution compared to the high post-weld heat treatment (PWHT) temperature (580 °C) suggested by other research. KW - 9%Ni steel KW - Ni-based austenitic filler metal KW - Mechanical mismatching KW - Microstructure KW - Post-weld heat treatment KW - Preheating KW - Matching ferritic filler metal PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564610 DO - https://doi.org/10.3390/ma15238538 SN - 1996-1944 VL - 15 IS - 23 SP - 1 EP - 14 PB - MDPI AN - OPUS4-56461 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Garrido, E. A1 - Hernández-Sigüenza, G. A1 - Climent, Estela A1 - Marcos, M. D. A1 - Rurack, Knut A1 - Gaviña, P. A1 - Parra, M. A1 - Sancenón, F. A1 - Martí-Centelles, V. A1 - Martínez-Máñez, R. T1 - Strip-based lateral flow-type indicator displacement assay for γ-hydroxybutyric acid (GHB) detection in beverages N2 - The use of gamma-hydroxybutyric acid (GHB) in drug-facilitated sexual assault has increased due to its availability and high solubility in aqueous solutions and alcoholic beverages, necessitating the development of rapid methods for GHB detection. In this respect, portable testing methods for use in the field, based on lateral flow assays (LFAs) and capable of detecting trace concentrations of target analytes, are particularly attractive and hold enormous potential for the detection of illicit drugs. Using this strategy, here we report a rapid, low cost, easy-to-handle strip-based LFA for GHB analysis employing a smartphone for fluorescence readout. At molecular signalling level, the ensemble is based on a Cu2+ complex with a tetradentate ligand and the fluorescent dye coumarin 343, which indicate GHB through an indicator displacement assay (IDA) in aqueous solution. When incorporated in a LFA-based strip test this system shows a detection limit as low as 0.03 μM for GHB in MES buffer solution and is able to detect GHB at concentrations of 0.1 μM in soft drinks and alcoholic beverages in only 1 min. KW - Indicator displacement assay KW - Gamma-hydroxybutyric acid KW - Lateral flow assay KW - Test strip KW - Fluorescent dyes KW - Smartphone readout PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564631 DO - https://doi.org/10.1016/j.snb.2022.133043 SN - 0925-4005 VL - 377 SP - 1 EP - 7 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-56463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kömmling, Anja A1 - Grelle, Tobias A1 - Jaunich, Matthias A1 - Goral, Milan A1 - Wolff, Dietmar T1 - Three-dimensional thermal expansion of neat and irradiated (U)HMWPE materials at elevated temperatures N2 - The thermal expansion of polymeric parts can be an issue in many applications where the available space is limited, or exact dimensions of the part are required. For this study, a device was designed and built that allowed measuring the thermal expansion simultaneously in all three spatial directions on cubic samples with real-scale dimensions (78 mm edge length). The results are shown between 25 °C and 125 °C for two PE materials, one HMWPE and one tempered UHMWPE, for non-irradiated samples as well as cubes that have been irradiated with 100 and 400 kGy. The results measured with the new device were very similar to those measured with conventional thermo-mechanical analysis equipment and to literature data of UHMWPE. The HMWPE material shows a much larger thermal expansion coefficient in one direction compared to the other two directions during the first heating due to frozen stresses from the pressing step during material manufacturing. These stresses are mostly released by the expansion during the first heating, so that the expansion during the second heating is more uniform. The overall volumetric expansion is the same for both heating runs. By contrast, the tempered UHMWPE material shows no significant difference between first and second heating run, as the stresses from processing could already relax in the tempering step. The irradiation treatment does not affect the values significantly for the given test set-up. KW - Lupolen KW - Ultra high molecular weight polyethylene KW - GUR KW - Coefficient of thermal expansion KW - High temperature PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563987 DO - https://doi.org/10.1016/j.polymertesting.2022.107841 SN - 0142-9418 VL - 117 SP - 1 EP - 8 PB - Elsevier Ltd. AN - OPUS4-56398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Nietzke, Jonathan A1 - Richter, Tim A1 - Mente, Tobias A1 - Mayr, P A1 - Nitsche, A T1 - Hydrogen effect on mechanical properties and cracking of creep‑resistant 9% Cr P92 steel and P91 weld metal N2 - Martensitic 9% Cr steels like P91 and P92 can show an increased susceptibility to delayed hydrogen-assisted cracking. The focus of this study was the microstructure and heat treatment efect on the mechanical properties of P92 base material and P91 multi-layer weld metal in both as-welded and post weld heat treated (PWHT) condition. Tensile tests with hydrogen free reference samples and electrochemically hydrogen charged samples were carried out; the mechanical properties were assessed and supported by detailed fractographic analysis. Finally, a hydrogen and microstructure-dependent fracture criterion is established. All investigated microstructures showed a hydrogen-infuenced degradation of the mechanical properties compared to the hydrogen-free reference samples. The as-welded martensitic P91 weld metal had the highest degree of degradation in the presence of hydrogen. The P91 PWHT weld metal and the P92 base material had comparable properties. From that point of view, a signifcantly increased risk for hydrogen-assisted cold cracking during welding fabrication of P91 weld joints must be considered before any heat treatment is conducted. T2 - IIW Annual Assembly, Meeting of Commission IX-C CY - Tokyo, Japan DA - 16.07.2022 KW - Creep-resisting materials KW - Welding KW - Hydrogen assisted cracking KW - Hydrogen embrittlement KW - Mechanical properties PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564070 DO - https://doi.org/10.1007/s40194-022-01410-5 SN - 0043-2288 SP - 1 EP - 12 PB - Springer Nature CY - Basel (CH) AN - OPUS4-56407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Klewe, Tim T1 - Comparison of the Calcium Carbide Method and Darr Drying to Quantify the Amount of Chemically Bound Water in Early Age Concrete N2 - Hydration is the exothermic reaction between anhydrous cement and water, which forms the solid cement matrix of concrete. Being able to evaluate the hydration is of high interest for the use of both conventional and more climate-friendly building materials. The experimental monitoring is based on temperature or moisture measurements. The first needs adiabatic conditions, which can only be achieved in laboratory. The latter is often measured comparing the weight of the material sample before and after oven drying, which is time-consuming. This study investigates the moisture content of two cement-based and two calcium sulphate based mixtures for the first 90 days by using the calcium carbide method and oven drying at 40 °C and 105 °C (Darr method). Thereby, the amount of chemically bound water is determined to derive the degree of hydration. The calcium carbide measurements highly coincide with oven drying at 40 °C. The calcium carbide method is therefore evaluated as a suitable alternative to the time-consuming Darr drying. The prompt results are seen as a remarkable advantage and can be obtained easily in laboratory as well as in the field. KW - Concrete KW - Hydration KW - Material moisture KW - Calcium carbide method KW - Bound water KW - Darr method KW - Oven drying KW - Chemisorption KW - Physisorption PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564519 DO - https://doi.org/10.3390/ma15238422 VL - 15 IS - 23 SP - 1 EP - 16 PB - MDPI AN - OPUS4-56451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Junge, P. A1 - Greinacher, M. A1 - Kober, D. A1 - Stargardt, Patrick A1 - Rupprecht, C. T1 - Metastable Phase Formation, Microstructure, and Dielectric Properties in Plasma-Sprayed Alumina Ceramic Coatings N2 - The need for new solutions for electrical insulation is growing due to the increased electrification in numerous industrial sectors, opening the door for innovation. Plasma spraying is a fast and efficient way to deposit various ceramics as electrical insulators, which are used in conditions where polymers are not suitable. Alumina (Al2O3) is among the most employed ceramics in the coating industry since it exhibits good dielectric properties, high hardness, and high melting point, while still being cost-effective. Various parameters (e.g., feedstock type, spray distance, plasma power) significantly influence the resulting coating in terms of microstructure, porosity, and metastable phase formation. Consequently, these parameters need to be investigated to estimate the impact on the dielectric properties of plasma-sprayed alumina coatings. In this work, alumina coatings with different spray distances have been prepared via atmospheric plasma spray (APS) on copper substrates. The microstructure, porosity, and corresponding phase formation have been analyzed with optical microscopy, X-ray diffraction (XRD), and scanning electron microscopy (SEM). Moreover, we present an in-depth analysis of the fundamental dielectric properties e.g., direct current (DC) resistance, breakdown strength, dielectric loss tangent, and permittivity. Our results show that decreasing spray distance reduces the resistivity from 6.31 × 109 Ωm (130 mm) to 6.33 × 108 Ωm (70 mm), while at the same time enhances the formation of the metastable δ-Al2O3 phase. Furthermore, space charge polarization is determined as the main polarization mechanism at low frequencies. KW - Alumina KW - Plasma spray KW - Dielectric properties PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564394 DO - https://doi.org/10.3390/coatings12121847 SN - 2079-6412 VL - 12 SP - 1 EP - 15 PB - MDPI CY - Basel AN - OPUS4-56439 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pinomaa, T. A1 - Lindroos, M. A1 - Jreidini, P. A1 - Haapalehto, M. A1 - Ammar, K. A1 - Wang, Lei A1 - Forest, S. A1 - Provatas, N. A1 - Laukkanen, A. T1 - Multiscale analysis of crystalline defect formation in rapid solidification of pure aluminium and aluminium-copper alloys N2 - Rapid solidification leads to unique microstructural features, where a less studied topic is the formation of various crystalline defects, including high dislocation densities, as well as gradients and splitting of the crystalline orientation. As these defects critically affect the material’s mechanical properties and performance features, it is important to understand the defect formation mechanisms, and how they depend on the solidification conditions and alloying. To illuminate the formation mechanisms of the rapid solidification induced crystalline defects, we conduct a multiscale modelling analysis consisting of bond-order potential-based molecular dynamics (MD), phase field crystal-based amplitude expansion simulations, and sequentially coupled phase field–crystal plasticity simulations. The resulting dislocation densities are quantified and compared to past experiments. The atomistic approaches (MD, PFC) can be used to calibrate continuum level crystal plasticity models, and the framework adds mechanistic insights arising from the multiscale analysis. This article is part of the theme issue ‘Transport phenomena in complex systems (part 2)’. KW - Rapid solidification KW - Crystalline defects KW - Molecular dynamics KW - Phase field crystal KW - Phase field method KW - Crystal plasticity PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542156 DO - https://doi.org/10.1098/rsta.2020.0319 SN - 1364-503X VL - 380 IS - 2217 SP - 1 EP - 20 PB - Royal Society CY - London AN - OPUS4-54215 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schoknecht, Ute A1 - Tietje, O. A1 - Borho, N. A1 - Burkhardt, M. A1 - Rohr, M. A1 - Vollpracht, A. A1 - Weiler, L. T1 - Environmental impact of construction products on aquatic systems - Principles of an integrated source-path-target concept N2 - Buildings exposed to water can release undesirable substances which, once transported to environmental compartments, may cause unwanted effects. These exposure pathways need to be investigated and included in risk assessments to safeguard water quality and promote the sustainability of construction materials. The applied materials, exposure conditions, distribution routes and resilience of receiving compartments vary considerably. This demonstrates the need for a consistent concept that integrates knowledge of emission sources, leaching processes, transport pathways, and effects on targets. Such a consistent concept can serve as the basis for environmental risk assessment for several scenarios using experimentally determined emissions. Typically, a source–path–target concept integrates data from standardized leaching tests and models to describe leaching processes, the distribution of substances in the environment and the occurrence of substances at different points of compliance. This article presents an integrated concept for assessing the environmental impact of construction products on aquatic systems and unravels currently existing gaps and necessary actions. This manuscript outlines a source–path–target concept applicable to a large variety of construction products. It is intended to highlight key elements of a holistic evaluation concept that could assist authorities in developing procedures for environmental risk assessments and mitigation measures and identifying knowledge gaps. KW - Construction products KW - Environmental impact KW - Assessment KW - Concept PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542175 DO - https://doi.org/10.3390/w14020228 SN - 2073-4441 VL - 14 IS - 2 SP - 1 EP - 19 PB - MDPI CY - Basel AN - OPUS4-54217 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Villajos Collado, José Antonio T1 - Experimental volumetric hydrogen uptake determination at 77 K of commercially available metal-organic framework materials N2 - Storage is still limiting the implementation of hydrogen as an energy carrier to integrate the intermittent operation of renewable energy sources. Among different solutions to the currently used compressed or liquified hydrogen systems, physical adsorption at cryogenic temperature in porous materials is an attractive alternative due to its fast and reversible operation and the resulting reduction in storage pressure. The feasibility of cryoadsorption for hydrogen storage depends mainly on the performance of the used materials for the specific application, where metal-organic frameworks or MOFs are remarkable candidates. In this work, gravimetric and volumetric hydrogen uptakes at 77 K and up to 100 bar of commercially available MOFs were measured since these materials are made from relatively cheap and accessible building blocks. These materials also show relatively high porous properties and are currently near to large-scale production. The measuring device was calibrated at different room temperatures to calculate an average correction factor and standard deviation so that the correction deviation is included in the measurement error for better comparability with different measurements. The influence of measurement conditions was also studied, concluding that the available adsorbing area of material and the occupied volume of the sample are the most critical factors for a reproducible measurement, apart from the samples’ preparation before measurement. Finally, the actual volumetric storage density of the used powders was calculated by directly measuring their volume in the analysis cell, comparing that value with the maximum volumetric uptake considering the measured density of crystals. From this selection of commercial MOFs, the materials HKUST-1, PCN-250(Fe), MOF-177, and MOF-5 show true potential to fulfill a volumetric requirement of 40 g·L−1 on a material basis for hydrogen storage systems without further packing of the powders. KW - Hydrogen adsorption KW - Commercial metal-organic frameworks KW - Hydrogen uptake reproducibility KW - Volumetric uptake KW - Packing density PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542215 DO - https://doi.org/10.3390/c8010005 SN - 2311-5629 VL - 8 IS - 1 SP - 1 EP - 14 PB - MDPI CY - Basel AN - OPUS4-54221 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mehri, S. A1 - Kolmangadi, Mohamed Aejaz A1 - Dyre, J.C. A1 - Ingebrigtsen, T.S. T1 - Lines of invariant physics in the isotropic phase of the discotic Gay-Berne model N2 - The Gay-Berne model is studied numerically with a choice of parameters allowing for the formation of a discotic liquid crystal at low temperatures. We show that the model has strong virial potential-energy correlations in the isotropic phase at high temperatures, i.e., it obeys the criterion for the existence of isomorphs, which are curves of approximately invariant structure and dynamics. These properties are demonstrated to be approximately invariant in reduced units along the isomorph studied. The isomorph is described well by the constant density-scaling exponent 11.5, a number that is significantly larger than the density-scaling exponents of various Lennard-Jones models that are always below 6. KW - Liquid Crystal KW - Molecular Dynamics PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547611 DO - https://doi.org/10.1016/j.nocx.2022.100085 VL - 14 SP - 1 EP - 7 PB - Elsevier B.V. AN - OPUS4-54761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bugel, S. A1 - Hahnel, M. A1 - Kunde, T. A1 - de Sousa Amadeu, Nadar A1 - Sun, Y. A1 - Spieß, A. A1 - Beglau, T. H. Y. A1 - Janiak, C. A1 - Schmidt, B. M. T1 - Synthesis and Characterization of a Crystalline Imine-Based Covalent Organic Framework with Triazine Node and Biphenyl Linker and Its Fluorinated Derivate for CO2/CH4 Separation N2 - A catalyst-free Schiff base reaction was applied to synthesize two imine-linked covalent organic frameworks (COFs). The condensation reaction of 1,3,5-tris-(4-aminophenyl)triazine (TAPT) with 4,4′-biphenyldicarboxaldehyde led to the structure of HHU-COF-1 (HHU = Heinrich-Heine University). The fluorinated analog HHU-COF-2 was obtained with 2,2′,3,3′,5,5′,6,6′-octafluoro-4,4′-biphenyldicarboxaldehyde. Solid-state NMR, infrared spectroscopy, X-ray photoelectron spectroscopy, and elemental analysis confirmed the successful formation of the two network structures. The crystalline materials are characterized by high Brunauer–Emmett–Teller surface areas of 2352 m2/g for HHU-COF-1 and 1356 m2/g for HHU-COF-2. The products of a larger-scale synthesis were applied to prepare mixed-matrix membranes (MMMs) with the polymer Matrimid. CO2/CH4 permeation tests revealed a moderate increase in CO2 permeability at constant selectivity for HHU-COF-1 as a dispersed phase, whereas application of the fluorinated COF led to a CO2/CH4 selectivity increase from 42 for the pure Matrimid membrane to 51 for 8 wt% of HHU-COF-2 and a permeability increase from 6.8 to 13.0 Barrer for the 24 wt% MMM. KW - MOF KW - Filter PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547632 DO - https://doi.org/10.3390/ma15082807 SN - 1996-1944 VL - 15 IS - 8 SP - 1 EP - 18 PB - MDPI AN - OPUS4-54763 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zänker, Steffen A1 - Scholz, G. A1 - Marquardt, Julien A1 - Emmerling, Franziska T1 - Structural changes in Ba-compounds of different hardness induced by high-energy ball milling – evidenced by 137Ba NMR and X-ray powder diffraction N2 - Changes in the global bulk and local structures, of three different barium compounds (BaZrO3, BaF2, and BaFCl),were induced by mechanical milling and followed using X-ray powder diffraction (PXRD), subsequent microstructure analysis, and 137Ba solid state NMR spectroscopy. Harder materials like BaZrO3 experience significantly higher structural changes upon milling than softer materials like BaF2. Moreover, soft materials with layered structures, like BaFCl, show a pronounced structural change during the milling process. By combining PXRD and solid state NMR, detailed information on the changes to the global and local structures were obtained, which are of interest for mechanochemical synthesis, mechanically treated catalysts or ionic conductors. KW - Mechanochemistry KW - X-ray diffraction KW - Solid state NMR PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547397 DO - https://doi.org/10.1002/zaac.202200026 SN - 0044-2313 VL - 648 IS - 10 SP - 1 EP - 8 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Artzt, K. A1 - Haubrich, J. A1 - Sevostianov, I. A1 - Requena, G. A1 - Bruno, Giovanni T1 - Micromechanical behavior of annealed Ti-6Al-4V produced by Laser Powder Bed Fusion N2 - The micromechanical behavior of an annealed Ti-6Al-4V material produced by Laser Powder Bed Fusion was characterized by means of in-situ synchrotron X-ray diffraction during a tensile test. The lattice strain evolution was obtained parallel and transversal to the loading direction. The elastic constants were determined and compared with the conventionally manufactured alloy. In the plastic regime, a lower plastic anisotropy exhibited by the lattice planes was observed along the load axis (parallel to the building direction) than in the transverse direction. Also, the load transfer from α to β phase was observed, increasing global ductility of the material. The material seems to accumulate a significant amount of intergranular strain in the transverse direction. KW - Additive manufacturing KW - Ti-6Al-4V KW - Anisotropy KW - Intergranular strain KW - Synchrotron X-ray diffraction PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547406 DO - https://doi.org/10.1080/26889277.2022.2063763 VL - 2 IS - 1 SP - 186 EP - 201 PB - Taylor & Francis AN - OPUS4-54740 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Stegemann, R. A1 - Lyamkin, V. A1 - Cabeza, S. A1 - Evsevleev, S. A1 - Pelkner, Matthias A1 - Bruno, Giovanni T1 - Subsurface and Bulk Residual Stress Analysis of S235JRC + C Steel TIG Weld by Diffraction and Magnetic Stray Field Measurements N2 - Background Due to physical coupling between mechanical stress and magnetization in ferromagnetic materials, it is assumed in the literature that the distribution of the magnetic stray field corresponds to the internal (residual) stress of the specimen. The correlation is, however, not trivial, since the magnetic stray field is also influenced by the microstructure and the geometry of component. The understanding of the correlation between residual stress and magnetic stray field could help to evaluate the integrity of welded components. Objective This study aims at understanding the possible correlation of subsurface and bulk residual stress with magnetic stray field in a low carbon steel weld. Methods The residual stress was determined by synchrotron X-ray diffraction (SXRD, subsurface region) and by neutron diffraction (ND, bulk region). SXRD possesses a higher spatial resolution than ND. Magnetic stray fields were mapped by utilizing high-spatial-resolution giant magneto resistance (GMR) sensors. Results The subsurface residual stress overall correlates better with the magnetic stray field distribution than the bulk stress. This correlation is especially visible in the regions outside the heat affected zone, where the influence of the microstructural features is less pronounced but steep residual stress gradients are present. Conclusions It was demonstrated that the localized stray field sources without any obvious microstructural variations are associated with steep stress gradients. The good correlation between subsurface residual stress and magnetic signal indicates that the source of the magnetic stray fields is to be found in the range of the penetration depth of the SXRD measurements. KW - Residual stress KW - Magnetic stray field KW - Synchrotron X-ray diffraction KW - Neutron diffraction KW - TIG welding PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547419 DO - https://doi.org/10.1007/s11340-022-00841-x VL - 62 IS - 6 SP - 1017 EP - 1025 PB - Springer AN - OPUS4-54741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lu, Xin A1 - Chruscicki, Sebastian A1 - Schukar, Marcus A1 - Münzenberger, Sven A1 - Krebber, Katerina T1 - Application of Intensity-Based Coherent Optical Time Domain Reflectometry to Bridge Monitoring N2 - Although distributed fiber sensing techniques have been widely used in structural health monitoring, the measurement results of bridge monitoring, particularly under destructive testing, have rarely been reported. To the best of our knowledge, this paper is the first report of distributed vibration measurement results, which we obtained during a three-day destructive test on an abolished bridge. A coherent optical time domain reflectometry (COTDR) was used to acquire the vibration information while the bridge was being sawed. The obtained signal was analyzed in time and frequency domain. Some characteristics of the sawing-induced vibration were retrieved by the short-time Fourier transform; the vibration exhibited several high frequency components within the measured range up to 20 kHz and all the components appeared in the same time slot. Some unexpected signals were also detected. Thorough analysis showed that they are quite different from the sawing-induced vibration and are believed to originate from internal damage to the bridge (probably the occurrence of cracks). KW - Destructive testing KW - Structural health monitoring KW - Distributed fiber sensing KW - Distributed acoustic sensing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547451 DO - https://doi.org/10.3390/s22093434 VL - 22 IS - 9 SP - 3434 PB - MDPI AN - OPUS4-54745 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schneider, Beate A1 - Pfeiffer, F. A1 - Dyall-Smith, M. A1 - Kunte, Hans-Jörg T1 - Genome Sequence of Micromonospora aurantiaca Strain G9, a Member of a Bacterial Consortium Capable of Polyethylene Degradation N2 - Nine different bacterial isolates were recovered from landfills. Each isolate was obtained in pure culture. As a consortium, the bacteria degrade polyethylene. The complete genome sequence of strain G9 was determined by PacBio sequencing. Using the TYGS server for taxonomic classification, strain G9 was assigned to the species Micromonospora aurantiaca. KW - Polyethylene KW - Micromonospora aurantiaca KW - Degradation KW - iChip PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547181 DO - https://doi.org/10.1128/mra.01148-21 SN - 2576-098X VL - 11 IS - 5 SP - 1 EP - 2 PB - American Society for Microbiology CY - Washington, DC AN - OPUS4-54718 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hübler, Daniela A1 - Gradt, Thomas T1 - Effect of different binders and secondary carbides on NbC cermets T1 - Einfluss unterschiedlicher Binder und Sekundärkarbide auf NbC-Hartmetalle N2 - Due to the rapidly increasing price of tungsten carbide and the significant health risks associated with the wear products of WC-Co (Co3O4 and Wo3), an alternative is required. Niobium carbide (NbC) is well suited as a cutting tool due to its high melting point and low solubility in iron. So far, NbC-Ni cermets best met the requirements of high hardness and toughness. Various secondary carbides such as VC, Mo2C, TiC, but also WC were added to further improve the hardness. N2 - Aufgrund des rasanten Preisanstiegs von Wolframcarbid und signifikanter Gesundheitsrisiken, die mit den Verschleißprodukten von WC-Co-Hartmetallen (Co3O4 and Wo3) einhergehen, wird eine Alternative benötigt. Niobcarbid (NbC) ist als Zerspanwerkzeug aufgrund seiner hohen Schmelztemperatur und seiner geringen Löslichkeit in Eisen gut geeignet. Im Vergleich zu reinem NbC, führte eine vollständige Substitution von WC zu NbC-Co zu einem Anstieg der Zähigkeit und Festigkeit. Als alternative Binder wurden anschließend Nickel- und Eisengebundene Binder untersucht. Obwohl eisengebundene Hartmetalle im Vergleich zu NbC-Ni Hartmetallen eine ökonomische und kostengünstigere Alternative darstellen würden, zeigten sie einen höheren Reibkoeffizienten und eine höhere Verschleißrate. Bisher erfüllen die NbC-Ni-Hartmetalle die Anforderungen hinsichtlich einer hohen Härte und Zähigkeit am besten. Verschiedene Sekundärkarbide, wie VC, Mo2C, TiC, aber auch WC wurden zusätzlich hinzugefügt, um die Härte weiter zu steigern. Elementanalysen der NbC-Ni-MeC Hartmetalle (Me = Metall) zeigten, dass der Binder eine kubisch-flächenzentrierter Mischkristall ist, während die NbC Phase ein Mischkristall des Typs (Nb, Me)C ist. KW - Niobium carbide (NbC) KW - Cutting tool KW - Binders PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547202 DO - https://doi.org/10.1007/s10010-022-00583-1 SN - 0015-7899 VL - 86 IS - 2 SP - 197 EP - 211 PB - Springer CY - Berlin AN - OPUS4-54720 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altenburg, T. A1 - Giese, S. A1 - Wang, S. A1 - Muth, Thilo A1 - Renard, B.Y. T1 - Ad hoc learning of peptide fragmentation from mass spectra enables an interpretable detection of phosphorylated and cross-linked peptides N2 - Mass spectrometry-based proteomics provides a holistic snapshot of the entire protein set of living cells on a molecular level. Currently, only a few deep learning approaches exist that involve peptide fragmentation spectra, which represent partial sequence information of proteins. Commonly, these approaches lack the ability to characterize less studied or even unknown patterns in spectra because of their use of explicit domain knowledge. Here, to elevate unrestricted learning from spectra, we introduce ‘ad hoc learning of fragmentation’ (AHLF), a deep learning model that is end-to-end trained on 19.2 million spectra from several phosphoproteomic datasets. AHLF is interpretable, and we show that peak-level feature importance values and pairwise interactions between peaks are in line with corresponding peptide fragments. We demonstrate our approach by detecting post-translational modifications, specifically protein phosphorylation based on only the fragmentation spectrum without a database search. AHLF increases the area under the receiver operating characteristic curve (AUC) by an average of 9.4% on recent phosphoproteomic data compared with the current state of the art on this task. Furthermore, use of AHLF in rescoring search results increases the number of phosphopeptide identifications by a margin of up to 15.1% at a constant false discovery rate. To show the broad applicability of AHLF, we use transfer learning to also detect cross-linked peptides, as used in protein structure analysis, with an AUC of up to 94%. KW - Mass spectrometry KW - Machine learning KW - Deep learning KW - Peptide identification PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547580 DO - https://doi.org/10.1038/s42256-022-00467-7 SN - 2522-5839 VL - 4 SP - 378 EP - 388 PB - Springer Nature CY - London AN - OPUS4-54758 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Langenhan, Jennifer A1 - Jaeger, Carsten A1 - Baum, K. A1 - Simon, M. A1 - Lisec, Jan T1 - A Flexible Tool to Correct Superimposed Mass Isotopologue Distributions in GC‐APCI‐MS Flux Experiments N2 - The investigation of metabolic fluxes and metabolite distributions within cells by means of tracer molecules is a valuable tool to unravel the complexity of biological systems. Technological advances in mass spectrometry (MS) technology such as atmospheric pressure chemical ionization (APCI) coupled with high resolution (HR), not only allows for highly sensitive analyses but also broadens the usefulness of tracer‐based experiments, as interesting signals can be annotated de novo when not yet present in a compound library. However, several effects in the APCI ion source, i.e., fragmentation and rearrangement, lead to superimposed mass isotopologue distributions (MID) within the mass spectra, which need to be corrected during data evaluation as they will impair enrichment calculation otherwise. Here, we present and evaluate a novel software tool to automatically perform such corrections. We discuss the different effects, explain the implemented algorithm, and show its application on several experimental datasets. This adjustable tool is available as an R package from CRAN. KW - Mass Spectrometry KW - Isotopologue Distribution KW - Metabolic Flux KW - R package PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547318 DO - https://doi.org/10.3390/metabo12050408 VL - 12 IS - 5 SP - 1 EP - 10 PB - MDPI AN - OPUS4-54731 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Veico, V. P. A1 - Karlagina, Yu. Yu. A1 - Samokhvalov, A. A. A1 - Polyakov, D. S. A1 - Manokhin, S. S. A1 - Radaev, M. M. A1 - Odintsova, G. V. A1 - Gornushkin, Igor B. T1 - Surface Structuring and Reverse Deposition of Nanoporous Titanium Oxides by Laser Ablation of Titanium in Air N2 - The deposition of titanium oxides during titanium laser ablation in air has been experimentally and numerically investigated. A titanium sample was irradiated by nanosecond pulses from an Yb-fber laser with a beam scanned across the sample surface for its texturing. As a result, the hierarchical structure was observed consisting of a microrelief formed by the laser ablation and a nanoporous coating formed by the reverse deposition from the laser induced plasma plume. The chemical and phase composition of the nanoporous coating, as well as the morphology and structure of the surface, were studied using scanning electron microscopy, atomic force microscopy, and X-ray microanalysis. It was found that the deposit consists mostly of porous TiO2 with 26% porosity and inclusions of TiO, Ti2O3, and Ti2O3N. Optical emission spectroscopy was used to control the plasma composition and estimate the effective temperature of plasma plume. The chemical-hydrodynamic model of laser induced plasma was developed to get a deeper insight into the deposition process. The model predicts that condensed titanium oxides, formed in peripheral plasma zones, gradually accumulate on the surface during the plasma plume evolution. A satisfactory agreement between the experimental and calculated chemical composition of the plasma plume as well as between the experimental and calculated composition and thickness of the deposited film was demonstrated. This allows a cautious conclusion that the formation of condensed oxides in the plasma and their consequent deposition onto the ablation surface are among the key mechanisms of formation of porous surface films. KW - Laser ablation KW - Laser induced plasma deposition KW - Surface coating KW - Titanium dioxide KW - Hydrodynamic model KW - Plasma chemistry KW - Emission spectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548555 DO - https://doi.org/10.1007/s11090-022-10256-0 VL - 42 IS - 4 SP - 923 EP - 937 PB - Springer AN - OPUS4-54855 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hirschberg, L. A1 - Bake, Friedrich A1 - Knobloch, K. A1 - Hulshoff, S. A1 - Hirschberg, A. T1 - Experimental investigations of indirect noise due to modulation of axial vorticity and entropy upstream of a choked nozzle N2 - An experimental cold-gas study of the response of a choked convergent–divergent nozzle to swirl perturbations is presented. The perturbations were obtained by means of upstream unsteady tangential injections into initially steady flows with different values of steady background swirl. The swirl perturbations induced changes in the axial mass-flow rate, due to either their ingestion or evacuation by the nozzle. This in turn caused a downstream acoustic response. For low-intensity background swirl the responses were found to be similar to those obtained without steady background swirl. Perturbations of a high-intensity background swirl led to different effects. For long injection times, the negative mass-flow rate modulation occurred in two stages. The first stage was similar to that of the background-swirl free case. The second stage occurred after a short time delay, and induced a much stronger negative acoustic response. This unexpected behavior suggests that a significant part of the tangentially injected fluid flows upstream inducing an accumulation of swirl, which is – after tangential injection is ceased – suddenly cleared out through the nozzle. A scaling rule for the amplitudes of these acoustic responses is reported. Furthermore, quasi-steady models, based on steady-state measurements are proposed. These models predict the downstream acoustic response amplitude within a factor two. Additionally, preliminary empirical evidence of the effect of swirl on the downstream acoustic response due to the interaction of entropy patches with a choked nozzle is reported. This was obtained by comparison of sound produced by abrupt radial or tangential sonic injection, upstream from the choked nozzle, of air from a reservoir at room temperature to that from a reservoir with a higher stagnation temperature. Because the mass flow through the nozzle does not increase instantaneously, the injected higher-enthalpy air accumulates upstream of the injection-port position in the main flow. This eventually induces a large downstream acoustic pulse when tangential injection is interrupted. The magnitude of the resulting sound pulse can reach that of a quasi-steady response of the nozzle to a large air patch with a uniform stagnation temperature equal to that of the upstream-injected heated air. This hypothesis is consistent with the fact that the initial indirect-sound pulse is identical to one obtained with unheated air injection. The authors posit that – given all of the insight gleaned from them in this case – acoustic measurements of indirect sound appear to be a potentially useful diagnostic tool. KW - Aeroacoustics KW - Indirect combustion noise KW - Vorticity noise KW - Entropy noise KW - Swirl PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548331 DO - https://doi.org/10.1016/j.jsv.2022.116989 SN - 0022-460X VL - 532 SP - 1 EP - 22 PB - Elsevier Ltd. AN - OPUS4-54833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaeger, Carsten A1 - Lisec, Jan T1 - Towards Unbiased Evaluation of Ionization Performance in LC-HRMS Metabolomics Method Development N2 - As metabolomics increasingly finds its way from basic science into applied and regulatory environments, analytical demands on nontargeted mass spectrometric detection methods continue to rise. In addition to improved chemical comprehensiveness, current developments aim at enhanced robustness and repeatability to allow long-term, inter-study, and meta-analyses. Comprehensive metabolomics relies on electrospray ionization (ESI) as the most versatile ionization technique, and recent liquid chromatography-high resolution mass spectrometry (LC-HRMS) instrumentation continues to overcome technical limitations that have hindered the adoption of ESI for applications in the past. Still, developing and standardizing nontargeted ESI methods and instrumental setups remains costly in terms of time and required chemicals, as large panels of metabolite standards are needed to reflect biochemical diversity. In this paper, we investigated in how far a nontargeted pilot experiment, consisting only of a few measurements of a test sample dilution series and comprehensive statistical analysis, can replace conventional targeted evaluation procedures. To examine this potential, two instrumental ESI ion source setups were compared, reflecting a common scenario in practical method development. Two types of feature evaluations were performed, (a) summary statistics solely involving feature intensity values, and (b) analyses additionally including chemical interpretation. Results were compared in detail to a targeted evaluation of a large metabolite standard panel. We reflect on the advantages and shortcomings of both strategies in the context of current harmonization initiatives in the metabolomics field. KW - Mass Spectrometry KW - Non-targeted analysis KW - Method development PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548065 DO - https://doi.org/10.3390/metabo12050426 VL - 12 IS - 5 SP - 1 EP - 13 PB - MDPI AN - OPUS4-54806 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chambers, M. S. A1 - Hunter, R. D. A1 - Hollamby, M. J. A1 - Pauw, Brian Richard A1 - Smith, A. J. A1 - Snow, T. A1 - Danks, A. E. A1 - Schnepp, Z. T1 - In Situ and Ex Situ X‑ray Diffraction and Small-Angle X‑ray Scattering Investigations of the Sol−Gel Synthesis of Fe3N and Fe3C N2 - Iron nitride (Fe3N) and iron carbide (Fe3C) nanoparticles can be prepared via sol−gel synthesis. While sol−gel methods are simple, it can be difficult to control the crystalline composition, i.e., to achieve a Rietveld-pure product. In a previous in situ synchrotron study of the sol−gel synthesis of Fe3N/Fe3C, we showed that the reaction proceeds as follows: Fe3O4 → FeOx → Fe3N → Fe3C. There was considerable overlap between the different phases, but we were unable to ascertain whether this was due to the experimental setup (side-on heating of a quartz capillary which could lead to thermal gradients) or whether individual particle reactions proceed at different rates. In this paper, we use in situ wide- and small-angle X-ray scattering (wide-angle X-ray scattering (WAXS) and small-angle X-ray scattering (SAXS)) to demonstrate that the overlapping phases are indeed due to variable reaction rates. While the initial oxide nanoparticles have a small range of diameters, the size range expands considerably and very rapidly during the oxide−nitride transition. This has implications for the isolation of Rietveld-pure Fe3N, and in an extensive laboratory study, we were indeed unable to isolate phasepure Fe3N. However, we made the surprising discovery that Rietveld-pure Fe3C nanoparticles can be produced at 500 °C with a sufficient furnace dwell time. This is considerably lower than the previous reports of the sol−gel synthesis of Fe3C nanoparticles. KW - Small-angle X-ray Scattering KW - SAXS KW - Diffraction KW - XRD KW - Scattering KW - Sol-gel KW - Iron nitride KW - Nanoparticles KW - Iron carbide KW - Catalyst KW - In-situ KW - Ex-situ KW - Synthesis KW - Synchrotron PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548226 DO - https://doi.org/10.1021/acs.inorgchem.1c03442 VL - 61 IS - 18 SP - 6742 EP - 6749 PB - ACS Publications CY - Washington AN - OPUS4-54822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mazzeo, P. P. A1 - Prencipe, M. A1 - Feiler, Torvid A1 - Emmerling, Franziska A1 - Bacchi, A. T1 - On the mechanism of cocrystal mechanochemical reaction via low melting eutectic: A time-resolved in situ monitoring investigation N2 - Mechanochemistry has become a sustainable and attractive cost-effective synthetic technique, largely used within the frame of crystal engineering. Cocrystals, namely, crystalline compounds made of different chemical entities within the same crystal structure, are typically synthesized in bulk via mechanochemistry; however, whereas the macroscopic aspects of grinding are becoming clear, the fundamental principles that underlie mechanochemical cocrystallization at the microscopic level remain poorly understood. Time-resolved in situ (TRIS) monitoring approaches have opened the door to exceptional detail regarding mechanochemical reactions. We here report a clear example of cocrystallization between two solid coformers that proceeds through the formation of a metastable low melting binary eutectic phase. The overall cocrystallization process has been monitored by time-resolved in situ (TRIS) synchrotron X-ray powder diffraction with a customized ball milling setup, currently available at μ Spot beamline at BESSY-II, Helmholtz-Zentrum Berlin. The binary system and the low melting eutectic phase were further characterized via DSC, HSM, and VT-XRPD. KW - Mechanochemistry KW - In situ KW - Cocrystal PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552977 DO - https://doi.org/10.1021/acs.cgd.2c00262 SN - 1528-7505 VL - 22 IS - 7 SP - 4260 EP - 4267 PB - ACS Publ. CY - Washington, DC AN - OPUS4-55297 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlick-Hasper, Eva A1 - Bethke, John A1 - Vogler, Nico A1 - Goedecke, Thomas T1 - Flow properties of powdery or granular filling substances of dangerous goods packagings - Comparison of the measurement of the angle of repose and the determination of the Hausner ratio N2 - To ensure safety when transporting dangerous goods, it is important to specify the flow properties of the respective solid filling substance of the packagings. For this purpose, the angle of repose is currently used for the UN approvals in Germany. Measurements were carried out on 12 powdery or granular substances applying the angle of repose measuring methods customary in the test centres. The results of the methods differ significantly from each other. In addition, some of the techniques cannot be applied for very cohesive or coarse-grained materials. The results for the angle of repose show a strong scatter for some constellations (coefficient of variation more than 20 %). Safety during transport of dangerous goods cannot be guaranteed with this currently practiced system of measuring the angle of repose. As a consequence, an alternative parameter to characterize the flow properties of bulk materials should be used in the recognized test centers for dangerous goods packagings, such as the Hausner ratio. This approach leads to more precise test results for the substances examined (maximum coefficient of variation 2.8 %). It also has advantages in terms of applicability and occupational safety. Since the flow properties are safety-relevant, both in terms of mechanical safety and safety against the release of dangerous substances, the testing practice in the recognized test labs should be improved and standardized. KW - Sift-proofness KW - Powders KW - Flowability KW - Flow properties KW - Angle of repose KW - Hausner ratio PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552990 DO - https://doi.org/10.1002/pts.2678 SP - 1 EP - 18 PB - Wiley online library AN - OPUS4-55299 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jiang, Shan A1 - Wang, T. A1 - Behren, S. A1 - Westerlind, U. A1 - Gawlitza, Kornelia A1 - Persson, J. L. A1 - Rurack, Knut T1 - Sialyl-Tn Antigen-Imprinted Dual Fluorescent Core–Shell Nanoparticles for Ratiometric Sialyl-Tn Antigen Detection and Dual-Color Labeling of Cancer Cells N2 - Sialyl-Tn (STn or sialyl-Thomsen-nouveau) is a carbohydrate antigen expressed by more than 80% of human carcinomas. We here report a strategy for ratiometric STn detection and dual-color cancer cell labeling, particularly, by molecularly imprinted polymers (MIPs). Imprinting was based on spectroscopic studies of a urea-containing green-fluorescent monomer 1 and STn-Thr-Na (sodium salt of Neu5Acα2-6GalNAcα-O-Thr). A few-nanometer-thin green-fluorescent polymer shell, in which STn-Thr-Na was imprinted with 1, other comonomers, and a cross-linker, was synthesized from the surface of red-emissive carbon nanodot (R-CND)-doped silica nanoparticles, resulting in dual fluorescent STn-MIPs. Dual-color labeling of cancer cells was achieved since both red and green emissions were detected in two separate channels of the microscope and an improved accuracy was obtained in comparison with single-signal MIPs. The flow cytometric cell analysis showed that the binding of STn-MIPs was significantly higher (p < 0.001) than that of non-imprinted polymer (NIP) control particles within the same cell line, allowing to distinguish populations. Based on the modularity of the luminescent core–fluorescent MIP shell architecture, the concept can be transferred in a straightforward manner to other target analytes. KW - Cancer KW - Core−shell particles KW - Dual-color labeling glycan KW - Molecular imprinting PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563106 DO - https://doi.org/10.1021/acsanm.2c03252 SP - 1 EP - 14 PB - ACS Publications AN - OPUS4-56310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Landis, E. A1 - Hassefras, Emiel A1 - Oesch, Tyler A1 - Niederleithinger, Ernst T1 - A Microstructural Basis for Diffuse Ultrasound in Concrete N2 - Attenuation of ultrasonic signals in concrete has the potential to carry much information about the microstructure of the material. In this work a series of concrete specimens of varying porosities and pore size distributions were internally imaged with x-ray computed tomography (CT), and then subsequently examined with throughtransmission ultrasound. The CT images were used to quantify both capillary porosity of cement paste as well as internal interfaces that are likely to produce elastic wave scattering. Ultrasound signals were represented as a diffusion process such that absorption and scattering attenuation could be isolated. As implemented, the diffusion model was a poor predictor of capillary porosity, while diffusivity was a reasonable predictor of scattering interfaces. Diffusivity was found to scale extremely well with small scale porosity, which made it a good predictor of compressive strength. T2 - NDT-CE 2022 CY - Zurich, Switzerland DA - 16.08.2022 KW - Concrete KW - X-ray tomography KW - Ultrasound PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563371 UR - https://www.ndt.net/article/ndtce2022/paper/61592_manuscript.pdf SP - 1 EP - 4 PB - NDT.net AN - OPUS4-56337 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Üstündag, Ömer A1 - Bakir, Nasim A1 - Gumenyuk, Andrey A1 - Rethmeier, Michael T1 - Improvement of Charpy impact toughness by using an AC magnet backing system for laser hybrid welding of thick S690QL steels N2 - The study deals with the influence of the heat input and the resulting cooling times on the microstructure and Charpy impact toughness of single-pass laser hybrid welded 20-mm thick high-strength steel S690QL. The main focus is on the change of the mechanical properties over the entire seam thickness. The cooling times were measured in-situ using a pyrometer and an optical fibre in three different depths of the seam where Charpy impact test specimens were also later taken. Thereby, three different heat inputs from 1.3 kJ/mm to 2 kJ/mm were investigated. Despite the observed decreased values of both t8/5-cooling time and the Charpy impact toughness in the root part of the seam, the required impact toughness of 38 J/cm2 could be reached in dependance on applied heat input, especially at the heat input of 1.6 kJ/mm. T2 - 12th CIRP conference on photonic technologies [lane 2022] CY - Fürth, Germany DA - 04.09.2022 KW - Thick-plate welding KW - Laser hybrid welding KW - Electromagnetic backing KW - Charpy impact toughness KW - Thermal cycles PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563731 DO - https://doi.org/10.1016/j.procir.2022.08.067 VL - 111 SP - 462 EP - 465 PB - Elsevier B.V. AN - OPUS4-56373 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steinhäuser, Lorin A1 - Piechotta, Christian A1 - Westphalen, Tanja A1 - Kaminski, Katja T1 - Evaluation, comparison and combination of molecularly imprinted polymer solid phase extraction and classical solid phase extraction for the preconcentration of endocrine disrupting chemicals from representative whole water samples N2 - Estrogens are endocrine disrupting chemicals and of high concerns due to demonstrated harmful effects on the environment and low effect levels. For monitoring and risk assessment, several estrogens were included in the "watch list" of the EU Water Framework Directive which sets very low environmental quality standard (EQS) levels for Estrone (E1) and 17β-Estradiol (E2) of 0.4 ng L−1 and for 17α-Ethinylestradiol (EE2) of 0.035 ng L−1 requiring sensitive detection methods, as well as extensive sample preparation. A sensitive, derivatization-free, isotope dilution calibration HPLC-MS/MS method for a panel of 5 selected estrogens (including the 3 estrogens of the EU WFD watchlist), and a procedure for the reproducible preparation of a representative whole water matrix including mineral water, humic acids and solid particulate matter are presented. These are used in a diligent comparison of classical solid phase extraction (SPE) on hydrophilic-lipophilic balanced (HLB) phase to SPE on an estrogen-specific molecularly imprinted polymer phase (MISPE) for ultra-trace levels of the analytes (1–10 ng L−1). Additionally, a two-step procedure combining HLB SPE disks followed by MISPE is evaluated. The tow-step procedure provides superior enrichment, matrix removal and sample throughput while maintaining comparable recovery rates to simple cartridge SPE. Estimated method quantification limits (MQLs) range from 0.109–0.184 ng L−1 and thus meet EQS-levels for E1 and E2, but not EE2. The representative whole water matrix provides a reproducible comparison of sample preparation methods and lays the foundation for a certified reference material for estrogen analysis. The presented method will serve as the basis for an extended validation study to assess its use for estrogen monitoring in the environment. KW - Estrogens KW - Whole water samples KW - Molecular imprinted polymers KW - EU-WFD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563547 DO - https://doi.org/10.1016/j.talo.2022.100163 SN - 2666-8319 VL - 6 SP - 1 EP - 5 PB - Elsevier B.V. CY - Amsterdam, Niederlande AN - OPUS4-56354 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bakir, Nasim A1 - Üstündag, Ömer A1 - Gumenyuk, Andrey A1 - Rethmeier, Michael T1 - Influence of the weld pool geometry on solidification cracking in partial penetration high power laser beam welding N2 - Solidification cracking is still a serious problem in laser beam welding, especially in the welding of thick-walled plates. The influence of weld pool geometry on solidification cracking in partial penetration welding of thick plates is investigated within scope of this study. Therefore, a specific experimental setup of steel and quartz glass in butt configuration and on the side with high-speed camera were used to record the weld pool shape. In addition, the influence of laser inclination angle on the weld pool geometry and on solidification crack formation was investigated. The results show a bulge in the weld pool root, which is separated from an upper region by a necking region. This leads to a case where there are three different longitudinal region lengths with different solidification zones. This temporal sequence of solidification strongly promotes the formation of solidification cracks in the weld root. T2 - 12th CIRP Conference on photonic technologies (LANE 2022) CY - Fürth, Germany DA - 04.09.2022 KW - Laser beam welding KW - Partial penetration KW - Weld pool shape PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563940 DO - https://doi.org/10.1016/j.procir.2022.08.174 VL - 111 SP - 397 EP - 400 PB - Elsevier B.V. AN - OPUS4-56394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abraham, O. A1 - Niederleithinger, Ernst A1 - Schmidt, F. A1 - Sörensen, J.D. A1 - Thöns, S. A1 - Chapeleau, X. A1 - Ferria, H. T1 - Infrastar Training School on Fatigue and Reliability Analysis of Structures - Training for Assessment of Risk N2 - The Infrastar training school provides lectures and hands-on training to Master and PhD students, early-stage researchers and (young) professionals on all aspects of asset management of civil infrastructures with respect to fatigue of materials. It is organized yearly since 2019 and up to 20 profiles are selected to attend the 3.5-day training. A team of 7 teachers provides insight in multi-disciplinary and intersectoral basic concepts in three core fields, ranging from the design to the dismantling of the structures (bridges and wind turbines): 1. Monitoring and auscultation, 2. Structural and action models, 3. Reliability, risk and decision analyses. Each year, a recognized expert is invited to deliver a keynote lecture to raise interest in a specific aspect of one of the fields covered. The presentation is recorded and published on the training school website. T2 - NDT-CE 2022 CY - Zurich, Switzerland DA - 16.08.2022 KW - Doctoral School KW - Multidisciplinary KW - Fatigue KW - Reliability PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563253 UR - https://www.ndt.net/article/ndtce2022/paper/61021_manuscript.pdf SP - 1 EP - 3 PB - NDT.net AN - OPUS4-56325 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabe, U. A1 - Pudovikov, S. A1 - Herrmann, H.-G. A1 - Wiggenhauser, H. A1 - Prabhakara, Prathik A1 - Niederleithinger, Ernst T1 - Evaluation of retroreflective corner echo for detection of surface breaking cracks in concrete by ultrasound N2 - The retroreflective corner echo is used, for example, in ultrasonic non-destructive testing of metals to find fatigue cracks in tubes or shafts. If the much weaker crack tip signal is additionally detected, the crack length can also be determined. A corner reflection occurs in cases of surface breaking cracks with predominantly perpendicular orientation to the surface. The intensity of the corner reflection depends on the angle of incidence and on the ultrasonic wave mode used. For the reliable detection of vertical surface breaking cracks in metals, transversal waves are commonly used, which propagate at an angle of 37° to 53° to the inspection surface. As shown in this contribution, the wide spread low frequency ultrasonic arrays with dry point contact sources available for ultrasonic testing of concrete also allow to receive corner echoes. These devices generate transversal waves in concrete structures with a large divergence of the sound field. A series of experiments was carried out with such dry point contact arrays on concrete specimens with artificial test defects and controlled induced cracks of different depths. The ultrasonic time-of-flight signals were recorded, exported and reconstructed utilising the SAFT (Synthetic Aperture Focusing Technique) algorithm. The SAFT reconstruction parameters were adjusted to visualize the corner echo indication. As will be shown, with this targeted processing, the reproducible detection of surface breaking cracks in concrete is possible. The retroreflective corner echo can thus be exploited in civil engineering for non-destructive inspection of concrete. T2 - NDT-CE 2022 CY - Zurich, Switzerland DA - 16.08.2022 KW - Concrete KW - Crack depth KW - Ultrasound KW - SAFT PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563365 UR - https://www.ndt.net/article/ndtce2022/paper/27256_manuscript.pdf IS - 27256 SP - 1 EP - 4 PB - NDT.net AN - OPUS4-56336 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Krüger, Jörg T1 - Structuring of thin films by ultrashort laser pulses N2 - Modern life and global communication would not be possible without technologically tailored thin films; they are omnipresent in daily life applications. In most cases, the films are deposited entirely at the carrying substrates in a specific processing step of the device or sample. In some cases, however, removal or modification must be performed locally, i.e., site-controlled and material selective through an additional laser processing step. For that ultrashort laser pulses with durations in the femtosecond and picosecond range can provide unique advantages and capabilities in industrially scalable schemes. This article reviews the current state of the research and corresponding industrial transfer related to the structuring of thin films by ultrashort pulsed lasers. It focuses on the pertinent historic developments, reveals the relevant physical and chemical effects, explores the ultimate limits, and discusses selected industrial and scientific applications. KW - Thin films KW - Laser processing KW - Ultrashort lasers KW - Laser damage KW - Femtosecond laser ablation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565732 DO - https://doi.org/10.1007/s00339-022-06229-x SN - 0947-8396 SN - 1432-0630 VL - 129 IS - 1 SP - 1 EP - 38 PB - Springer CY - Berlin AN - OPUS4-56573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jasiuniene, E. A1 - Yilmaz, Bengisu A1 - Smagulova, D. A1 - Bhat, G. A. A1 - Cicenas, V. A1 - Zukauskas, E. A1 - Mazeika, L. T1 - Non-Destructive Evaluation of the Quality of Adhesive Joints Using Ultrasound, X-ray, and Feature-Based Data Fusion N2 - The aim of this work is to achieve reliable nondestructive evaluation (NDE) of adhesively bonded aerospace components by developing novel multidimensional data fusion techniques, which would combine the information obtained by ultrasonic and X-ray NDE methods. Separately, both NDE techniques have their advantages and limitations. The integration of data obtained from pulse echo immersion ultrasound testing and radiography holds immense potential to help improve the reliability of non-destructive evaluation. In this study, distinctive features obtained from single techniques, traditional ultrasonic pulse echo testing, and radiography, as well as fused images, were investigated and the suitability of these distinctive features and fusion techniques for improving the probability of defect detection was evaluated. For this purpose, aluminum single lap joints with brass inclusions were analyzed using ultrasound pulse echo and radiography techniques. The distinctive features were extracted from the data obtained, and images of features obtained by both techniques were fused together. Different combinations of features and fusion algorithms were investigated, considering the desire to automate data evaluation in the future. KW - Data fusion KW - Ultrasonics KW - Radiography PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565789 DO - https://doi.org/10.3390/app122412930 VL - 12 IS - 24 SP - 1 EP - 20 PB - MDPI AN - OPUS4-56578 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen A1 - Meyer, A. T1 - About the Influence of (Non-)Solvents on the Ring Expansion Polymerization of l-Lactide and the Formation of Extended Ring Crystals N2 - Ring-expansion polymerizations (REPs) catalyzed by two cyclic tin catalysts(2-stanna-1.3-dioxa-4,5,6,7-dibenzazepine [SnBiph] and 2,2-dibutyl-2-stanna-1,3-dithiolane [DSTL) are performed at 140 °C in bulk. Small amounts (4 vol%) of chlorobenzene or other solvents are added to facilitate transesterification reactions (ring–ring equilibration) in the solid poly(l-lactide)s. In the mass range up to m/z 13 000 crystalline PLAs displaying a so-called saw-tooth pattern in the MALDI-TOF mass spectra are obtained indicating the formation of extended-ring crystals. The characteristics of extended-ring crystallites and folded-ring crystallites are discussed. Furthermore, extremely high melting temperatures (Tm’s up to 201.2 °C) and melting enthalpies (𝚫Hm’s up to 106 J g−1)) are found confirming that 𝚫Hmmax, the 𝚫Hm of a perfect crystal, is around or above 115 J g−1 in contrast to literature data. KW - Polylactide KW - MALDI-TOF MS KW - Ring-expansion polymerization KW - Crystals PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565038 DO - https://doi.org/10.1002/macp.202200385 SN - 1022-1352 SP - 1 EP - 8 PB - Wiley VHC-Verlag AN - OPUS4-56503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kohlbrecher, J. A1 - Breßler, Ingo T1 - Updates in SASfit for fitting analytical expressions and numerical models to small-angle scattering patterns N2 - Small-angle scattering is an increasingly common method for characterizing particle ensembles in a wide variety of sample types and for diverse areas of application. SASfit has been one of the most comprehensive and flexible curve-fitting programs for decades, with many specialized tools for various fields. Here, a selection of enhancements and additions to the SASfit program are presented that may be of great benefit to interested and advanced users alike: (a) further development of the technical basis of the program, such as new numerical algorithms currently in use, a continuous integration practice for automated building and packaging of the software, and upgrades on the plug-in system for easier adoption by third-party developers; (b) a selection of new form factors for anisotropic scattering patterns and updates to existing form factors to account for multiple scattering effects; (c) a new type of a very flexible distribution called metalog [Keelin (2016). Decis. Anal. 13, 243–277], and regularization techniques such as the expectation-maximization method [Dempster et al. (1977). J. R. Stat. Soc. Ser. B (Methodological), 39, 1–22; Richardson (1972) J. Opt. Soc. Am. 62, 55; Lucy (1974). Astron. J. 79, 745; Lucy (1994). Astron. Astrophys. 289, 983–994], which is compared with fits of analytical size distributions via the non-linear least-squares method; and (d) new structure factors, especially for ordered nano- and meso-scaled material systems, as well as the Ornstein–Zernike solver for numerical determination of particle interactions and the resulting structure factor when no analytical solution is available, with the aim of incorporating its effects into the small-angle scattering intensity model used for fitting with SASfit. KW - Small-angle scattering KW - Numerical models KW - Structure factors KW - Regularization KW - SAXS KW - SANS PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565069 DO - https://doi.org/10.1107/S1600576722009037 SN - 0021-8898 SN - 1600-5767 VL - 55 IS - 6 SP - 1677 EP - 1688 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-56506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Babutzka, Martin A1 - Lehmann, Jens A1 - Burkert, Andreas T1 - Field exposure study under sheltered and open exposure conditions at different test sites in Germany: First‐year corrosion rate and atmospheric corrosivity N2 - The corrosivity of atmospheres in Europe has changed significantly in recent decades. For the Federal Republic of Germany, no current values for the corrosion rate based on 1‐year atmospheric exposure of standard specimens can be found in the scientific literature after 2000. This paper presents results from a field exposure study in the Berlin metropolitan area and Helgoland in 2016. Based on standard specimens, values for the corrosion rate and the corresponding atmospheric corrosivity category are determined for open exposure and indirect weathering in a ventilated enclosure as sheltering after 1 year of exposure. The results prove that determined corrosivity categories are material‐specific. Sheltered exposure is a typical atmospheric situation for many building components. It allows statements on the effect of the concentration of airborne substances on the corrosivity beyond the normative requirements. KW - Atmospheric corrosion KW - Corrosivity category KW - ISO 9223 KW - Mass loss KW - Atmosphärische Korrosion PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565099 DO - https://doi.org/10.1002/maco.202213582 SN - 0947-5117 (print) SN - 1521-4176 (online) SP - 1 EP - 15 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-56509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roveda, Ilaria A1 - Serrano Munoz, Itziar A1 - Mishurova, Tatiana A1 - Madia, Mauro A1 - Pirling, T. A1 - Evans, Alexander A1 - Klaus, M. A1 - Haubrich, J. A1 - Requena, G. A1 - Bruno, Giovanni T1 - Influence of a 265 °C heat treatment on the residual stress state of a PBF-LB/M AlSi10Mg alloy N2 - Laser Powder Bed Fusion (PBF-LB/M) additive manufacturing (AM) induces high magnitude residual stress (RS) in structures due to the extremely heterogeneous cooling and heating rates. As the RS can be deleterious to the fatigue resistance of engineering components, great efforts are focused on understanding their generation and evolution after post-process heat treatments. In this study, one of the few of its kind, the RS relaxation induced in an as-built PBF-LB/M AlSi10Mg material by a low-temperature heat treatment (265 °C for 1 h) is studied by means of X-ray and neutron diffraction. Since the specimens are manufactured using a baseplate heated up to 200 °C, low RS are found in the as-built condition. After heat treatment a redistribution of the RS is observed, while their magnitude remains constant. It is proposed that the redistribution is induced by a repartition of stresses between the a-aluminium matrix and the silicon phase, as the morphology of the silicon phase is affected by the heat treatment. A considerable scatter is observed in the neutron diffraction RS profiles, which is principally correlated to the presence (or absence) of pockets of porosity developed at the borders of the chessboard pattern. KW - Neutron diffraction KW - Additive manufacturing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565115 DO - https://doi.org/10.1007/s10853-022-07997-w SN - 1573-4803 VL - 57 SP - 22082 EP - 22098 PB - Springer Science + Business Media CY - Dordrecht AN - OPUS4-56511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xing, N. A1 - Höfler, T. A1 - Hearn, C. J. A1 - Nascimento, M. A1 - Camps Paradell, G. A1 - McMahon, Dino Peter A1 - Kunec, D. A1 - Osterrieder, N. A1 - Cheng, H. H. A1 - Trimpert, J. ED - Trimpert, Jakob T1 - Fast-forwarding evolution—Accelerated adaptation in a proofreading-deficient hypermutator herpesvirus N2 - Evolution relies on the availability of genetic diversity for fitness-based selection. However, most deoxyribonucleic acid (DNA) viruses employ DNA polymerases (Pol) capable of exonucleolytic proofreading to limit mutation rates during DNA replication. The relative genetic stability produced by high-fidelity genome replication can make studying DNA virus adaptation and evolution an intensive endeavor, especially in slowly replicating viruses. Here, we present a proofreading-impaired Pol mutant (Y547S) of Marek’s disease virus that exhibits a hypermutator phenotype while maintaining unimpaired growth in vitro and wild-type (WT)-like pathogenicity in vivo. At the same time, mutation frequencies observed in Y547S virus populations are 2–5-fold higher compared to the parental WT virus. We find that Y547S adapts faster to growth in originally non-permissive cells, evades pressure conferred by antiviral inhibitors more efficiently, and is more easily attenuated by serial passage in cultured cells compared to WT. Our results suggest that hypermutator viruses can serve as a tool to accelerate evolutionary processes and help identify key genetic changes required for adaptation to novel host cells and resistance to antiviral therapy. Similarly, the rapid attenuation achieved through adaptation of hypermutators to growth in cell culture enables identification of genetic changes underlying attenuation and virulence, knowledge that could practically exploited, e.g. in the rational design of vaccines. KW - Polymerase mutant KW - Proofreading deficient KW - Hypermutation KW - Adaption KW - DNA polymerase KW - Marek's Disease Virus PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565631 DO - https://doi.org/10.1093/ve/veac099 SN - 2057-1577 VL - 8 IS - 2 SP - 1 EP - 11 PB - Oxford University Press CY - Oxford, UK AN - OPUS4-56563 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baensch, Franziska A1 - Baer, Wolfram A1 - Wossidlo, Peter A1 - Habib, Abdel Karim T1 - Damage evolution detection in a pipeline segment under bending by means of acoustic emission N2 - A steel pipeline segment of 2.5 m length was subjected to quasi-static four-point bending load in three steps for studying the initial cracking and damage accumulation based on the Acoustic Emission (AE) technique and by the direct current potential drop (DCPD) technique. For the latter, a new post-test analysis method was established. AE is found more sensitive to crack initiation than DCPD. Formation of mesoscopic and macroscopic cracks as well as their closure and the resulting friction generate weighted peak frequencies below 400 kHz, whereas microscopic cracking produces AE with broad band spectra identifiable by weighted peak frequencies above 400 kHz. Critical states alike the maximum load level and the leak opening were accompanied by peak amplitudes above 85 dBAE. This rather fundamental study provides a data base for possibly developing advanced strategies of detection and alarm systems based on acoustic monitoring of pipelines, or at least, steel structures. KW - Crack KW - Accoustic emission KW - Frequency domain KW - Potential drop technique KW - Fracture PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565171 DO - https://doi.org/10.1016/j.ijpvp.2022.104863 SN - 0308-0161 VL - 201 IS - 104863 SP - 1 EP - 9 PB - Elsevier Science CY - Amsterdam AN - OPUS4-56517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Linberg, Kevin A1 - Emmerling, Franziska A1 - Michalchuk, Adam T1 - Unintended Rate Enhancement in Mechanochemical Kinetics by Using Poly(methyl methacrylate) Jars N2 - Time-resolved in situ (TRIS) X-ray diffraction has changed how mechanochemical transformations are studied but requires the use of X-ray transparent jars often made from poly(methyl methacrylate) (PMMA). However, using PMMA jars can alter the apparent kinetics of mechanochemical polymorphism by an order of magnitude, questioning the interpretability of established TRIS methods. Our results suggest that rate enhancement in PMMA jars may not be dominated by chemical effects of the polymer, but rather a result of different equilibrium temperatures within the jar. These features must be better understood before control over mechanochemical reactions can be achieved. KW - Mechanochemistry KW - Organic compounds KW - Polymers KW - Materials PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565276 DO - https://doi.org/10.1021/acs.cgd.2c01227 SN - 1528-7483 SP - 1 EP - 5 PB - ACS Publications AN - OPUS4-56527 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ravi, J. A1 - Feiler, Torvid A1 - Mondal, A. A1 - Michalchuk, Adam A1 - Reddy, C. M. A1 - Bhattacharya, Biswajit A1 - Emmerling, Franziska A1 - Chandrasekar, R. T1 - Plastically bendable organic crystals for monolithic and hybrid micro-optical circuits N2 - Fluorescent plastically bendable crystals are a promising alternative to silicon-based materials for fabricating photonic integrated circuits, owing to their optical attributes and mechanical compliance. Mechanically bendable plastic organic crystals are rare. Their formation requires anisotropic intermolecular interactions and slip planes in the crystal lattice. This work presents three fluorescent plastically bendable crystalline materials namely, 2-((E)-(6-methylpyridin-2-ylimino)methyl)-4-chlorophenol (SB1), 2-((E)-(6-methylpyridin-2-ylimino)methyl)-4-bromophenol (SB2), and 2-((E)-(6-Bromopyridin-2-ylimino)methyl)-4-bromophenol (SB3) molecules. The crystal plasticity in response to mechanical stress facilitates the fabrication of various monolithic and hybrid (with a tip-to-tip coupling) photonic circuits using mechanical micromanipulation with an atomic force microscope cantilever tip. These plastically bendable crystals act as active (self-guiding of fluorescence) and passive waveguides both in straight and extremely bent (U-, J-, and O-shaped) geometries. These microcircuits use active and passive waveguiding principles and reabsorbance and energy-transfer mechanisms for their operation, allowing input-selective and direction-specific signal transduction. KW - Flexible crystals KW - Flexible waveguide PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565302 DO - https://doi.org/10.1002/adom.202201518 SN - 2195-1071 SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56530 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bulling, Jannis A1 - Jurgelucks, B. A1 - Prager, Jens A1 - Walther, A. T1 - Defect reconstruction in a two-dimensional semi-analytical waveguide model via derivative-based optimization N2 - This paper considers an indirect measurement approach to reconstruct a defect in a two-dimensional waveguide model for a non-destructive ultrasonic inspection via derivative-based optimization. The propagation of the mechanical waves is simulated by the scaled boundary finite element method that builds on a semi-analytical approach. The simulated data are then fitted to given data associated with the reflected waves from a defect which is to be reconstructed. For this purpose, we apply an iteratively regularized Gauss-Newton method in combination with algorithmic differentiation to provide the required derivative information accurately and efficiently. We present numerical results for three kinds of defects, namely, a crack, delamination, and corrosion. The objective function and the properties of the reconstruction method are investigated. The examples show that the parameterization of the defect can be reconstructed efficiently as well as robustly in the presence of noise. KW - Mechanical waves KW - Corrosion KW - Finite-element analysis KW - Ultrasonic testing KW - Nondestructive testing techniques KW - Symbolic computation KW - Materials analysis KW - MATLAB KW - Newton Raphson method PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565485 DO - https://doi.org/10.1121/10.0013574 VL - 152 IS - 2 SP - 1217 EP - 1229 PB - AIP Publ. CY - Melville, NY AN - OPUS4-56548 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böttcher, Katrin A1 - Schmitt Rahner, M. A1 - Stolzenberg, U. A1 - Kraft, Sebastian A1 - Bonse, Jörn A1 - Feist, C. A1 - Albrecht, D. A1 - Pullner, B. A1 - Krüger, Jörg T1 - Worst-case X-ray photon energies in ultrashort pulse laser processing N2 - Ultrashort pulse laser processing can result in the secondary generation of unwanted X-rays if a critical laser irradiance of about 10^13 W/cm^2 is exceeded. Spectral X-ray emissions were investigated during the processing of tungsten and steel using three complementary spectrometers (based on CdTe and silicon drift detectors) simultaneously for the identification of a worst-case spectral scenario. Therefore, maximum X-ray photon energies were determined, and corresponding dose equivalent rates were calculated. An ultrashort pulse laser workstation with a pulse duration of 274 fs, a center wavelength of 1030 nm, pulse repetition rates between 50 kHz and 200 kHz, and a Gaussian laser beam focused to a spot diameter of 33 µm was employed in a single pulse and burst laser operation mode. Different combinations of laser pulse energy and repetition rate were utilized, keeping the average laser power constant close to the maximum power of 20 W. Peak irradiances ranging from 7.3 × 10^13 W/cm^2 up to 3.0 × 10^14 W/cm^2 were used. The X-ray dose equivalent rate increases for lower repetition rates and higher pulse energy if a constant average power is used. Laser processing with burst mode significantly increases the dose rates and the X-ray photon energies. A maximum X-ray photon energy of about 40 keV was observed for burst mode processing of tungsten with a repetition rate of 50 kHz and a peak irradiance of 3 × 10^14 W/cm^2. KW - Ultrashort pulsed laser KW - X-ray emission KW - X-ray spectrum KW - X-ray energies KW - Radiation protection PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-566176 DO - https://doi.org/10.3390/ma15248996 VL - 15 IS - 24 SP - 1 EP - 17 PB - MDPI AN - OPUS4-56617 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Koch, Claudia T1 - Knowledge and technology transfer via publications, patents, standards: Exploring the hydrogen technological innovation system N2 - Clean technologies play a crucial role in reducing greenhouse gas emissions and protecting the climate. Hydrogen is a promising energy carrier and fuel that can be used in many applications. We explore the global hydrogen technological innovation system (TIS) by analyzing the three knowledge and technology transfer channels of publications, patents, and standards. Since the adoption of hydrogen technologies requires trust in their safety,this study specifically also focuses on hydrogen safety. Our results show that general and hydrogen safety research has increased significantly while patenting experienced stagnation. An analysis of the non-patent literature in safety patents shows little recognition of scientific publications. Similarly, publications are underrepresented in the analyzed 75 international hydrogen and fuel cell standards. This limited transfer of knowledge from published research to standards points to the necessity for greater involvement of researchers in standardization. We further derive implications for the hydrogen TIS and recommendations for a better and more impactful alignment of the three transfer channels. KW - Technological innovation system KW - Hydrogen safety KW - Knowledge and technology transfer KW - Publications KW - Patents KW - Standards PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564250 DO - https://doi.org/10.1016/j.techfore.2022.122201 SN - 0040-1625 VL - 187 SP - 1 EP - 14 PB - Elsevier Inc. AN - OPUS4-56425 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wild, B. A1 - Gerrits, Ruben A1 - Bonneville, S. T1 - The contribution of living organisms to rock weathering in the critical zone N2 - Rock weathering is a key process in global elemental cycling. Life participates in this process with tangible consequences observed from the mineral interface to the planetary scale. Multiple lines of evidence show that microorganisms may play a pivotal—yet overlooked—role in weathering. This topic is reviewed here with an emphasis on the following questions that remain unanswered: What is the quantitative contribution of bacteria and fungi to weathering? What are the associated mechanisms and do they leave characteristic imprints on mineral surfaces or in the geological record? Does biogenic weathering fulfill an ecological function, or does it occur as a side effect of unrelated metabolic functions and biological processes? An overview of efforts to integrate the contribution of living organisms into reactive transport models is provided. We also highlight prospective opportunities to harness microbial weathering in order to support sustainable agroforestry practices and mining activities, soil remediation, and carbon sequestration. KW - Bio-weathering KW - Fungi KW - Mineral PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-566748 DO - https://doi.org/10.1038/s41529-022-00312-7 SN - 2397-2106 VL - 6 SP - 1 EP - 16 PB - Macmillan CY - London AN - OPUS4-56674 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schnur, C. A1 - Goodarzi, P. A1 - Lugovtsova, Yevgeniya A1 - Bulling, Jannis A1 - Prager, Jens A1 - Tschöke, K. A1 - Moll, J. A1 - Schütze, A. A1 - Schneider, T. T1 - Towards interpretable machine learning for automated damage detection based on ultrasonic guided waves N2 - Data-driven analysis for damage assessment has a large potential in structural health monitoring (SHM) systems, where sensors are permanently attached to the structure, enabling continuous and frequent measurements. In this contribution, we propose a machine learning (ML) approach for automated damage detection, based on an ML toolbox for industrial condition monitoring. The toolbox combines multiple complementary algorithms for feature extraction and selection and automatically chooses the best combination of methods for the dataset at hand. Here, this toolbox is applied to a guided wave-based SHM dataset for varying temperatures and damage locations, which is freely available on the Open Guided Waves platform. A classification rate of 96.2% is achieved, demonstrating reliable and automated damage detection. Moreover, the ability of the ML model to identify a damaged structure at untrained damage locations and temperatures is demonstrated. KW - Composite structures KW - Structural health monitoring KW - Carbon fibre-reinforced plastic KW - Interpretable machine learning KW - Automotive industry PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542060 DO - https://doi.org/10.3390/s22010406 SN - 1424-8220 VL - 22 IS - 1 SP - 1 EP - 19 PB - MDPI CY - Basel AN - OPUS4-54206 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mellios, N. A1 - Oesch, Tyler A1 - Spyridis, P. T1 - Finite element modelling of UHPC under pulsating load using X-ray computed tomography based fiber distributions N2 - The benefits of including fibers in ultra-high performance concrete (UHPC) are attributed to their good bond with the matrix and, hence, an optimal utilization of their properties. At the same time, though, fiber reinforcement may contribute to anisotropy in the composite material and induce weak areas. The influence of the fibers’ orientation on the material properties is a matter of current scientific discourse and it is known to play a vital role in structural design. In the case studies presented herein, mechanical laboratory tests using pulsating load regimes on UHPC with a strength of more than 200 MPa were simulated by use of finite element models. The orientations of the fibers were measured for each test sample prior to failure using an X-ray computed tomography (CT) scanner, and these orientations are explicitly implemented into the model. The paper discusses the methodology of merging data retrieved by CT image processing and state-of-the-art FE simulation techniques Moreover, the CT scanning was carried out throughout the testing procedure, which further enables the comparison of the mechanical tests and the FE models in terms of damage propagation and failure patterns. The results indicate that the overall fiber configuration and behavior of the samples can be realistically modelled and validated by the proposed CT-FE coupling, which can enhance the structural analysis and design process of elements produced with steel fiber reinforced and UHPC materials. KW - Ultra-high performance concrete KW - Steel fiber reinforced concrete KW - Fiber orientation KW - X-ray computed tomography KW - Non-linear finite element modelling PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542105 DO - https://doi.org/10.1617/s11527-021-01833-4 SN - 1871-6873 VL - 55 IS - 1 SP - 1 EP - 20 PB - Springer CY - Dordrecht AN - OPUS4-54210 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scacco, F. A1 - Zerbst, Uwe A1 - Meneghetti, G. A1 - Madia, Mauro T1 - Comparison between PSM and IBESS approaches for the fatigue life estimation of weldments N2 - In the framework of the fatigue assessment of welded components, several methods are available in design standards such as the nominal stress, hot-spot stress, notch stress and linear elastic fracture mechanics approaches. The present paper aims at comparing two advanced local approaches for the fatigue strength assessment of different welded joints made of steel. The first one is IBESS which is based on short crack fracture mechanics. The second one is the PSM which instead involves the strain energy density approach. Both methods will be briefly presented, and the fatigue life prediction results discussed. The results obtained for the joint geometries considered in this work show advantages and drawbacks of the approaches, which are thoroughly analysed as well. KW - Fatigue KW - Welded joints KW - FAT class KW - IBESS KW - Peak stress method (PSM) KW - Finite element (FE) PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545139 DO - https://doi.org/10.1007/s40194-022-01284-7 SP - 1 EP - 23 PB - Springer AN - OPUS4-54513 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Valderrey, Virginia A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Thiourea- and Amino-Substituted Benzoxadiazole Dyes with Large Stokes Shifts as Red-Emitting Probe Monomers for Imprinted Polymer Layers Targeting Carboxylate-Containing Antibiotics N2 - Bifunctional fluorescent molecular oxoanion probes based on the benzoxadiazole (BD) chromophore are described which integrate a thiourea binding motif and a polymerizable 2-aminoethyl methacrylate unit in the 4,7-positions of the BD core. Concerted charge transfer in this electron donor-acceptor-donor architecture endows the dyes with strongly Stokes shifted (up to >250 nm) absorption and fluorescence. Binding of electron-rich carboxylate guests at the thiourea receptor leads to further analyte-induced red-shifts of the emission, shifting the fluorescence maximum of the complexes to ≥700 nm. Association constants for acetate are ranging from 1–5×105 M−1 in acetonitrile. Integration of one of the fluorescent probes through its polymerizable moiety into molecularly imprinted polymers (MIPs) grafted from the surface of submicron silica cores yielded fluorescent MIP-coated particle probes for the selective detection of antibiotics containing aliphatic carboxylate groups such as enoxacin (ENOX) at micromolar concentrations in highly polar solvents like acetonitrile. KW - Molecular imprinting KW - Anion recognition KW - Antibiotics KW - Benzoxadiazole dyes KW - Charge transfer KW - Fluorescence PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545027 DO - https://doi.org/10.1002/chem.202104525 SN - 1521-3765 SP - 1 EP - 9 PB - Wiley-VCH AN - OPUS4-54502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen T1 - Synthesis of polylactides by means of tin catalysts N2 - This article reviews the usefulness of tin(II) and tin(IV) salts and compounds as catalysts for the polymerization of lactides. The text is subdivided into nine parts mainly reflecting different polymerization strategies, such as ring-opening polymerization (ROP), ring-expansion polymerization (REP), ROP combined with simultaneous polycondensation (ROPPOC), various catalysts with unknown polymerization mechanisms, and polycondensation of lactic acid. Since the toxicity of tin salts and compounds is a matter of concern and frequently mentioned in numerous publications, the first section deals with facts instead of myths about the toxicity of tin salts and compounds. KW - Polylactide KW - MALDI-TOF MS KW - Tin catalysts PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545050 DO - https://doi.org/10.1039/d2py00092j SP - 1 EP - 30 PB - Royal Society for Chemistry AN - OPUS4-54505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Artinov, Antoni A1 - Meng, Xiangmeng A1 - Bachmann, Marcel A1 - Rethmeier, Michael T1 - Study on the transition behavior of the bulging effect during deep penetration laser beam welding N2 - The present work is devoted to the study of the transition behavior of the recently confirmed widening of the weld pool, known as the bulging effect, during high-power deep penetration laser beam welding of thick unalloyed steel sheets. A three-dimensional transient multi-physics numerical model is developed, allowing for the prediction of the bulge formation and the study of its temporal behavior. The model is generalized to account automatically for the transition from partial to complete penetration. Several experimental measurements and observations, such as drilling period, weld pool length, temperature, efficiency, and metallographic cross-sections are used to verify the model and assure the plausibility of the numerical results. The analysis of the calculated temperature and velocity distributions, as well as the evolution of the keyhole geometry, shows that the formation of a bulging region strongly depends on the penetration depth of the weld. Based on the numerical results, the bulge is found to occur transiently, having its transition from a slight bulge to a fully developed bulging between penetration depths of 6 mm and 9 mm, respectively. KW - Laser beam welding KW - Deep penetration KW - Bulge formation KW - Numerical modeling PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545067 DO - https://doi.org/10.1016/j.ijheatmasstransfer.2021.122171 VL - 184 SP - 122171 PB - Elsevier Ltd. AN - OPUS4-54506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ziesche, R.F. A1 - Hack, J. A1 - Rasha, L. A1 - Maier, M. A1 - Tan, C. A1 - Heenan, T.M.M. A1 - Markötter, Henning A1 - Kardjilov, N. A1 - Manke, I. A1 - Kockelmann, W. A1 - Brett, D.J.L. A1 - Shearing, P.R. T1 - High-speed 4D neutron computed tomography for quantifying water dynamics in polymer electrolyte fuel cells N2 - In recent years, low-temperature polymer electrolyte fuel cells have become an increasingly important pillar in a zero-carbon strategy for curbing climate change, with their potential to power multiscale stationary and mobile applications. The performance improvement is a particular focus of research and engineering roadmaps, with water management being one of the major areas of interest for development. Appropriate characterisation tools for mapping the evolution, motion and removal of water are of high importance to tackle shortcomings. This article demonstrates the development of a 4D high-speed neutron imaging technique, which enables a quantitative analysis of the local water evolution. 4D visualisation allows the time-resolved studies of droplet formation in the flow fields and water quantification in various cell parts. Performance parameters for water management are identified that offer a method of cell classification, which will, in turn, support computer modelling and the engineering of next-generation flow field designs. KW - Neutron imaging KW - Tomography KW - Polymer electrolyte membrane fuel cell PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545978 DO - https://doi.org/10.1038/s41467-022-29313-5 VL - 13 IS - 1 SP - 1616 PB - Nature Publishing Group UK CY - London AN - OPUS4-54597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riechers, Birte A1 - Roed, L. A1 - Mehri, S. A1 - Ingebrigtsen, T. A1 - Hecksher, T. A1 - Dyre, J. A1 - Niss, K. T1 - Predicting nonlinear physical aging of glasses from equilibrium relaxation via the material time N2 - The noncrystalline glassy state of matter plays a role in virtually all fields of materials science and offers complementary properties to those of the crystalline counterpart. The caveat of the glassy state is that it is out of equilibrium and therefore exhibits physical aging, i.e., material properties change over time. For half a century, the physical aging of glasses has been known to be described well by the material-time concept, although the existence of a material time has never been directly validated. We do this here by successfully predicting the aging of the molecular glass 4-vinyl-1,3-dioxolan-2-one from its linear relaxation behavior. This establishes the defining property of the material time. Via the fluctuation-dissipation theorem, our results imply that physical aging can be predicted from thermal-equilibrium fluctuation data, which is confirmed by computer simulations of a binary liquid mixture. KW - Physical aging KW - Equilibrium relaxation KW - Glass PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546015 DO - https://doi.org/10.1126/sciadv.abl9809 SN - 2375-2548 VL - 8 IS - 11 SP - 1 EP - 8 PB - American Association for the Advancement of Science CY - Washington, DC AN - OPUS4-54601 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kudela, P. A1 - Radzienski, M. A1 - Moix-Bonet, M. A1 - Willberg, C. A1 - Lugovtsova, Yevgeniya A1 - Bulling, Jannis A1 - Tschöke, K. A1 - Moll, J. T1 - Dataset on full ultrasonic guided wavefield measurements of a CFRP plate with fully bonded and partially debonded omega stringer N2 - The fourth dataset dedicated to the Open Guided Waves platform presented in this work aims at a carbon fiber composite plate with an additional omega stringer at constant temperature conditions. The dataset provides full ultrasonic guided wavefields. Two types of signals were used for guided wave excitation, namely chirp signal and tone-burst signal. The chirp signal had a frequency range of 20-500kHz. The tone-burst signals had a form of sine modulated by Hann window with 5 cycles and carrier frequencies 16.5kHz, 50kHz, 100kHz, 200kHz, 300kHz. The piezoceramic actuator used for this purpose was attached to the center of the stringer side surface of the core plate. Three scenarios are provided with this setup: (1) wavefield measurements without damage, (2) wavefield measurements with a local stringer debond and (3) wavefield measurements with a large stringer debond. The defects were caused by impacts performed from the backside of the plate. As result, the stringer feet debonds locally which was verified with conventional ultrasound measurements. KW - Lamb waves KW - Composite panel KW - Impact damage KW - Damage detection KW - Scanning laser Doppler vibrometry KW - Structural health monitoring KW - Non-destructive evaluation KW - Open data PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545242 DO - https://doi.org/10.1016/j.dib.2022.108078 SN - 2352-3409 VL - 42 SP - 1 EP - 13 PB - Elsevier CY - Amsterdam AN - OPUS4-54524 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Doolette, A. A1 - Huang, J. T1 - Combining diffusive gradients in thin-films (DGT) and 31P NMR spectroscopy to determine phosphorus species in soil N2 - The diffusive gradients in thin-films (DGT) technique shows in many publications a superior correlation to the amount of plant-available phosphorus (P) in soil. However, this technique cannot give information on the plant-available P species in soil. Therefore, we combined DGT with solution 31P nuclear magnetic resonance (NMR) spectroscopy. This was achieved by using a modified DGT device in which the diffusive layer had a larger pore size, the binding layer incorporated an adsorption material with a higher capacity, and the device had a larger exposure area. The spectroscopic investigation was undertaken after elution of the deployed DGT binding layer in a NaOH solution. Adsorption tests using solutions of known organic P compounds showed that a sufficient amount of these compounds could be adsorbed on the binding layer in order for them to be analyzed by solution 31P NMR spectroscopy. Furthermore, various intermediates of the hydrolysis of trimetaphosphate in soil could be also analyzed over time. KW - Phosphorus KW - Diffusive gradients in thin-films (DGT) KW - Passive sampling KW - fertilizer PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545759 DO - https://doi.org/10.1002/ael2.20068 VL - 7 IS - 1 SP - e20068 PB - Wiley online library AN - OPUS4-54575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kromm, Arne A1 - Thomas, Maximilian A1 - Kannengießer, Thomas A1 - Gibmeier, J. A1 - Vollert, F. T1 - Assessment of the Solidification Cracking Susceptibility of Welding Consumables in the Varestraint Test by Means of an Extended Evaluation Methodology N2 - Various test methods are available for assessing the susceptibility of materials to solidification cracking during welding. In the widely used Varestraint test, the crack length is selected as a criterion as a function of the applied bending strain. Unfortunately, the crack length does not characterize the material behavior alone but depends to varying degrees on the individual test parameters used, which makes the interpretation of the results difficult. In addition, the crack length is not comparable under different test conditions. To overcome these disadvantages, we have developed a novel evaluation methodology that decouples the machine influence from the material behavior. The measured crack length is related to the maximum possible value specified by welding speed and deformation time. This relative crack length is calculated numerically, considering the orientation of the cracks. Experiments on two high-alloy martensitic welding consumables show that, in contrast to the conventional evaluation, a comparison of different welding parameters becomes possible. Furthermore, the strain rate proved to be a suitable crack criterion in agreement with Prokhorov's hot cracking model. KW - Welding KW - Solidification cracking KW - Varestraint test PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545780 DO - https://doi.org/10.1002/adem.202101650 SN - 1438-1656 SP - 2101650 PB - Wiley online library AN - OPUS4-54578 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zaghdoudi, Maha A1 - Kömmling, Anja A1 - Jaunich, Matthias A1 - Wolff, Dietmar T1 - Oxidative ageing of elastomers: Experiment and modelling N2 - During an extensive test programme at the Bundesanstalt für Materialforschung und prüfung, material property changes of EPDM O-rings were investigated at different ageing times and two ageing temperatures of 125∘C and 150∘C. To exclude possible diffusion-limited oxidation (DLO) effects that can distort the data, IRHD microhardness measurements were taken over the cross section of compressed O-rings. Continuous stress relaxation measurements were taken on samples free of DLO effects. The additional effect of physical processes to irreversible chemical ones during a long-term thermal exposure is quantified by the analysis of compression set measurements under various test conditions. By combining the different experimental methods, characteristic times relative to the degradation processes were determined. On the basis of experimental data, a microphysically motivated model that takes into account reversible and irreversible processes was developed. The parameter identification strategy of the material model is based on our experimental investigations on homogeneously aged elastomer O-rings. The simulated results are in good agreement with the experiments. KW - Compression stress relaxation KW - Compression set KW - IRHD microhardness KW - Modelling PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545910 DO - https://doi.org/10.1007/s00161-022-01093-9 SN - 1432-0959 SP - 1 EP - 9 PB - Springer CY - Berlin AN - OPUS4-54591 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zorn, R. A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed Aejaz A1 - Malpass-Evans, R. A1 - McKeown, N. A1 - Tyagi, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Low frequency vibrations and diffusion in disordered polymers bearing an intrinsic microporosity as revealed by neutron scattering N2 - The microscopic diffusion and the low frequency density of states (VDOS) of PIM-EATB(CH3) are investigated by inelastic and quasi-elastic neutron scattering where also the demethylated counterpart of PIM-EA-TB(H2) is considered. These intrinsic microporous polymers are characterized by large BET surface area values of several hundred m2/g and pore sizes between 0.5 and 2 nm. Detailed comparison is made to the archetype of polymers of intrinsic microporosity, PIM-1, and polynorbornenes also bearing a microporosity. Due to the wavelength of neutrons, the diffusion and vibrations can be addressed on microscopic length and time scales. From the inelastic neutron scattering experiments the low frequency density of states (VDOS) is estimated which shows excess contributions to the Debye-type VDOS known as Boson peak. It was found that the maximum frequency of the Boson peak decreases with increasing microporosity characterized by the BET surface area. However, besides the BET surface area, additional factors such as the backbone stiffness govern the maximum frequency of the Boson peak. Further the mean squared displacement related to microscopic motions was estimated from elastic fixed window scans. At temperatures above 175 K, the mean squared displacement PIM-EA-TB(CH3) is higher than that for the demethylated counterpart PIM-EA-TB(H2). The additional contribution found for PIM-EATB(CH3) is ascribed to the rotation of the methyl group in this polymer because the only difference between the two structures is that PIM-EA-TB(CH3) has methyl groups where PIM-EA-TB(H2) has none. A detailed comparison of the molecular dynamics is also made to that of PIM-1 and the microporous polynorbornene PTCNSi1. The manuscript focuses on the importance of vibrations and the localized molecular mobility characterized by the microscopic diffusion on the gas Transport in polymeric separation membranes. In the frame of the random gate model localized fluctuations can open or close bottlenecks between pores to enable the diffusion of gas molecules. KW - Polymer of intrisic microporosity KW - Neutron scattering KW - Boson peak KW - Methyl group rotation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538490 DO - https://doi.org/10.3390/cryst11121482 VL - 11 IS - 12 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-53849 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Wiehle, Philipp A1 - Munsch, Sarah Mandy T1 - About the dominance of mesopores in physisorption in amorphous materials N2 - Amorphous, porous materials represent by far the largest proportion of natural and men-made materials. Their pore networks consists of a wide range of pore sizes, including mesoand macropores. Within such a pore network, material moisture plays a crucial role in almost all transport processes. In the hygroscopic range, the pores are partially saturated and liquid water is only located at the pore fringe due to physisorption. Therefore, material parameters such as porosity or median pore diameter are inadequate to predict material moisture and moisture transport. To quantify the spatial distribution of material moisture, Hillerborg’s adsorption Theory is used to predict the water layer thickness for different pore geometries. This is done for all pore sizes, including those in the lower nanometre range. Based on this approach, it is shown that the material moisture is almost completely located in mesopores, although the pore network is highly dominated by macropores. Thus, mesopores are mainly responsible for the moisture storage capacity, while macropores determine the moisture transport capacity, of an amorphous material. Finally, an electrical analogical circuit is used as a model to predict the diffusion coefficient based on the pore-size distribution, including physisorption. KW - Physisorption KW - Mesopores KW - Amorphous materials KW - Macropores KW - Adsorbed water layer thickness KW - Material moisture KW - Moisture distribution PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538525 UR - https://dataverse.harvard.edu/dataset.xhtml?persistentId=doi:10.7910/DVN/NILGW2 DO - https://doi.org/10.3390/molecules26237190 VL - 26 IS - 23 SP - 1 EP - 22 PB - MDPI AN - OPUS4-53852 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Musl, O. A1 - Sulaeva, I. A1 - Sumerskii, I. A1 - Mahler, A.K. A1 - Rosenau, T. A1 - Falkenhagen, Jana A1 - Potthast, A. T1 - Mapping of the Hydrophobic Composition of Lignosulfonates N2 - Lignosulfonates are industrial biorefinery products that are characterized by significant variability and heterogeneity in their structural composition. Typically, they exhibit high dispersities in molar mass (molar mass distribution-MMD) and in functionalities (functionality-type distribution - FTD), which crucially affect their material usage. In terms of FTD, state-of-the-art Lignin analytics still rely mainly on the determination of functional group contents, which are statistical averages with limited explanatory power. In contrast, our online hydrophobic interaction chromatography−size-exclusion chromatography 2D-LC approach combines the determination of both MMD and FTD in a single measurement to provide a comprehensive picture of the characteristic composition of industrial lignosulfonates information hitherto inaccessible by state-of-the-art lignin analytics. In this way, the complex inter - relationships between these two important structural parameters can be studied in an unprecedented manner. In this study, we reveal the considerable differences in terms of hydrophobic composition and its dispersity present in a range of different industrial lignosulfonates - data desperately needed in tailoring and refining of lignosulfonate composition for material usage. KW - Lignosulfonates KW - Amphiphilicity KW - Hydrophobic interaction chromatography KW - Two-dimensional chromatography (2D-LC) KW - Charge-to-size-ratio PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538612 DO - https://doi.org/10.1021/acssuschemeng.1c06469 VL - 9 IS - 49 SP - 16786 EP - 16795 PB - ASC Publications AN - OPUS4-53861 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Erdmann, Eileen A1 - Nitsche, Sarah A1 - Gorbushina, Anna A1 - Schumacher, Julia T1 - Genetic Engineering of the Rock Inhabitant Knufia petricola Provides Insight Into the Biology of Extremotolerant Black Fungi N2 - Black microcolonial fungi (Ascomycetes from Arthonio-, Dothideo-, and Eurotiomycetes) are stress-tolerant and persistent dwellers of natural and anthropogenic extreme habitats. They exhibit slow yeast-like or meristematic growth, do not form specialized reproduction structures and accumulate the black pigment 1,8-dihydroxynaphthalene (DHN) melanin in the multilayered cell walls. To understand how black fungi live, survive, colonize mineral substrates, and interact with phototrophs genetic methods are needed to test these functions and interactions. We chose the rock inhabitant Knufia petricola of the Chaetothyriales as a model for developing methods for genetic manipulation. Here, we report on the expansion of the genetic toolkit by more efficient multiplex CRISPR/Cas9 using a plasmid-based system for expression of Cas9 and multiple sgRNAs and the implementation of the three resistance selection markers genR (geneticin/nptII), baR (glufosinate/bar), and suR (chlorimuron ethyl/sur). The targeted integration of expression constructs by replacement of essential genes for pigment synthesis allows for an additional color screening of the transformants. The black-pink screening due to the elimination of pks1 (melanin) was applied for promoter studies using GFP fluorescence as reporter. The black-white screening due to the concurrent elimination of pks1 and phs1 (carotenoids) allows to identify transformants that contain the two expression constructs for co-localization or bimolecular fluorescence complementation (BiFC) studies. The co-localization and interaction of the two K. petricola White Collar orthologs were demonstrated. Two intergenic regions (igr1, igr2) were identified in which expression constructs can be inserted without causing obvious phenotypes. Plasmids of the pNXR-XXX series and new compatible entry plasmids were used for fast and easy generation of expression constructs and are suitable for a broad implementation in other fungi. This variety of genetic tools is opening a completely new perspective for mechanistic and very detailed study of expression, functioning and regulation of the genes/proteins encoded by the genomes of black fungi. KW - Microcolonial fungi KW - DHN melanin KW - Cloning vectors KW - Genetics PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546192 DO - https://doi.org/10.3389/ffunb.2022.862429 SN - 2673-6128 VL - 3 PB - Frontiers Media CY - Lausanne AN - OPUS4-54619 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beyer, S. A1 - Kimani, Martha Wamaitha A1 - Zhang, Y. A1 - Verhassel, A. A1 - Sternbæk, L. A1 - Wang, T. A1 - Persson, J. L. A1 - Härkönen, P. A1 - Johansson, E. A1 - Caraballo, R. A1 - Elofsson, M. A1 - Gawlitza, Kornelia A1 - Rurack, Knut A1 - Ohlsson, L. A1 - El-Schich, Z. A1 - Gjörloff Wingren, A. A1 - Stollenwerk, M. M. T1 - Fluorescent Molecularly Imprinted Polymer Layers against Sialic Acid on Silica-coated Polystyrene Cores - Assessment of the Binding Behavior to Cancer Cells N2 - Sialic acid (SA) is a monosaccharide usually linked to the terminus of glycan chains on the cell surface. It plays a crucial role in many biological processes, and hypersialylation is a common feature in cancer. Lectins are widely used to analyze the cell surface expression of SA. However, these protein molecules are usually expensive and easily denatured, which calls for the development of alternative glycan-specific receptors and cell imaging technologies. In this study, SA-imprinted fluorescent core-shell molecularly imprinted polymer particles (SA-MIPs) were employed to recognize SA on the cell surface of cancer cell lines. The SA-MIPs improved suspensibility and scattering properties compared with previously used core-shell SA-MIPs. Although SA-imprinting was performed using SA without preference for the alpha-2,3- and alpha-2,6-SA forms, we screened the cancer cell lines analyzed using the lectins Maackia Amurensis Lectin I (MAL I, alpha-2,3-SA) and Sambucus Nigra Lectin (SNA, alpha-2,6-SA). Our results show that the selected cancer cell lines in this study presented a varied binding behavior with the SA-MIPs. The binding pattern of the lectins was also demonstrated. Moreover, two different pentavalent SA conjugates were used to inhibit the binding of the SA-MIPs to breast, skin, and lung cancer cell lines, demonstrating the specificity of the SA-MIPs in both flow cytometry and confocal fluorescence microscopy. We concluded that the synthesized SA-MIPs might be a powerful future tool in the diagnostic analysis of various cancer cells. KW - Cancer KW - Imprinting KW - Molecularly imprinted polymers KW - SA conjugates KW - Sialic acid PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546625 DO - https://doi.org/110.3390/cancers14081875 SN - 2072-6694 VL - 14 IS - 8 PB - MDPI CY - Basel AN - OPUS4-54662 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauzon, C. A1 - Mishurova, Tatiana A1 - Fischer, M. A1 - Ahlström, J. A1 - Fritsch, Tobias A1 - Bruno, Giovanni A1 - Hryha, Eduard T1 - Impact of contour scanning and helium-rich process gas on performances of Alloy 718 lattices produced by laser powder bed fusion N2 - Contour scanning and process gas type are process parameters typically considered achieving second order effects compared to first order factors such as laser power and scanning speed. The present work highlights that contour scanning is crucial to ensure geometrical accuracy and thereby the high performance under uniaxial compression of complex Alloy 718 lattice structures. Studies of X-ray computed tomography visualizations of as-built and compression-strained structures reveal the continuous and smooth bending and compression of the walls, and the earlier onset of internal contact appearance in the denser lattices printed with contour. In contrast, the effect of addition of He to the Ar process gas appears to have limited influence on the mechanical response of the lattices and their microstructure as characterized by electron backscattered diffraction. However, the addition of He proved to significantly enhance the cooling rate and to reduce the amount of the generated spatters as evidenced by in situ monitoring of the process emissions, which is very promising for the process stability and powder reusability during laser powder bed fusion. KW - Additive manufacturing KW - Laser powder bed fusion KW - Gyroid lattice KW - Process atmosphere PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546632 DO - https://doi.org/10.1016/j.matdes.2022.110501 SN - 0264-1275 VL - 215 SP - 110501 PB - Elsevier Ltd. AN - OPUS4-54663 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - D'Accardi, E. A1 - Krankenhagen, Rainer A1 - Ulbricht, Alexander A1 - Pelkner, Matthias A1 - Pohl, Rainer A1 - Palumbo, D. A1 - Galietti, U. T1 - Capability to detect and localize typical defects of laser powder bed fusion (L‑PBF) process: an experimental investigation with different non‑destructive techniques N2 - Additive manufacturing (AM) technologies, generally called 3D printing, are widely used because their use provides a high added value in manufacturing complex-shaped components and objects. Defects may occur within the components at different time of manufacturing, and in this regard, non-destructive techniques (NDT) represent a key tool for the quality control of AM components in many industrial fields, such as aerospace, oil and gas, and power industries. In this work, the capability of active thermography and eddy current techniques to detect real imposed defects that are representative of the laser powder bed fusion process has been investigated. A 3D complex shape of defects was revealed by a μCT investigation used as reference results for the other NDT methods. The study was focused on two different types of defects: porosities generated in keyhole mode as well as in lack of fusion mode. Different thermographic and eddy current measurements were carried out on AM samples, providing the capability to detect volumetric irregularly shaped defects using non-destructive methods. KW - Additive Manufacturing KW - Defect detection KW - Thermography KW - Eddy-current testing KW - Micro-computed tomography PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546680 DO - https://doi.org/10.1007/s40964-022-00297-4 SN - 2363-9512 VL - 7 IS - 6 SP - 1239 EP - 1256 PB - Springer AN - OPUS4-54668 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Getenet, M. A1 - Garcia-Ruiz, J. M. A1 - Otálora, F. A1 - Emmerling, Franziska A1 - Al-Sabbagh, Dominik A1 - Verdugo-Escamilla, E. T1 - A comprehensive methodology for monitoring evaporitic mineral precipitation and hydrochemical evolution of saline lakes: The case of Lake Magadi soda brine (East African Rift Valley, Kenya) N2 - Lake Magadi, East African Rift Valley, is a hyperalkaline and saline soda lake highly enriched in Na+, K+, CO32–, Cl–, HCO3–, and SiO2 and depleted in Ca2+ and Mg2+, where thick evaporite deposits and siliceous sediments have been forming for 100 000 years. The hydrogeochemistry and the evaporite deposits of soda lakes are subjects of growing interest in paleoclimatology, astrobiology, and planetary sciences. In Lake Magadi, different hydrates of sodium carbonate/bicarbonate and other saline minerals precipitate. The precipitation sequence of these minerals is a key for understanding the hydrochemical evolution, the paleoenvironmental conditions of ancient evaporite deposits, and industrial crystallization. However, accurate determination of the precipitation sequence of these minerals was challenging due to the dependency of the different hydrates on temperature, water activity, pH and pCO2, which could induce phase transformation and secondary mineral precipitation during sample handling. Here, we report a comprehensive methodology applied for monitoring the evaporitic mineral precipitation and hydrochemical evolution of Lake Magadi. Evaporation and mineral precipitations were monitored by using in situ video microscopy and synchrotron X-ray diffraction of acoustically levitated droplets. The mineral patterns were characterized by ex situ Raman spectroscopy, X-ray diffraction, and scanning electron microscopy. Experiments were coupled with thermodynamic models to understand the evaporation and precipitation-driven hydrochemical evolution of brines. Our results closely reproduced the mineral assemblages, patterns, and textural relations observed in the natural setting. Alkaline earth carbonates and fluorite were predicted to precipitate first followed by siliceous sediments. Among the salts, dendritic and acicular trona precipitate first via fractional crystallization─reminiscent of grasslike trona layers of Lake Magadi. Halite/villiaumite, thermonatrite, and sylvite precipitate sequentially after trona from residual brines depleted in HCO3–. The precipitation of these minerals between trona crystals resembles the precipitation process observed in the interstitial brines of the trona layers. Thermonatrite precipitation began after trona equilibrated with the residual brines due to the absence of excess CO2 input. We have shown that evaporation and mineral precipitation are the major drivers for the formation of hyperalkaline, saline, and SiO2-rich brines. The discrepancy between predicted and actual sulfate and phosphate ion concentrations implies the biological cycling of these ions. The combination of different in situ and ex situ methods and modeling is key to understanding the mineral phases, precipitation sequences, and textural relations of modern and ancient evaporite deposits. The synergy of these methods could be applicable in industrial crystallization and natural brines to reconstruct the hydrogeochemical and hydroclimatic conditions of soda lakes, evaporite settings, and potentially soda oceans of early Earth and extraterrestrial planets. KW - Crystallization KW - Precipitation KW - Crystals KW - Evaporation KW - Minerals PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546712 DO - https://doi.org/10.1021/acs.cgd.1c01391 SN - 1528-7483 VL - 22 IS - 4 SP - 2307 EP - 2317 PB - ACS Publications CY - Washington, DC AN - OPUS4-54671 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Straße, Anne A1 - Gumenyuk, Andrey A1 - Rethmeier, Michael T1 - Study on Duplex Stainless Steel Powder Compositions for the Coating of thick Plates of Laser Beam Welding N2 - Duplex stainless steels combine the positive properties of its two phases, austenite and ferrite. Due to its good corrosion resistance, high tensile strength, and good ductility, it has multiple applications. But laser beam welding of duplex steels changes the balanced phase distribution in favor of ferrite. This results in a higher vulnerability to corrosion and a lower ductility. Herein, different powder combinations consisting of duplex and nickel for coating layers by laser metal deposition (LMD) are investigated. Afterward, laser tracks are welded, and the temperature cycles are measured. The ferrite content of the tracks is analyzed by feritscope, metallographic analysis, and electron backscatter diffraction. The goal is the development of a powder mixture allowing for a duplex microstructure in a two-step process, where first the edges of the weld partners are coated with the powder mixture by LMD and second those edges are laser beam welded. The powder mixture identified by the pretests is tested in the two-step process and analyzed by metallographic analysis, energy-dispersive X-ray spectroscopy, and Vickers hardness tests. The resulting weld seams show a balanced duplex microstructure with a homogenous nickel distribution and a hardness of the weld seam similar to the base material. KW - Duplex AISI 2205 KW - Laser metal deposition KW - Laser beam welding KW - Nickel KW - Stainless steels PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547024 DO - https://doi.org/10.1002/adem.202101327 SN - 1438-1656 SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54702 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Marko, A. A1 - Bähring, S. A1 - Raute, J. A1 - Biegler, M. A1 - Rethmeier, Michael T1 - Quality Prediction in Directed Energy Deposition Using Artificial Neural Networks Based on Process Signals N2 - The Directed Energy Deposition process is used in a wide range of applications including the repair, coating or modification of existing structures and the additive manufacturing of individual parts. As the process is frequently applied in the aerospace industry, the requirements for quality assurance are extremely high. Therefore, more and more sensor systems are being implemented for process monitoring. To evaluate the generated data, suitable methods must be developed. A solution, in this context, was the application of artificial neural networks (ANNs). This article demonstrates how measurement data can be used as input data for ANNs. The measurement data were generated using a pyrometer, an emission spectrometer, a camera (Charge-Coupled Device) and a laser scanner. First, a concept for the extraction of relevant features from dynamic measurement data series was presented. The developed method was then applied to generate a data set for the quality prediction of various geometries, including weld beads, coatings and cubes. The results were compared to ANNs trained with process parameters such as laser power, scan speed and powder mass flow. It was shown that the use of measurement data provides additional value. Neural networks trained with measurement data achieve significantly higher prediction accuracy, especially for more complex geometries. KW - DED KW - Artificial neural network KW - Process monitoring KW - Quality assurance KW - Data preparation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547039 DO - https://doi.org/10.3390/app12083955 VL - 12 IS - 8 SP - 1 EP - 13 PB - MDPI AN - OPUS4-54703 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geisen, O. A1 - Müller, V. A1 - Graf, B. A1 - Rethmeier, Michael T1 - Integrated weld preparation designs for the joining of L‑PBF and conventional components via TIG welding N2 - size limitations and high production costs of L-PBF make it competitive for smaller, highly complex components, while the less complex elements of an assembly are manufactured conventionally. This leads to scenarios that use L-PBF only where it’s beneficial, and it require an integration and joining to form the final product. For example, L-PBF combustion swirlers are welded onto cast parts to produce combustion systems for stationary gas turbines. Today, the welding process requires complex welding fixtures and tack welds to ensure the correct alignment and positioning of the parts for repeatable weld results. In this paper, L-PBF and milled weld preparations are presented as a way to simplify the Tungsten inert gas (TIG) welding of rotationally symmetrical geometries using integrated features for alignment and fixation. Pipe specimens with the proposed designs are manufactured in Inconel 625 using L-PBF and milling. The pipe assembly is tested and TIG welding is performed for validation. 3D scans of the pipes before and after welding are evaluated, and the weld quality is examined via metallography and computed tomography (CT) scans. All welds produced in this study passed the highest evaluation group B according to DIN 5817. Thanks to good component alignment, safe handling, and a stable welding process, the developed designs eliminate the need for part-specific fixtures, simplify the process chain, and increase the process reliability. The results are applicable to a wide range of components with similar requirements. KW - L-PBF KW - AM feature integration KW - TIG welding KW - Integrated alignment features KW - Pipe weld preparation KW - Dissimilar joints KW - Inconel 625 PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547042 DO - https://doi.org/10.1007/s40964-021-00221-2 SN - 2363-9512 SP - 1 EP - 11 PB - Springer AN - OPUS4-54704 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kolmangadi, Mohamed Aejaz A1 - Szymoniak, Paulina A1 - Zorn, R. A1 - Böhning, Martin A1 - Wolff, M. A1 - Zamponi, M. A1 - Schönhals, Andreas T1 - Molecular mobility in high-performance polynorbornenes:A combined broadband dielectric, advanced calorimetry,and neutron scattering investigation N2 - The molecular dynamics of two addition type polynorbornenes, exo-PNBSiand PTCNSi1, bearing microporosity has been investigated by broadbanddielectric spectroscopy, fast scanning calorimetry, and neutron scattering. Bothpolymers have the same side groups but different backbones. Due to theirfavorable transport properties, these polymers have potential applications inseparation membranes for gases. It is established in literature that molecularfluctuations are important for the diffusion of small molecules through poly-mers. For exo-PNBSi, two dielectric processes are observed, which are assignedto Maxwell/Wagner/Sillars (MWS) process due to blocking of charge carriersat internal voids or pore walls. For PTCNSi1, one MWS-polarization process isfound. This points to a bimodal pore-size distribution for exo-PNBSi. A glasstransition for exo-PNBSi and for PTCNSi1 could be evidenced for the first timeusing fast scanning calorimetry. For Tgand the corresponding apparent activa-tion energy, higher values were found for PTCNSi1 compared to exo-PNBSi.For both polymers, the neutron scattering data reveal one relaxation process.This process is mainly assigned to methyl group rotation probably overlayedby carbon–carbon torsional fluctuations. KW - Advanced calorimetry KW - Dielectric spectroscopy KW - Neutron scattering KW - Polynorbornenes PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547086 DO - https://doi.org/10.1002/pen.25995 SN - 0032-3888 VL - 62 IS - 7 SP - 2143 EP - 2155 PB - Wiley AN - OPUS4-54708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Anderhalten, L. A1 - Silva, R. V. A1 - Morr, A. A1 - Wang, S. A1 - Smorodchenko, A. A1 - Saatz, Jessica A1 - Traub, Heike A1 - Mueller, S. A1 - Boehm-Sturm, P. A1 - Rodriguez-Sillke, Y. A1 - Kunkel, D. A1 - Hahndorf, J. A1 - Paul, F. A1 - Taupitz, M. A1 - Sack, I. A1 - Infante-Duarte, C. T1 - Different Impact of Gadopentetate and Gadobutrol on Inflammation-Promoted Retention and Toxicity of Gadolinium Within the Mouse Brain N2 - Objectives: Using a murine model of multiple sclerosis, we previously showed that repeated administration of gadopentetate dimeglumine led to retention of gadolinium (Gd) within cerebellar structures and that this process was enhanced with inflammation. This study aimed to compare the kinetics and retention profiles of Gd in inflamed and healthy brains after application of the macrocyclic Gd-based contrast agent (GBCA) gadobutrol or the linear GBCA gadopentetate. Moreover, potential Gd-induced neurotoxicity was investigated in living hippocampal slices ex vivo. Materials and Methods: Mice at peak of experimental autoimmune encephalomyelitis (EAE; n = 29) and healthy control mice (HC; n = 24) were exposed to a cumulative dose of 20 mmol/kg bodyweight of either gadopentetate dimeglumine or gadobutrol (8 injections of 2.5 mmol/kg over 10 days). Magnetic resonance imaging (7 T) was performed at baseline as well as at day 1, 10, and 40 post final injection (pfi) of GBCAs. Mice were sacrificed after magnetic resonance imaging and brain and blood Gd content was assessed by laser ablation-inductively coupled plasma (ICP)-mass spectrometry (MS) and ICP-MS, respectively. In addition, using chronic organotypic hippocampal slice cultures, Gd-induced neurotoxicity was addressed in living brain tissue ex vivo, both under control or inflammatory (tumor necrosis factor α [TNF-α] at 50 ng/μL) conditions. Results: Neuroinflammation promoted a significant decrease in T1 relaxation times after multiple injections of both GBCAs as shown by quantitative T1 mapping of EAE brains compared with HC. This corresponded to higher Gd retention within the EAE brains at 1, 10, and 40 days pfi as determined by laser ablation-ICP-MS. In inflamed cerebellum, in particular in the deep cerebellar nuclei (CN), elevated Gd retention was observed until day 40 after last gadopentetate application (CN: EAE vs HC, 55.06 ± 0.16 μM vs 30.44 ± 4.43 μM). In contrast, gadobutrol application led to a rather diffuse Gd content in the inflamed brains, which strongly diminished until day 40 (CN: EAE vs HC, 0.38 ± 0.08 μM vs 0.17 ± 0.03 μM). The analysis of cytotoxic effects of both GBCAs using living brain tissue revealed an elevated cell death rate after incubation with gadopentetate but not gadobutrol at 50 mM. The cytotoxic effect due to gadopentetate increased in the presence of the inflammatory mediator TNF-α (with vs without TNF-α, 3.15% ± 1.18% vs 2.17% ± 1.14%; P = 0.0345). Conclusions: In the EAE model, neuroinflammation promoted increased Gd retention in the brain for both GBCAs. Whereas in the inflamed brains, efficient clearance of macrocyclic gadobutrol during the investigated time period was observed, the Gd retention after application of linear gadopentetate persisted over the entire observational period. Gadopentetate but not gadubutrol appeared to be neurotoxic in an ex vivo paradigm of neuronal inflammation. KW - Imaging KW - ICP-MS KW - Gadolinium KW - Contrast agent KW - Laser ablation KW - Brain KW - Multiple sclerosis PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546910 DO - https://doi.org/10.1097/RLI.0000000000000884 SN - 0020-9996/22/0000–0000 VL - 57 IS - 10 SP - 677 EP - 688 PB - Wolters Kluwer N.V. CY - Alphen aan den Rijn, The Netherlands AN - OPUS4-54691 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Almalla, A. A1 - Özcan Sandikcioglu, Özlem A1 - Witt, Julia T1 - In Situ Atomic Force Microscopy Analysis of the Corrosion Processes at the Buried Interface of an Epoxy-like Model Organic Film and AA2024-T3 Aluminum Alloy N2 - The application of characterization methods with high spatial resolution to the analysis of buried coating/metal interfaces requires the design and use of model systems. Herein, an epoxy-like thin film is used as a model coating resembling the epoxy-based coatings and adhesives widely used in technical applications. Spin coating is used for the deposition of a 30 nm-thin bilayer (BL) composed of poly-(ethylenimine) (PEI) and poly[(o-cresyl glycidyl ether)-co-formaldehyde] (CNER). Fourier-transform infrared spectroscopy (FTIR) results confirm that the exposure of coated AA2024-T3 (AA) samples to the corrosive electrolyte solution does not cause the degradation of the polymer layer. In situ atomic force microscopy (AFM) studies are performed to monitor local corrosion processes at the buried interface of the epoxy-like film and the AA2024-T3 aluminum alloy surface in an aqueous electrolyte solution. Hydrogen evolution due to the reduction of water as the cathodic corrosion reaction leads to local blister formation. Based on the results of the complementary energy-dispersive X-ray spectroscopy (EDX) analysis performed at the same region of interest, most of the hydrogen evolved originates at the vicinity of Mg-containing intermetallic particles. KW - Scanning Kelvin probe force microscopy KW - Aluminum alloys KW - Buried interfaces KW - In situ atomic force microscopy KW - Local corrosion PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546932 DO - https://doi.org/10.1002/adem.202101342 SN - 1438-1656 SP - 1 EP - 9 PB - Wiley VHC-Verlag AN - OPUS4-54693 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sözen, H.I. A1 - Mendive-Tapia, E. A1 - Hickel, Tilmann A1 - Neugebauer, J. T1 - Ab initio investigations of point and complex defect structures in B2-FeAl N2 - We study single-site and two-site defect structures in B2-type Fe-Al alloys by means of density functional theory supercell calculations. The defect formation energies are calculated as functions of the chemical potential, which are used to obtain the dependence of the defect concentrations on Al content at different temperatures. We also examine the converging behavior of the formation energies with respect to the supercell size to study the corresponding limit of dilute defects. The effect of magnetism is investigated by considering nonmagnetic, ferromagnetic, and paramagnetic states, calculations for the latter showing that the magnitude of the local magnetic moments strongly impacts the defect formation energies. The methodological studies are used to provide explanations for the wide spread of defect formation energies reported by experiments and other theoretical investigations. Based on these insights, the stability of the B2-FeAl structure as a function of Al concentration is obtained and discussed. KW - Atomistic models KW - Defects KW - Thermodynamics PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546956 DO - https://doi.org/10.1103/PhysRevMaterials.6.023603 SN - 2475-9953 VL - 6 IS - 2 SP - 1 EP - 11 PB - APS CY - College Park, MD AN - OPUS4-54695 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hieu, D.T. A1 - Kosslick, H. A1 - Riaz, M. A1 - Schulz, A. A1 - Springer, A. A1 - Frank, M. A1 - Jäger, Christian A1 - Minh Thu, N.T. A1 - Son, L.T. T1 - Acidity and Stability of Bronsted Acid Sites in Green Clinoptilolite Catalysts and Catalytic Performance in the Etherification of Glycerol N2 - Natural zeolite clinoptilolite CLIN with a framework ratio of Si/Al ≥ 4 containing mainly potassium and calcium ions in its internal channel system was used as a starting material. The acidic HCLIN catalysts were prepared under soft conditions avoiding the use of environmental less benign mineral acids. The starting material was ion exchanged using a 0.2 M aqueous ammonium nitrate solution at a temperature 80 ◦C for 2 h. The obtained NH4CLIN was converted into the acid HCLIN catalyst by calcination at 300–600 ◦C. The obtained samples were characterized by XRD, FTIR, SEM/TEM, AAS, and EDX element mapping. The state of aluminium and silicon was studied by 27Al- and 29SiMAS NMR spectroscopy. The textural properties of the catalysts were investigated by nitrogen adsorption and desorption measurements. The Brønsted acidity of the HCLIN catalysts was studied by temperature-programmed decomposition of the exchanged ammonium ions releasing ammonia as well as 1H MAS NMR, {1H–27Al} Trapdor, and {1H–27Al} Redor experiments. The strongly agglomerated samples were crystalline and thermally stable up to >500 ◦C. Although a part of the clinoptilolite framework is maintained up to 600 ◦C, a loss of crystallinity is already observed starting from 450 ◦C. The specific surface areas of the starting CLIN and ammonium exchanged NH4CLIN are low with ca. 26 m2/g. The pores are nearly blocked by the exchangeable cations located in the zeolite pores. The thermal decomposition of the ammonium ions by calcination at 400 ◦C causes an opening of the pore entrances and a markable increase in the specific micropore area and micropore volume to ca. 163 m2/g and 0.07 cm3/g, respectively. It decreases with further rising calcination temperature indicating some structural loss. The catalysts show a broad distribution of Brønsted acid sites (BS) ranging from weak to strong sites as indicated the thermal decomposition of exchanged ammonium ions (TPDA). The ammonium ion decomposition leaving BS, i.e., H+ located at Al–O–Si framework bridges, starts at ≥250 ◦C. A part of the Brønsted sites is lost after calcination specifically at 500 ◦C. It is related to the formation of penta-coordinated aluminium at the expense of tetrahedral framework aluminium. The Brønsted sites are partially recreated after repeated ammonium ion exchange. The catalytic performance of the acidic HCLIN catalysts was tested in the etherification of glycerol as a green renewable resource with different C1 -C4 alcohols. The catalysts are highly active in the etherification of glycerol, especially with alcohols containing the branched, tertiary alkyl groups. Highest activity is observed with the soft activated catalyst HCLIN300 (300 ◦C, temperature holding time: 1 min). A total of 78% conversion of glycerol to mono and di ether were achieved with tert-butanol at 140 ◦C after 4 h of reaction. The mono- and di-ether selectivity were 75% and 25%, respectively. The catalyst can be reused. KW - Etherification KW - Glycerol KW - Zeolite KW - Clinoptilolite KW - Bronsted acidity KW - Dehydroxylation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546982 DO - https://doi.org/10.3390/catal12030253 VL - 12 IS - 3 SP - 1 EP - 24 PB - MDPI AN - OPUS4-54698 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karapanagiotis, Christos A1 - Hicke, Konstantin A1 - Wosniok, Aleksander A1 - Krebber, Katerina T1 - Distributed humidity fiber-optic sensor based on BOFDA using a simple machine learning approach N2 - We report, to our knowledge for the first time, on distributed relative humidity sensing in silica polyimide-coated optical fibers using Brillouin optical frequency domain analysis (BOFDA). Linear regression, which is a simple and well-interpretable algorithm in machine learning and statistics, is utilized. The algorithm is trained using as features the Brillouin frequency shifts and linewidths of the fiber’s multipeak Brillouin spectrum. To assess and improve the effectiveness of the regression algorithm, we make use of machine learning concepts to estimate the model’s uncertainties and select the features that contribute most to the model’s performance. In addition to relative humidity, the model is also able to simultaneously provide distributed temperature information addressing the well-known cross-sensitivity effects. KW - Fiber optics sensors KW - Machine learning KW - Brillouin distributed sensing KW - Humidity sensing KW - Simultaneous temperature and humidity sensing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546294 DO - https://doi.org/10.1364/OE.453906 VL - 30 IS - 8 SP - 12484 EP - 12494 PB - OPTICA AN - OPUS4-54629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -