TY - CONF A1 - Kupsch, Andreas A1 - Schob, D. A1 - Léonard, Fabien A1 - Müller, Bernd R. A1 - Sagradov, I. A1 - Roszak, R. A1 - Sparr, H. A1 - Franke, R. A1 - Ziegenhorn, M. A1 - Bruno, Giovanni T1 - Bestimmung der Mikrostruktur und Simulation des Schädigungsverhaltens von lasergesintertem Polyamid 12 unter quasistatischer Zugbelastung N2 - Um das Material- und Schädigungsverhalten von additiv gefertigtem Polyamid 12 (PA12) unter quasistatischer Belastung zu charakterisieren, wurden mechanische Tests und Röntgenverfahren zur Bestimmung der Mikrostruktur eingesetzt. Die Proben wurden nach dem Prinzip des Selektiven Lasersinterns (SLS) hergestellt. Unter quasistatischer Belastung mit Haltezeiten ergab sich ein viskoplastisches Materialverhalten. Im Zugversuch wurde eine maximale Zugfestigkeit von 40.6 MPa und eine Bruchdehnung von 7.4% beobachtet. Mittels Röntgenrefraktion wurde eine Erhöhung von inneren Oberflächen beobachtet, die senkrecht zur Zugrichtung orientiert sind. Die Analyse der Gesamtporosität aus Computertomographie-Messungen ergab keine Änderung infolge der Zugbelastung. Jedoch wurde eine bimodale Porengrößenverteilung und eine steigende Sphärizität festgestellt. Das Materialverhalten wurde mit dem Chaboche-Modell simuliert und ergab eine sehr gute Übereinstimmung mit den experimentellen Ergebnissen. Allerdings gestattet dieses Modell nicht, das Schädigungsverhalten abzubilden. Daher wurde zur Simulation des Schädigungsverhaltens das Modell gemäß dem Ansatz von Gurson, Tvergaard und Needleman unter Berücksichtigung der mikrostrukturellen Parameter erweitert. Der Schwerpunkt des Beitrags liegt auf den Röntgenverfahren zur experimentellen Bestimmung der Mikrostruktur. T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Additive Fertigung (AM) KW - Polyamid 12 KW - Röntgenrefraktion KW - Computertomographie KW - Numerische Simulation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526833 UR - https://jahrestagung.dgzfp.de/Portals/jt2021/bb/P16.pdf SP - 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-52683 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. A1 - Camin, B. A1 - Hansen, L. A1 - Heuser, M. A1 - Lopez-Galilea, I. A1 - Ruttert, B. A1 - Theisen, W. A1 - Fedelich, Bernard T1 - Refinement and Experimental Validation of a Vacancy Model of Pore Annihilation in Single-Crystal Nickel-Base Superalloys during Hot Isostatic Pressing N2 - Initially, as-cast and homogenized single crystals of nickel-base superalloy CMSX-4 are subjected to hot isostatic pressing at 1288 °C. Two series of experiments are conducted: under the same pressure of 103 MPa but with different durations, between 0.5 and 6 h, and under different pressures, between 15 and 150 MPa, but for the same time of 0.5 h. The porosity annihilation is investigated metallographically and by high-resolution synchrotron X-ray tomography. The obtained experimental results are compared with the predictions of the vacancy model proposed recently in the group. Herein, the model is further refined by coupling with X-ray tomography. The model describes the evolution of the pore arrays enclosed in the 3D synchrotron tomograms during hot isostatic pressing and properly predicts the time and stress dependences of the pore annihilation kinetics. The validated model and the obtained experimental results are used for selecting the optimal technological parameters such as applied pressure and processing time KW - Superalloys KW - HIP KW - Single-Crystal KW - Diffusion PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526859 DO - https://doi.org/10.1002/adem.202100211 VL - 23 IS - 7 SP - 211 AN - OPUS4-52685 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Serrano Munoz, Itziar A1 - Ulbricht, Alexander A1 - Fritsch, Tobias A1 - Mishurova, Tatiana A1 - Kromm, Arne A1 - Hofmann, M. A1 - Wimpory, R. C. A1 - Evans, Alexander A1 - Bruno, Giovanni T1 - Scanning Manufacturing Parameters Determining the Residual Stress State in LPBF IN718 Small Parts N2 - The influence of scan strategy on the residual stress (RS) state of an as-built IN718 alloy produced by means of laser powder bed fusion (LPBF) is investigated. Two scan vector rotations (90°-alternation and 67°-rotation), each produced following two different scan vector lengths (long and short), are used to manufacture four rectangular prisms. Neutron diffraction (ND) and laboratory X-ray diffraction (XRD) techniques are used to map the bulk and surface RS state, respectively. The distortion induced upon removal from the baseplate is measured via profilometry. XRD measurements show that the two long scan vector strategies lead to higher RS when compared with the equivalent short scan vector strategies. Also, the 67°-rotation strategies generate lower RS than their 90°-alternation counterparts. Due to the lack of reliable stress-free d0 references, the ND results are analyzed using von Mises stress. In general, ND results show significant RS spatial non-uniformity. A comparison between ND and distortion results indicates that the RS component parallel to the building direction (Z-axis) has a predominant role in the Z-displacement. The use of a stress balance scheme allows to discuss the d0 variability along the length of the specimens, as well as examine the absolute RS state. KW - As-built LPBF IN718 alloy KW - Scan strategy influence KW - Neutron diffraction KW - Residual stress state KW - Stress balance condition KW - Distortion PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526360 DO - https://doi.org/10.1002/adem.202100158 VL - 23 IS - 7 SP - 158 PB - Wiley AN - OPUS4-52636 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kjaervik, Marit A1 - Ramstedt, M. A1 - Schwibbert, Karin A1 - Dietrich, P. M A1 - Unger, Wolfgang T1 - Comparative Study of NAP-XPS and Cryo-XPS for the Investigation of Surface Chemistry of the Bacterial Cell-Envelope N2 - Bacteria generally interact with the environment via processes involving their cell-envelope. Thus, techniques that may shed light on their surface chemistry are attractive tools for providing an understanding of bacterial interactions. One of these tools is Al Kα-excited photoelectron spectroscopy (XPS) with its estimated information depth of <10 nm. XPS-analyses of bacteria have been performed for several decades on freeze-dried specimens in order to be compatible with the vacuum in the analysis chamber of the spectrometer. A limitation of these studies has been that the freeze-drying method may collapse cell structure as well as introduce surface contaminants. However, recent developments in XPS allow for analysis of biological samples at near ambient pressure (NAP-XPS) or as frozen hydrated specimens (cryo-XPS) in vacuum. In this work, we have analyzed bacterial samples from a reference strain of the Gram-negative bacterium Pseudomonas fluorescens using both techniques. We compare the results obtained and, in general, observe good agreement between the two techniques. Furthermore, we discuss advantages and disadvantages with the two analysis approaches and the output data they provide. XPS reference data from the bacterial strain are provided, and we propose that planktonic cells of this strain (DSM 50090) are used as a reference material for surface chemical analysis of bacterial systems. KW - P. Fluorescens KW - Cryo XPS KW - NAP-XPS KW - DSM 5009 PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525640 DO - https://doi.org/10.3389/fchem.2021.666161 VL - 9 SP - Article 666161 PB - Frontiers CY - Switzerland AN - OPUS4-52564 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Feiler, Torvid A1 - Bhattacharya, Biswajit A1 - Michalchuk, Adam A1 - Rhim, S.-Y. A1 - Schöder, V. A1 - List-Kratochvil, E. A1 - Emmerling, Franziska T1 - Tuning the mechanical flexibility of organic molecular crystals by polymorphism for flexible optical waveguides N2 - The ability to selectively tune the optical and the mechanical properties of organic molecular crystals offers a promising approach towards developing flexible optical devices. These functional properties are sensitive to crystallographic packing features and are hence expected to vary with polymorphic modification. Using as a model system the photoluminescent material 4-bromo-6-[(6-chloropyridin-2-ylimino)methyl]phenol (CPMBP), we herein demonstrate the simultaneous tuning of mechanical flexibility and photoluminescence properties via polymorphism. Two new polymorphic forms of CPMBP were obtained from a solution and fully characterised using a combination of experiments and density functional theory simulations. These polymorphic forms exhibit remarkably distinct mechanical properties and an order of magnitude difference in photoluminescence quantum yield. The mechanically plastic form has a higher quantum yield than the brittle polymorphic form. However, their photoluminescence emission profile is largely unaffected by the observed polymorphism, thereby demonstrating that the optical properties and bulk mechanical properties can in principle be tuned independently. By distinguishing between active (involving absorption and emission) and passive (involving no absorption) light propagation, the waveguiding properties of the plastic form of CPMBP (form II) were explored using the straight and bent crystals to highlight the potential applications of CPMBP in designing flexible optical devices. Our results demonstrated that polymorph engineering would be a promising avenue to achieve concurrent modulation of the optical and mechanical properties of photoluminescent molecular crystals for next-generation flexible optical device applications. KW - Mechanochemistry KW - Flexible PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532075 DO - https://doi.org/10.1039/d1ce00642h VL - 23 IS - 34 SP - 5815 EP - 5825 PB - Royal Society of Chemistry CY - London AN - OPUS4-53207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quiroz, J. A1 - de Oliveira, P. F. M. A1 - Shetty, S. A1 - Oropeza, F. A1 - Peña O’Shea, V. A1 - Rodrigues, L. A1 - Rodrigues, M. A1 - Torresi, R. A1 - Emmerling, Franziska A1 - Camargo, P. T1 - Bringing earth-abundant plasmonic catalysis to light: Gram-scale mechanochemical synthesis and tuning of activity by dual excitation of antenna and reactor sites N2 - The localized surface plasmon resonance (LSPR) excitation in plasmonic nanoparticles (NPs) in the visible and near-infrared ranges is currently at the forefront of improving photocatalytic performances via plasmonic photocatalysis. One bottleneck of this field is that the NPs that often display the best optical properties in the visible and near-infrared ranges are based on expensive noble metals such as silver (Ag) and gold (Au). While earth-abundant plasmonic materials have been proposed together with catalytic metals in antenna–reactor systems, their performances remain limited by their optical properties. Importantly, the synthesis of plasmonic photocatalysts remains challenging in terms of scalability while often requiring several steps, high temperatures, and special conditions. Herein, we address these challenges by developing a one-pot, gram-scale, room-temperature synthesis of earth-abundant plasmonic photocatalysts while improving their activities beyond what has been dictated by the LSPR excitation of the plasmonic component. We describe the mechanochemical synthesis of earth-abundant plasmonic photocatalysts by using MoO3 (antenna) and Au (reactor) NPs as a proof-of-concept example and demonstrate that the dual plasmonic excitation of antenna and reactor sites enables the tuning of plasmonic photocatalytic performances toward the reductive coupling of nitrobenzene to azobenzene as a model reaction. In addition to providing a pathway to the facile and gram-scale synthesis of plasmonic photocatalysts, the results reported herein may open pathways to improved activities in plasmonic catalysis. KW - MoO3 KW - Au nanoparticles KW - Localized surface plasmon resonance KW - Plasmonic photocatalysis KW - Nitrobenzene reduction PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532089 DO - https://doi.org/10.1021/acssuschemeng.1c02063 VL - 9 IS - 29 SP - 9750 EP - 9760 PB - American Chemical Society CY - Washington, DC AN - OPUS4-53208 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schoknecht, Ute A1 - Mathies, Helena A1 - Lisec, Jan T1 - Leaching and transformation of film preservatives in paints induced by combined exposure to ultraviolet radiation and water contact under controlled laboratory conditions N2 - Stormwater from urban areas can transport biocidally active substances and related transformation products from buildings into the environment. The occurrence of these substances in urban runoff depends on the availability of water, and on ultraviolet radiation exposure that causes photolytic reactions. In a systematic laboratory study, painted test specimens were exposed to either ultraviolet radiation, water contact, or a combination of both. Leaching of the biocidally active substances carbendazim, diuron, octylisothiazolinone, terbutryn, and selected transformation products of terbutryn and diuron were observed under various exposure conditions. Remaining concentrations of these substances in the paint were quantified. It was demonstrated that the distribution of active substances and transformation products in eluates and in the coatings themselves differs with exposure conditions. Strategies for environmental monitoring of biocide emissions need to consider the most relevant transformation products. However, environmental concentrations of biocidally active substances and transformation products depend on earlier exposure conditions. As a consequence, monitoring data cannot describe emission processes and predict expected leaching of biocidally active substances from buildings if the data are collected only occasionally. KW - Substance release KW - Construction products KW - Biocides KW - Transformation KW - UV radiation KW - Water contact PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532114 DO - https://doi.org/10.3390/w13172390 SN - 2073-4441 VL - 13 IS - 17 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-53211 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 - Numerical analysis of the partial penetration high power laser beam welding of thick sheets at high process speeds N2 - The present work is devoted to the numerical analysis of the high-power laser beam welding of thick sheets at different welding speeds. A three-dimensional transient multi-physics numerical model is developed, allowing for the prediction of the keyhole geometry and the final penetration depth. Two ray tracing algorithms are implemented and compared, namely a standard ray tracing approach and an approach using a virtual mesh refinement for a more accurate calculation of the reflection points. Both algorithms are found to provide sufficient accuracy for the prediction of the keyhole depth during laser beam welding with process speeds of up to 1.5 m/min. However, with the standard algorithm, the penetration depth is underestimated by the model for a process speed of 2.5 m/min due to a trapping effect of the laser energy in the top region. In contrast, the virtually refined ray tracing approach results in high accuracy results for process speeds of both 1.5 m/min and 2.5 m/min. A detailed study on the trapping effect is provided, accompanied by a benchmark including a predefined keyhole geometry with typical characteristics for the high-power laser beam welding of thick plates at high process speed, such as deep keyhole, inclined front keyhole wall, and a hump. KW - High-power laser beam welding KW - High process speeds KW - Deep penetration KW - Numerical modeling KW - Ray tracing PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532170 DO - https://doi.org/10.3390/met11081319 SN - 2075-4701 VL - 11 IS - 8 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-53217 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Munir, R. A1 - Lisec, Jan A1 - Jaeger, Carsten A1 - Zaidi, N. T1 - Abundance, fatty acid composition and saturation index of neutral lipids in colorectal cancer cell lines N2 - Lipid droplets, the dynamic organelles that store Triglycerides (TG) and cholesterol esters (CE), are highly accumulated in colon cancer cells. This work studies the TG and CE subspecies profile in colon carcinoma cell lines, SW480 derived from primary tumor, and SW620 derived from a metastasis of the same tumor. It was previously reported that the total TG and CE content is dramatically higher in SW620 cells; however, TG and CE subspecies profile has not been investigated in detail. The work presented here confirms that the total TG and CE Content is significantly higher in the SW620 cells. Moreover, the fatty acid (FA) composition of TG is significantly altered in the SW620 cells, with significant decrease in the abundance of saturated triglycerides. This resulted in a significantly decreased TG saturation index in the SW620 cells. The saturation index of CE was also significantly decreased in the SW620 cells. KW - Mass Spectroscopy KW - Metabolomics KW - Cancer PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533504 DO - https://doi.org/10.18388/abp.2020_5465 VL - 68 IS - 1 SP - 1 EP - 4 PB - ABP Acta Biochimica Polonica AN - OPUS4-53350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lisec, Jan A1 - Kobelt, D. A1 - Walther, W. A1 - Mokrizkij, M. A1 - Grötzinger, C. A1 - Jaeger, Carsten A1 - Baum, K. A1 - Simon, M. A1 - Wolf, J. A1 - Beindorf, N. A1 - Brenner, W. A1 - Stein, U. T1 - Systematic Identification of MACC1-Driven Metabolic Networks in Colorectal Cancer N2 - MACC1 is a prognostic and predictive metastasis biomarker for more than 20 solid Cancer entities. However, its role in cancer metabolism is not sufficiently explored. Here, we report on how MACC1 impacts the use of glucose, glutamine, lactate, pyruvate and fatty acids and show the comprehensive analysis of MACC1-driven metabolic networks. We analyzed concentrationdependent changes in nutrient use, nutrient depletion, metabolic tracing employing 13C-labeled substrates, and in vivo studies. We found that MACC1 permits numerous effects on cancer metabolism. Most of those effects increased nutrient uptake. Furthermore, MACC1 alters metabolic pathways by affecting metabolite production or turnover from metabolic substrates. MACC1 supports use of glucose, glutamine and pyruvate via their increased depletion or altered distribution within metabolic pathways. In summary, we demonstrate that MACC1 is an important regulator of metabolism in cancer cells. KW - Mass Spectroscopy KW - Metabolomics KW - Cancer PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533526 DO - https://doi.org/10.3390/cancers13050978 VL - 13 IS - 5 SP - 1 EP - 22 PB - MDPI Journal Cancers AN - OPUS4-53352 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adamus, A. A1 - Ali, I. A1 - Vasileiadis, V. A1 - Al-Hileh, L. A1 - Lisec, Jan A1 - Frank, M. A1 - Seitz, G. A1 - Engel, N. T1 - Vincetoxicum arnottianum modulates motility features and metastatic marker expression in pediatric rhabdomyosarcoma by stabilizing the actin cytoskeleton N2 - Background: Prevention of metastatic invasion is one of the main challenges in the treatment of alveolar rhabdomyosarcoma. Still the therapeutic options are limited. Therefore, an anti-tumor screening was initiated focusing on the anti-metastatic and anti-invasion properties of selected medicinal plant extracts and phytoestrogens, already known to be effective in the prevention and treatment of different cancer entities. Methods: Treatment effects were first evaluated by cell viability, migration, invasion, and colony forming assays on the alveolar rhabdomyosarcoma cell line RH-30 in comparison with healthy primary cells. Results: Initial anti-tumor screenings of all substances analyzed in this study, identified the plant extract of Vincetoxicum arnottianum (VSM) as the most promising candidate, harboring the highest anti-metastatic potential. Those significant anti-motility properties were proven by a reduced ability for migration (60%), invasion (99%) and colony formation (61%) under 48 h exposure to 25 μg/ml VSM. The restricted motility features were due to an induction of the stabilization of the cytoskeleton – actin fibers were 2.5-fold longer and were spanning the entire cell. Decreased proliferation (PCNA, AMT, GCSH) and altered metastasis (e. g. SGPL1, CXCR4, stathmin) marker expression on transcript and protein level confirmed the significant lowered tumorigenicity under VSM treatment. Finally, significant alterations in the cell metabolism were detected for 25 metabolites, with levels of uracil, N-acetyl serine and propanoyl phosphate harboring the greatest alterations. Compared to the conventional therapy with cisplatin, VSM treated cells demonstrated a similar metabolic shutdown of the primary cell metabolism. Primary control cells were not affected by the VSM treatment. Conclusions: This study revealed the VSM root extract as a potential, new migrastatic drug candidate for the putative treatment of pediatric alveolar rhabdomyosarcoma with actin filament stabilizing properties and accompanied by a marginal effect on the vitality of primary cells. KW - Mass Spectroscopy KW - Metabolomics KW - Cancer PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533530 DO - https://doi.org/10.1186/s12906-021-03299-x VL - 21 IS - 1 PB - Springer Nature AN - OPUS4-53353 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geißler, Daniel A1 - Nirmalananthan-Budau, Nithiya A1 - Scholtz, Lena A1 - Tavernaro, Isabella A1 - Resch-Genger, Ute T1 - Analyzing the surface of functional nanomaterials — how to quantify the total and derivatizable number of functional groups and ligands N2 - Functional nanomaterials (NM) of different size, shape, chemical composition, and surface chemistry are of increasing relevance for many key technologies of the twenty-first century. This includes polymer and silica or silica-coated nanoparticles (NP) with covalently bound surface groups, semiconductor quantum dots (QD), metal and metal oxide NP, and lanthanide-based NP with coordinatively or electrostatically bound ligands, as well as surface-coated nanostructures like micellar encapsulated NP. The surface chemistry can significantly affect the physicochemical properties of NM, their charge, their processability and performance, as well as their impact on human health and the environment. Thus, analytical methods for the characterization of NM surface chemistry regarding chemical identification, quantification, and accessibility of functional groups (FG) and surface ligands bearing such FG are of increasing importance for quality control of NM synthesis up to nanosafety. Here, we provide an overview of analytical methods for FG analysis and quantification with special emphasis on bioanalytically relevant FG broadly utilized for the covalent attachment of biomolecules like proteins, peptides, and oligonucleotides and address methodand material-related challenges and limitations. Analytical techniques reviewed include electrochemical titration methods, optical assays, nuclear magnetic resonance and vibrational spectroscopy, as well as X-ray based and thermal analysis methods, covering the last 5–10 years. Criteria for method classification and evaluation include the need for a signal-generating label, provision of either the total or derivatizable number of FG, need for expensive instrumentation, and suitability for process and production control during NM synthesis and functionalization. KW - Functional group quantification KW - Surface ligand KW - Nanomaterial KW - Optical detection KW - Electrochemical titration KW - Nanosafety (Safe-by-design) PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533597 DO - https://doi.org/10.1007/s00604-021-04960-5 VL - 188 IS - 10 SP - 1 EP - 28 PB - Springer Nature AN - OPUS4-53359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klewe, Tim A1 - Strangfeld, Christoph A1 - Ritzer, Tobias A1 - Kruschwitz, Sabine T1 - Combining Signal Features of Ground-Penetrating Radar to Classify Moisture Damage in Layered Building Floors N2 - To date, the destructive extraction and analysis of drilling cores is the main possibility to obtain depth information about damaging water ingress in building floors. The time- and costintensive procedure constitutes an additional burden for building insurances that already list piped water damage as their largest item. With its high sensitivity for water, a ground-penetrating radar (GPR) could provide important support to approach this problem in a non-destructive way. In this research, we study the influence of moisture damage on GPR signals at different floor constructions. For this purpose, a modular specimen with interchangeable layers is developed to vary the screed and insulation material, as well as the respective layer thickness. The obtained data set is then used to investigate suitable signal features to classify three scenarios: dry, damaged insulation, and damaged screed. It was found that analyzing statistical distributions of A-scan features inside one B-scan allows for accurate classification on unknown floor constructions. Combining the features with multivariate data analysis and machine learning was the key to achieve satisfying results. The developed method provides a basis for upcoming validations on real damage cases. KW - Radar KW - Material Moisture KW - Non-destructive testing KW - Signal Features KW - Civil Engineering KW - Machine Learning PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533606 DO - https://doi.org/10.3390/app11198820 VL - 11 IS - 19 SP - 8820 PB - MDPI AN - OPUS4-53360 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Seher, Julia A1 - Fröba, M. T1 - Shape matters: The effect of particle morphology on the fast-charging performance of LiFePO4/C nanoparticle composite electrodes N2 - For the successful use of lithium-ion batteries in automotive applications, reliable availability of high storage capacity and very short recharging times are essential. In order to develop the perfect battery for a certain application, structure–property relationships of each active material must be fully understood. LiFePO4 is of great interest due to its fast-charging capability and high stability regarding its thermal resistance and chemical reactivity. The anisotropic lithium-ion diffusion through the LiFePO4 crystal structure indicates a strong dependence of the electrochemical performance of a nanostructured active material on particle morphology. In this paper, the relationship of the particle morphology and fast-charging capability of LiFePO4/C core/shell nanoparticles in half-cells was studied. For this purpose, a new multistep synthesis strategy was developed. It involves the combination of a solvothermal synthesis followed by an in situ polymer coating and thermal calcination step. Monodisperse rodlike LiFePO4 nanoparticles with comparable elongation along the b-axis (30–50 nm) and a varying aspect ratio c/a (2.4–6.9) were obtained. A strong correlation of the fast-charging capability with the aspect ratio c/a was observed. When using LiFePO4 nanoparticles with the smallest aspect ratio c/a, the best electrochemical performance was received regarding the specific capacity at high C-rates and the cycling stability. A reduction of the aspect ratio c/a by 30% (3.6 to 2.4) was found to enhance the charge capacity at 10 C up to an order of magnitude (7.4–73 mA h·g–1). KW - LiFePO4 KW - Schnellladung KW - Nanoparticles KW - Carbon KW - Chemical synthesis KW - Electrochemical cells KW - Materials PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533004 DO - https://doi.org/10.1021/acsomega.1c03432 SN - 2470-1343 VL - 6 IS - 37 SP - 24062 EP - 24069 PB - American Chemical Society CY - Washington, DC AN - OPUS4-53300 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröpfer, Dirk A1 - Scharf-Wildenhain, R. A1 - Hälsig, A. A1 - Wandtke, Karsten A1 - Kromm, Arne A1 - Kannengießer, Thomas T1 - Process-related influences and correlations in wire arc additive manufacturing of high-strength steels N2 - High-strength fine-grained structural steels have great potential for weight-optimized, efficient structures in many modern steel applications. Further advances in efficiency can be achieved through additive manufacturing and bionic design. Commercial high-strength filler materials for wire arc additive manufacturing (WAAM) are already provided by the consumable producers. Today, application would be strictly limited due to absence of quantitative findings or any guidelines for the industry regarding welding-related stresses and component safety during manufacturing and service. Hence, process- and material-related influences and design-related restraint conditions associated with formation of residual stresses and cold cracking risk are investigated. The aim is the accessibility of special WAAM self-restraining cold cracking tests and easy applicable processing recommendations, enabling an economical, fit-for-purpose and crack-safe WAAM of high-strength steels. This first study focuses on determination of interactions between WAAM process parameters, resulting layer geometry, microstructure and residual stresses, analyzed via X-ray diffraction. Defined reference specimens are automated welded using a special WAAM solid wire (yield strength >820 MPa). Geometric properties can be specifically adjusted by wire feed and welding speed, but cannot be varied arbitrarily, since a high heat input causes local overheating, inadmissible changes of microstructure and mechanical properties, defects and comparable high tensile residual stresses. T2 - 22. Werkstofftechnischen Kolloquium der TU Chemnitz CY - Online meeting DA - 24.03.2021 KW - Residual stresses KW - Additive Manufacturing KW - High-strength steel PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533300 DO - https://doi.org/10.1088/1757-899X/1147/1/012002 VL - 1147 SP - 012002 PB - IOP Publishing Ltd AN - OPUS4-53330 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wittmar, J. A1 - Ohle, Corina A1 - Kunte, Hans-Jörg A1 - Brand, I. T1 - Effect of Ectoine on the Conformation and Hybridization of dsDNA in Monolayer Films: A Spectroelectrochemical Study N2 - Lack of long-time stability of dsDNA-based supramolecular assemblies is an important issue that hinders their applications. In this work, 20 base pairs long dsDNA fragments [(dCdG)20 65%] composed of 65% dCdG and 35% dAdT nucleotides were tethered via a thiol to the surface of a gold electrode. The selfassembled (dCdG)20 -65% monolayer was immersed in solutions containing ectoine, a compatible solute. Electrochemical results showed that these monolayers were stable for one month. In situ IR spectroscopy indicated that ectoine interacts weakly with the phosphate-ribose backbone, dehydrating the phosphate groups and stabilizing the A-DNA conformation. This structural reorganization led to a reorientation of nucleic acid base pairs and a local disruption of the double-helix structure. However, the conformation and orientation of the dsDNA fragment was stable in the KW - Ectoine KW - dsDAN monolayer KW - A-DNA conformation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533346 DO - https://doi.org/10.1002/celc.202100816 SN - 2196-0216 VL - 8 IS - 20 SP - 3844 EP - 3854 PB - Wiley-VCH GmbH AN - OPUS4-53334 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friedrich, Sebastian A1 - Cappella, Brunero T1 - Friction and mechanical properties of AFM-scan-induced ripples in polymer films N2 - In the present paper, friction and mechanical properties of AFM-Scan-Induced ripple structures on films of polystyrene and poly-n-(butyl methacrylate) are investigated. Force volume measurements allow a quantitative analysis of the elastic moduli with nanometer resolution, showing a contrast in mechanical response between bundles and troughs. Additionally, analysis of the lateral cantilever deflection shows a clear correlation between friction and the sample topography. Those results support the theory of crack propagation and the formation of voids as a mechanism responsible for the formation of ripples. This paper also shows the limits of the presented measuring methods for soft, compliant, and small structures. KW - AFM KW - Polymer KW - Ripples KW - Mechanical properties KW - Friction PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532772 DO - https://doi.org/10.3389/fmech.2021.672898 SN - 2297-3079 VL - 7 SP - 1 EP - 8 PB - Frontiers Media CY - Lausanne AN - OPUS4-53277 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Serrano Munoz, Itziar A1 - Evans, Alexander A1 - Mishurova, Tatiana A1 - Sprengel, Maximilian A1 - Pirling, T. A1 - Kromm, Arne A1 - Bruno, Giovanni T1 - The importance of subsurface residual stress in laser powder bed fusion IN718 N2 - The residual stress (RS) in laser powder bed fusion (LPBF) IN718 alloy samples produced using a 67°-rotation scan strategy is investigated via laboratory X-ray diffraction (XRD) and neutron diffraction (ND). The location dependence of the strain-free (d₀) lattice spacing in ND is evaluated using a grid array of coupons extracted from the far-edge of the investigated specimen. No compositional spatial variation is observed in the grid array. The calculated RS fields show considerable non-uniformity, significant stress gradients in the region from 0.6 to 2 mm below the surface, as well as subsurface maxima that cannot be accounted for via XRD. It is concluded that failure to determine such maxima would hamper a quantitative determination of RS fields by means of the stress balance method. KW - Laser powder bed fusion KW - Neutron and X-ray diffraction KW - Residual stress analysis KW - Strain-free lattice references KW - Stress balance PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532707 DO - https://doi.org/10.1002/adem.202100895 SN - 1615-7508 SN - 1527-2648 VL - 24 IS - 6 SP - 1 EP - 7 PB - Wiley-VCH CY - Weinheim AN - OPUS4-53270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hobmeier, K. A1 - Cantone, M. A1 - Nguyen, Q. A. A1 - Pflüger-Grau, K. A1 - Kremling, A. A1 - Kunte, Hans-Jörg A1 - Pfeiffer, F. A1 - Marin-Sanguino, A. T1 - Adaptation to varying salinity in Halomonas elongata: Much more than ectoine accumulation N2 - The halophilic γ-proteobacterium Halomonas elongata DSM 2581T thrives at salt concentrations well above 10 % NaCl (1.7 M NaCl). A well-known osmoregulatory mechanism is the accumulation of the compatible solute ectoine within the cell in response to osmotic stress. While ectoine accumulation is central to osmoregulation and promotes resistance to high salinity in halophilic bacteria, ectoine has this effect only to a much lesser extent in non-halophiles. We carried out transcriptome analysis of H. elongata grown on two different carbon sources (acetate or glucose), and low (0.17 M NaCl), medium (1 M), and high salinity (2 M) to identify additional mechanisms for adaptation to high saline environments. To avoid a methodological bias, the transcripts were evaluated by applying two methods, DESeq2 and Transcripts Per Million (TPM). The differentially transcribed genes in response to the available carbon sources and salt stress were then compared to the transcriptome profile of Chromohalobacter salexigens, a closely related moderate halophilic bacterium. Transcriptome profiling supports the notion that glucose is degraded via the cytoplasmic Entner-Doudoroff pathway, whereas the Embden-Meyerhoff-Parnas pathway is employed for gluconeogenesis. The machinery of oxidative phosphorylation in H. elongata and C. salexigens differs greatly from that of non-halophilic organisms, and electron flow can occur from quinone to oxygen along four alternative routes. Two of these pathways via cytochrome bo' and cytochrome bd quinol oxidases seem to be upregulated in salt stressed cells. Among the most highly regulated genes in H. elongata and C. salexigens are those encoding chemotaxis and motility proteins, with genes for chemotaxis and flagellar assembly severely downregulated at low salt concentrations. We also compared transcripts at low and high-salt stress (low growth rate) with transcripts at optimal salt concentration and found that the majority of regulated genes were down-regulated in stressed cells, including many genes involved in carbohydrate metabolism, while ribosome synthesis was up-regulated, which is in contrast to what is known from non-halophiles at slow growth. Finally, comparing the acidity of the cytoplasmic proteomes of non-halophiles, extreme halophiles and moderate halophiles suggests adaptation to an increased cytoplasmic ion concentration of H. elongata. Taken together, these results lead us to propose a model for salt tolerance in H. elongata where ion accumulation plays a greater role in salt tolerance than previously assumed. KW - Ectoine KW - Osmoadaptation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545608 DO - https://doi.org/10.3389/fmicb.2022.846677 SN - 1664-302X VL - 13 SP - 1 EP - 19 PB - Frontiers Media CY - Lausanne AN - OPUS4-54560 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mueller, I. A1 - Memmolo, V. A1 - Tschöke, K. A1 - Moix-Bonet, M. A1 - Möllenhoff, K. A1 - Golub, M. A1 - Sridaran Venkat, R. A1 - Lugovtsova, Yevgeniya A1 - Eremin, A. A1 - Moll, J. T1 - Performance Assessment for a Guided Wave-Based SHM System Applied to a Stiffened Composite Structure N2 - To assess the ability of structural health monitoring (SHM) systems, a variety of prerequisites and contributing factors have to be taken into account. Within this publication, this variety is analyzed for actively introduced guided wave-based SHM systems. For these systems, it is not possible to analyze their performance without taking into account their structure and their applied system parameters. Therefore, interdependencies of performance assessment are displayed in an SHM pyramid based on the structure and its monitoring requirements. Factors influencing the quality, capability and reliability of the monitoring system are given and put into relation with state-of-the-art performance analysis in a non-destructive evaluation. While some aspects are similar and can be treated in similar ways, others, such as location, environmental condition and structural dependency, demand novel solutions. Using an open-access data set from the Open Guided Waves platform, a detailed method description and analysis of path-based performance assessment is presented.The adopted approach clearly begs the question about the decision framework, as the threshold affects the reliability of the system. In addition, the findings show the effect of the propagation path according to the damage position. Indeed, the distance of damage directly affects the system performance. Otherwise, the propagation direction does not alter the potentiality of the detection approach despite the anisotropy of composites. Nonetheless, the finite waveguide makes it necessary to look at the whole paths, as singular phenomena associated with the reflections may appear. Numerical investigation helps to clarify the centrality of wave mechanics and the necessity to take sensor position into account as an influencing factor. Starting from the findings achieved, all the issues are discussed, and potential future steps are outlined. KW - Reliability assessment KW - Ultrasonic Guided Waves KW - Structural Health Monitoring KW - Probability of detection KW - Path-based analysis PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-558853 DO - https://doi.org/10.3390/s22197529 VL - 22 IS - 19 SP - 1 EP - 28 PB - MDPI CY - Basel, Switzerland AN - OPUS4-55885 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 - Kinetics KW - In situ PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-558878 DO - https://doi.org/10.1039/d2fd00115b SP - 1 EP - 16 PB - Royal Society of Chemistry AN - OPUS4-55887 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heuser, Lina A1 - Nofz, Marianne A1 - Müller, Ralf A1 - Deubener, J. T1 - Silver dissolution and precipitation in an Na2O–ZnO–B2O3 metallization paste glass N2 - Thermally stimulated interactions between silver and glass, that is, silver dissolution as Ag+ and precipitation as Ag0 were studied in two glass series of molar target composition xAg2O–(19 − x)Na2O–28ZnO–53B2O3 with x = 0, 0.1, 0.5, 5 and (19Na2O–28ZnO–53B2O3)+yAg2O with y = 0.01, 0.05. These act as model for low-melting borate glasses being part of metallization pastes. The occurrence of metallic silver precipitates in melt-quenched glass ingots demonstrated that silver dissolved only in traces (< 0.01 mol%) in the glasses. The dissolved silver was detected by means of Raman spectroscopy and energy-dispersive X-ray spectroscopy. Increasing x in the batch could not lead to a significant increase of the silver ion fraction in the glass as possible in binary silver borate glasses. In situ observation of heated AgNO3 mixed with the base glass frit in a hot stage microscope showed that Ag0 precipitation occurs already at the solid state. At higher temperatures, small droplets of liquid silver were found to move freely within the melt, whereas coalescence caused a stepwise increase of their size. These results contribute to the understanding of formation of silver precipitates in metallization pastes described in the literature. KW - Silver metallization paste KW - Batch reactions KW - Borate KW - Glass forming melts KW - Glass manufacturing KW - Raman spectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559433 DO - https://doi.org/10.1111/ijag.16613 SN - 2041-1286 SP - 1 EP - 11 PB - Wiley Online Library AN - OPUS4-55943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klimek, André A1 - Stelzner, Ludwig A1 - Hothan, Sascha A1 - Rogge, Andreas T1 - Fire induced concrete spalling in combination with size effects N2 - The size effect has its origin in fracture mechanics and describes the formation as well as propagation of cracks in brittle and solid materials in dependence of the specimen size. However, the size effect in concrete spalling describes the damage behaviour on a macroscopic scale for different sized specimens in case of fire. Concrete spalling is a very complex and yet not fully understood phenomenon. To reduce the effort of fire tests to analyse the spalling behaviour of concrete mixtures, this study investigates the susceptibility to spalling for six different concrete mixtures and three specimen sizes. The sizes were divided in full scale slabs (1.8 m x 1.2 m x 0.3 m), intermediate scale cuboids (0.6 m x 0.6 m x 0.3 m) and small scale cylinders (Ø0.15 m x 0.3 m). For this purpose, a novel test set-up was built to test six intermediate scale or twelve small scale specimens simultaneously to ensure a similar heating regime for every specimen. All specimens were fire exposed on one side and remained unrestrained. A size effect occurred for four of the six concrete mixtures. Compared to the full scale specimens the spalling was reduced significantly for all smaller specimen sizes. Additionally, spalling did not occur for the small scale specimens. The results show that the specimen size is an essential parameter to investigate the susceptibility to spalling of a concrete mixture. For future investigations the testing conditions must be adjusted for the intermediate scale specimens to recreate the conditions of the slabs. KW - Concrete KW - Spalling KW - Size effect KW - Fire test PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559231 DO - https://doi.org/10.1617/s11527-022-02051-2 VL - 55 IS - 8 SP - 1 EP - 14 PB - Springer AN - OPUS4-55923 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Drexler, A A1 - Konert, Florian A1 - Sobol, Oded A1 - Rhode, Michael A1 - Domitner, J A1 - Sommitsch, C A1 - Boellinghaus, Thomas T1 - Enhanced gaseous hydrogen solubility in ferritic and martensitic steels at low temperatures N2 - Metals that are exposed to high pressure hydrogen gas may undergo detrimental failure by embrittlement. Understanding the mechanisms and driving forces of hydrogen absorption on the surface of metals is crucial for avoiding hydrogen embrittlement. In this study, the effect of stress-enhanced gaseous hydrogen uptake in bulk metals is investigated in detail. For that purpose, a generalized form of Sievert's law is derived from thermodynamic potentials considering the effect of microstructural trapping sites and multiaxial stresses. This new equation is parametrized and verified using experimental data for carbon steels, which were charged under gaseous hydrogen atmosphere at pressures up to 1000 bar. The role of microstructural trapping sites on the parameter identification is critically discussed. KW - Hydrogen KW - Thermodynamic modelling KW - Pressure-dependent solubility KW - Steel KW - Trapping PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559307 DO - https://doi.org/10.1016/j.ijhydene.2022.09.109 SN - 0360-3199 VL - 47 IS - 93 SP - 39639 EP - 39653 PB - Elsevier Ltd. AN - OPUS4-55930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Michalchuk, Adam T1 - The Mechanochemical Excitation of Crystalline LiN3 N2 - Mechanochemical reactions are driven by the direct absorption of mechanical energy by a solid (often crystalline) material. Understanding how this energy is absorbed and ultimately causes a chemical transformation is essential for understanding the elementary stages of mechanochemical transformations. Using as a model system the energetic material LiN3 we here consider how vibrational energy flows through the crystal structure. By considering the compression response of the crystalline material we identify the partitioning of energy into an initial vibrational excitation. Subsequent energy flow is based on concepts of phonon–phonon scattering, which we calculate within a quasi-equilibrium model facilitated by phonon scattering data obtained from Density Functional Theory (DFT). Using this model we demonstrate how the moments (picoseconds) immediately following mechanical impact lead to significant thermal excitation of crystalline LiN3, sufficient to drive marked changes in its electronic structure and hence chemical reactivity. This work paves the way towards an ab initio approach to studying elementary processes in mechanochemical reactions involving crystalline solids. KW - Energetic materials KW - Ab initio simulation KW - DFT KW - Mechanochemistry PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559310 DO - https://doi.org/10.1039/d2fd00112h SP - 1 EP - 20 PB - Royal Society of Chemistry AN - OPUS4-55931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Schmid, Thomas T1 - Raman focal point on Roman Egyptian blue elucidates disordered cuprorivaite, green glass phase and trace compounds N2 - The discussed comparative analyses of Roman Imperial pigment balls and fragmentary murals unearthed in the ancient cities of Aventicum and Augusta Raurica (Switzerland) by means of Raman microspectroscopy pertain to a predecessor study on trace compounds in Early Medieval Egyptian blue (St. Peter, Gratsch, South Tyrol, Northern Italy). The plethora of newly detected associated minerals of the raw materials surviving the synthesis procedure validate the use of quartz sand matching the composition of sediments transported by the Volturno river into the Gulf of Gaeta (Campania, Southern Italy) with a roasted sulphidic copper ore and a mixed-alkaline plant ash as fluxing agent. Thus, the results corroborate a monopolised pigment production site located in the northern Phlegrean Fields persisting over the first centuries A.D., this in line with statements of the antique Roman writers Vitruvius and Pliny the Elder and recent archaeological evidences. Beyond that, Raman spectra reveal through gradual peak shifts and changes of band width locally divergent process conditions and compositional inhomogeneities provoking crystal lattice disorder in the chromophoric cuprorivaite as well as the formation of a copper-bearing green glass phase, the latter probably in dependency of the concentration of alkali flux, notwithstanding that otherwise solid-state reactions predominate the synthesis. KW - Raman microspectroscopy KW - Egyptian blue KW - Cuprorivaite PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559028 DO - https://doi.org/10.1038/s41598-022-19923-w SN - 2045-2322 VL - 12 IS - 1 SP - 1 EP - 12 PB - Nature Publishing Group CY - London AN - OPUS4-55902 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sechi, R. A1 - Fackeldey, K. A1 - Chewle, Surahit A1 - Weber, M. T1 - SepFree NMF: A toolbox for analyzing the kinetics of sequential spectroscopic data N2 - This work addresses the problem of determining the number of components from sequential spectroscopic data analyzed by non-negative matrix factorization without separability assumption (SepFree NMF). These data are stored in a matrix M of dimension “measured times” versus “measured wavenumbers” and can be decomposed to obtain the spectral fingerprints of the states and their evolution over time. SepFree NMF assumes a memoryless (Markovian) process to underline the dynamics and decomposes M so that M = WH, with W representing the components’ fingerprints and H their kinetics. However, the rank of this decomposition (i.e., the number of physical states in the process) has to be guessed from pre-existing knowledge on the observed process. We propose a measure for determining the number of components with the computation of the minimal memory effect resulting from the decomposition; by quantifying how much the obtained factorization is deviating from the Markovian property, we are able to score factorizations of a different number of components. In this way, we estimate the number of different entities which contribute to the observed system, and we can extract kinetic information without knowing the characteristic spectra of the single components. This manuscript provides the mathematical background as well as an analysis of computer generated and experimental sequentially measured Raman spectra. KW - Kinetics from experiments KW - Separability assumption KW - Sequential spectroscopic data PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559046 DO - https://doi.org/10.3390/a15090297 SN - 1999-4893 VL - 15 IS - 9 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-55904 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fackeldey, K. A1 - Röhm, J. A1 - Niknejad, A. A1 - Chewle, Surahit A1 - Weber, M. T1 - Analyzing Raman spectral data without separabiliy assumption N2 - Raman spectroscopy is a well established tool for the analysis of vibration spectra, which then allow for the determination of individual substances in a chemical sample, or for their phase transitions. In the time-resolved-Raman-sprectroscopy the vibration spectra of a chemical sample are recorded sequentially over a time interval, such that conclusions for intermediate products (transients) can be drawn within a chemical process. The observed data-matrix M from a Raman spectroscopy can be regarded as a matrix product of two unknown matrices W and H, where the first is representing the contribution of the spectra and the latter represents the chemical spectra. One approach for obtaining W and H is the non-negative matrix factorization. We propose a novel approach, which does not need the commonly used separability assumption. The performance of this approach is shown on a real world chemical example. KW - Non-negative matrix factorization KW - NMF KW - Raman spectra KW - Separability condition KW - PCCA+ PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559051 DO - https://doi.org/10.1007/s10910-020-01201-7 SN - 1572-8897 VL - 59 SP - 575 EP - 596 PB - Springer Science + Business Media CY - Dordrecht AN - OPUS4-55905 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Henning, Ricky A1 - Sturm, Patrick A1 - Geddes, D.A. A1 - Keßler, S. A1 - Walkley, B. A1 - Gluth, Gregor T1 - The influence of curing temperature on the strength and phase assemblage of hybrid cements based on GGBFS/FA blends N2 - Hybrid cements are composites made of Portland cement or Portland clinker and one or more supplementary cementitious materials like slag, fly ash or metakaolin, activated with an alkali salt. To date, their hydration mechanism and the phase formation at various temperatures is insufficiently understood, partly due to the large variability of the raw materials used. In the present study, three hybrid cements based on ground granulated blast furnace slag, fly ash, Portland clinker and sodium sulfate, and an alkali-activated slag/fly ash blend were cured at 10 and 21.5°C, and subsequently analyzed by XRD, 27Al MAS NMR, and TGA. The compressive strength of the hybrid cements was higher by up to 27% after 91-day curing at 10°C, compared to curing at 21.5°C. The experimental results as well as thermodynamic modeling indicate that the differences in compressive strength were related to a different phase assemblage, mainly differing amounts of strätlingite and C-N-A-S-H, and the associated differences of the volume of hydration products. While the strätlingite was amorphous to X-rays, it could be identified by 27Al MAS NMR spectroscopy, TGA and thermodynamic modeling. The microstructural properties of the hybrid cements and the alkali-activated slag/fly ash blend as well as the compatibility between thermodynamic modeling results and experimental data as a function of curing temperature and time are discussed. KW - Hybrid cements KW - Strätlingite KW - Thermodynamic modelling KW - Hydration PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557767 DO - https://doi.org/10.3389/fmats.2022.982568 SN - 2296-8016 VL - 9 SP - 1 EP - 16 PB - Frontiers AN - OPUS4-55776 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Climent Terol, Estela A1 - Wan, Wei A1 - Rurack, Knut T1 - Toward Label-Free Optical Multiplexing of Analytes in Indicator Release Lateral Flow Assays via Detection Zones Containing Tailored Capture Materials N2 - The use of macromolecules and materials immobilized in the detection zone of test strips for indicator capture and focusing in label-free lateral flow assays (LFAs) is described, with emphasis on its future use in low number multiplexing. Several materials such as polyelectrolytes, functionalized mesoporous silica micro- and nanoparticles, chemically modified cellulose or glass fibre (GF) membranes and molecularly imprinted polymer gels coated onto membranes were studied in model assays, before the most promising materials were combined with antibody-gated indicator delivering (gAID) sensor materials. Cellulose, nitrocellulose and GF membranes were used as supports and highly fluorescent dyes of different charge states as model indicators. Combination of the best performing capture materials with gAID systems made it possible to distinctly increase the sensitivity and reduce the measurement uncertainty in the LFA testing of pentaerythritol tetranitrate (PETN) in aqueous samples. In addition, dual-plexing of PETN and 2,4,6-trinitrotoluene (TNT) was realized on a single test strip containing two dedicated capture zones. KW - Rapid tests KW - Vor-Ort-Analytik KW - Multiplexing KW - Teststreifen KW - Molecularly imprinted polymers PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557873 DO - https://doi.org/10.1002/anse.202100062 VL - 2 IS - 4 SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-55787 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Sebastian A1 - Bertmer, M. A1 - Gluth, Gregor T1 - Sol–gel synthesis and characterization of lithium aluminate (L–A–H) and lithium aluminosilicate (L–A–S–H) gels N2 - Hydrous lithium aluminosilicate (L–A–S–H) and lithium aluminate (L–A–H) gels are candidate precursors for glass-ceramics and ceramics with potential advantages over conventional processing routes. However, their structure before calcination remained largely unknown, despite the importance of precursor structure on the properties of the resulting materials. In the present study, it is demonstrated that L–A–S–H and L–A–H gels with Li/Al ≤ 1 can be produced via an organic steric entrapment route, while higher Li/Al ratios lead to crystallization of gibbsite or nordstrandite. The composition and the structure of the gels was studied by thermogravimetric analysis, X-ray diffraction, 27Al and 29Si magic-angle spinning nuclear magnetic resonance, and Raman spectroscopy. Aluminium was found to be almost exclusively in six-fold coordination in both the L–A–H and the L–A–S–H gels. Silicon in the L–A–S–H gels was mainly in Q4 sites and to a lesser extent in Q3 sites (four-fold coordination with no Si–O–Al bonds). The results thus indicate that silica-rich and aluminium-rich domains formed in these gels. KW - Lithium aluminosilicates KW - Raman spectroscopy KW - Sol-gel PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-558756 DO - https://doi.org/10.1111/ijac.14187 SN - 1546-542X VL - 19 IS - 6 SP - 3179 EP - 3190 PB - Wiley AN - OPUS4-55875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Griesche, Axel A1 - Pfretzschner, Beate A1 - Taparli, Ugur Alp A1 - Kardjilov, N. T1 - Time-Resolved Neutron Bragg-Edge Imaging: A Case Study by Observing Martensitic Phase Formation in Low Temperature Transformation (LTT) Steel during GTAW N2 - Polychromatic and wavelength-selective neutron transmission radiography were applied during bead-on-plate welding on 5 mm thick sheets on the face side of martensitic low transformation temperature (LTT) steel plates using gas tungsten arc welding (GTAW). The in situ visualization of austenitization upon welding and subsequent α’-martensite formation during cooling could be achieved with a temporal resolution of 2 s for monochromatic imaging using a single neutron wavelength and of 0.5 s for polychromatic imaging using the full spectrum of the beam (white beam). The spatial resolution achieved in the experiments was approximately 200 µm. The transmitted monochromatic neutron beam intensity at a wavelength of λ = 0.395 nm was significantly reduced during cooling below the martensitic start temperature M s since the emerging martensitic phase has a ~10% higher attenuation coefficient than the austenitic phase. Neutron imaging was significantly influenced by coherent neutron scattering caused by the thermal motion of the crystal lattice (Debye–Waller factor), resulting in a reduction in the neutron transmission by approx. 15% for monochromatic and by approx. 4% for polychromatic imaging. KW - Neutron radiography KW - Debye–Waller factor KW - Austenite-to-martensite transformation KW - Low transformation temperature (LTT) steel KW - Bragg-edge imaging KW - Gas tungsten arc welding (GTAW) PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559077 DO - https://doi.org/10.3390/app112210886 VL - 11 IS - 22 PB - MDPI AN - OPUS4-55907 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epping, Ruben A1 - Bliesener, Lilly A1 - Weiss, Tilman A1 - Koch, Matthias T1 - Marker Substances in the Aroma of Truffles N2 - The aim of this study was to identify specific truffle marker substances within the truffle aroma. The aroma profile of different truffle species was analyzed using static headspace sampling with gas chromatography mass spectrometry analysis (SHS/GC-MS). Possible marker substances were identified, taking the additional literature into account. The selected marker substances were tested in an experiment with 19 truffle dogs. The hypothesis “If trained truffle dogs recognize the substances as supposed truffles in the context of an experiment, they can be regarded as specific” was made. As it would be nearly impossible to investigate every other possible emitter of the same compounds to determine their specificity, this hypothesis was a reasonable approximation. We were interested in the question of what it is the dogs actually search for on a chemical level and whether we can link their ability to find truffles to one or more specific marker substances. The results of the dog experiment are not as unambiguous as could have been expected based on the SHS/GC-MS measurements. Presumably, the truffle aroma is mainly characterized and perceived by dogs by dimethyl sulfide and dimethyl disulfide. However, as dogs are living beings and not analytical instruments, it seems unavoidable that one must live with some degree of uncertainty regarding these results. KW - Truffle KW - Volatile organic compounds; KW - Gas chromatography KW - Mass spectrometry KW - Canine olfactometry PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556116 DO - https://doi.org/10.3390/molecules27165169 SN - 1420-3049 VL - 27 IS - 16 SP - 1 EP - 19 PB - MDPI CY - Basel AN - OPUS4-55611 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heuser, Lina A1 - Nofz, Marianne A1 - Müller, Ralf T1 - Alkali and alkaline earth zinc and lead borate glasses: Sintering and crystallization N2 - Glasses in the systems Me2O-ZnO-B2O3 with Me = Li, Na, K, Rb (MeZB), Na2O-ZnO-CuO-B2O3 (NZCuB), CaO-ZnO-B2O3 (CaZB), and Li2O-PbO-B2O3 (LPbB) as a reference, were studied by differential thermal analysis, dilatometry, rotational viscometry, and heating microscopy. A decrease of viscosity and sintering range was found with decreasing number of fourfold coordinated boron. The viscosity of the alkali zinc borate glasses varies only slightly. LPbB and CaZB stand out by their reduced and increased viscosities, respectively. Sodium, potassium, and calcium zinc borate glasses possess a fragility above 76. All glasses were sintered to full density before crystallization. Mostly binary zinc borate phases govern crystallization. A ternary crystalline phase was detected only in the potassium containing sample. The Weinberg glass stability parameter ranges between 0.07 and 0.12. This is caused by the presence of several crystalline phases and varying melting points of even the same crystalline phase in different glass matrices. KW - Alkali zinc borate glasses KW - Lead borate glasses KW - Viscosity KW - Sintering KW - Crystallization KW - Fragility PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556128 DO - https://doi.org/10.1016/j.nocx.2022.100116 SN - 2590-1591 VL - 15 SP - 1 EP - 8 PB - Elsevier CY - Amsterdam AN - OPUS4-55612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Spallanzani, Roberta A1 - Koga, K. A1 - Cichy, S. A1 - Wiedenbeck, M. A1 - Schmidt, B. A1 - Oelze, Marcus A1 - Wilke, M. T1 - Lithium and boron difusivity and isotopic fractionation in hydrated rhyolitic melts N2 - Lithium and boron are trace components of magmas, released during exsolution of a gas phase during volcanic activity. In this study, we determine the difusivity and isotopic fractionation of Li and B in hydrous silicate melts. Two glasses were synthesized with the same rhyolitic composition (4.2 wt% water), having diferent Li and B contents; these were studied in difusion-couple experiments that were performed using an internally heated pressure vessel, operated at 300 MPa in the temperature range 700–1250 °C for durations from 0 s to 24 h. From this we determined activation energies for Li and B difusion of 57±4 kJ/mol and 152±15 kJ/mol with pre-exponential factors of 1.53 × 10–7 m2/s and 3.80× 10–8 m2 /s, respectively. Lithium isotopic fractionation during difusion gave β values between 0.15 and 0.20, whereas B showed no clear isotopic fractionation. Our Li difusivities and isotopic fractionation results difer somewhat from earlier published values, but overall confrm that Li difusivity increases with water content. Our results on B difusion show that similarly to Li, B mobility increases in the presence of water. By applying the Eyring relation, we confrm that B difusivity is limited by viscous fow in silicate melts. Our results on Li and B difusion present a new tool for understanding degassing-related processes, ofering a potential geospeedometer to measure volcanic ascent rates. KW - Hydrated silicate melts KW - Stable isotopes KW - Diffusion KW - Isotopic fractionation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554496 DO - https://doi.org/10.1007/s00410-022-01937-2 VL - 177 IS - 8 SP - 1 EP - 17 PB - Springer AN - OPUS4-55449 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Balko, J. A1 - Büsse, T. A1 - Kunkel, J. A1 - Kupsch, Andreas A1 - Wieder, Frank T1 - Schau(m) an, es geht... – Geschäumter Biokunststoff PBS für Leichtbau, Isolierwerkstoffe und Verpackungsmittel N2 - Flexible, niedrigdichte Schäume aus Biokunststoffen im Extrusionsverfahren herzustellen war bisher industriell noch nicht möglich. Im Verarbeitungstechnikum Biopolymere des Fraunhofer IAP wurde in einem Projekt die Eignung von PBS-basierten Biokunststofftypen für Schaumanwendungen erforscht und weiterentwickelt. KW - Polymer KW - Schaum KW - Polybutylensuccinat (PBS) KW - Biokunststoff KW - Computertomographie PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555832 UR - https://www.plastverarbeiter.de/heftarchiv-ausgabendetail/plastverarbeiter-07-08-2022.html SN - 0032–1338 VL - 73 IS - 7/8 SP - 50 EP - 52 PB - Hüthig GmbH CY - Heidelberg AN - OPUS4-55583 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Olscher, C. A1 - Jandric, A. A1 - Zafiu, C. A1 - Part, Florian T1 - Evaluation of marker materials and spectroscopic methods for tracer-based sorting of plastic wastes N2 - Plastics are a ubiquitous material with good mechanical, chemical and thermal properties, and are used in all industrial sectors. Large quantities, widespread use, and insufficient management of plastic wastes lead to low recycling rates. The key challenge in recycling plastic waste is achieving a higher degree of homogeneity between the different polymer material streams. Modern waste sorting plants use automated sensor-based sorting systems capable to sort out commodity plastics, while many engineering plastics, such as polyoxymethylene (POM), will end up in mixed waste streams and are therefore not recycled. A novel approach to increasing recycling rates is tracer-based sorting (TBS), which uses a traceable plastic additive or marker that enables or enhances polymer type identification based on the tracer’s unique fingerprint (e.g., fluorescence). With future TBS applications in mind, we have summarized the literature and assessed TBS techniques and spectroscopic detection methods. Furthermore, a comprehensive list of potential tracer substances suitable for thermoplastics was derived from the literature. We also derived a set of criteria to select the most promising tracer candidates (3 out of 80) based on their material properties, toxicity profiles, and detectability that could be applied to enable the circularity of, for example, POM or other thermoplastics. KW - Circular economy KW - Post-consumer plastic waste KW - Plastic waste recycling KW - Tracer-based sorting KW - Sensor-based sorting KW - Spectroscopy KW - Fluorescent markers KW - Thermoplastics KW - Polyoxymethylene PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555624 DO - https://doi.org/10.3390/polym14153074 SN - 2073-4360 VL - 14 SP - 1 EP - 20 PB - MDPI CY - Basel AN - OPUS4-55562 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hobmeier, K. A1 - Oppermann, M. A1 - Stasinski, N. A1 - Kremling, A. A1 - Pflüger-Grau, K. A1 - Kunte, Hans-Jörg A1 - Marin Sanguino, A. T1 - Metabolic engineering of Halomonas elongata: Ectoine secretion is increased by demand and supply driven approaches N2 - The application of naturally-derived biomolecules in everyday products, replacing conventional synthetic manufacturing, is an ever-increasing market. An example of this is the compatible solute ectoine, which is contained in a plethora of treatment formulations for medicinal products and cosmetics. As of today, ectoine is produced in a scale of tons each year by the natural producer Halomonas elongata. In this work, we explore two complementary approaches to obtain genetically improved producer strains for ectoine production. We explore the effect of increased precursor supply (oxaloacetate) on ectoine production, as well as an implementation of increased ectoine demand through the overexpression of a transporter. Both approaches were implemented on an already genetically modified ectoine-excreting strain H. elongata KB2.13 (ΔteaABC ΔdoeA) and both led to new strains with higher ectoine excretion. The supply driven approach led to a 45% increase in ectoine titers in two different strains. This increase was attributed to the removal of phosphoenolpyruvate carboxykinase (PEPCK), which allowed the conversion of 17.9% of the glucose substrate to ectoine. For the demand driven approach, we investigated the potential of the TeaBC transmembrane proteins from the ectoine-specific Tripartite ATP-Independent Periplasmic (TRAP) transporter as export channels to improve ectoine excretion. In the absence of the substrate-binding protein TeaA, an overexpression of both subunits TeaBC facilitated a three-fold increased excretion rate of ectoine. Individually, the large subunit TeaC showed an approximately five times higher extracellular ectoine concentration per dry weight compared to TeaBC shortly after its expression was induced. However, the detrimental effect on growth and ectoine titer at the end of the process hints toward a negative impact of TeaC overexpression on membrane integrity and possibly leads to cell lysis. By using either strategy, the ectoine synthesis and excretion in H. elongata could be boosted drastically. The inherent complementary nature of these approaches point at a coordinated implementation of both as a promising strategy for future projects in Metabolic Engineering. Moreover, a wide variation of intracelllular ectoine levels was observed between the strains, which points at a major disruption of mechanisms responsible for ectoine regulation in strain KB2.13. KW - Osmoadaptation KW - Metabolic engineering PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555644 DO - https://doi.org/10.3389/fmicb.2022.968983 SN - 1664-302X VL - 13 SP - 1 EP - 13 PB - Frontiers Media CY - Lausanne AN - OPUS4-55564 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Amadeus A1 - Schröpfer, Dirk A1 - Kromm, Arne A1 - Kannengießer, Thomas T1 - Determination of residual stress evolution during repair welding of high-strength steel components N2 - During the assembly of steel structures, unacceptable weld defects may be found. An economical solution is local thermal gouging of the affected areas and re-welding. Due to high shrinkage restraints of repair weld and sur- rounding structure, high global and local welding stresses superimpose, and may lead to cracking and component failure, especially in connection with the degraded microstructure and mechanical properties of high-strength steels during the repair process. Component-related investigations of high-strength steels (FOSTA P1311/ IGF20162N) focus on welding residual stress evolution during local thermal gouging and rewelding. In this study, repair welding of S500MLO (EN 10225) is carried out using in-situ digital image correlation (DIC) and ex- situ X-ray diffraction (XRD) to analyse strains and stresses. Self-restrained slit specimen geometries were identified representing defined rigidity conditions of repair welds of real components, which were quantified using the restraint intensity concept. The specimens were rewelded with constant welding heat control and parameters. Weld specimens exhibited significantly increased transverse residual stresses with higher transverse restraint intensities, in the weld metal, and in the heat affected zone. Transverse stresses along the weld seam decrease at the weld seam ends leading to different stress state during gouging and welding. XRD analysis of the longitudinal and transverse local residual stresses after cooling to RT showed a good comparability with global DIC analyses. KW - Repair-welding KW - High-strength steels KW - X-ray diffraction KW - Digital image correlation KW - Residual stresses PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555672 DO - https://doi.org/10.1016/j.finmec.2022.100073 SN - 2666-3597 VL - 6 SP - 1 EP - 6 PB - Elsevier CY - Amsterdam AN - OPUS4-55567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Golusda, L. A1 - Kühl, A. A. A1 - Lehmann, M. A1 - Dahlke, K. A1 - Mueller, S. A1 - Boehm-Sturm, P. A1 - Saatz, Jessica A1 - Traub, Heike A1 - Schnorr, J. A1 - Freise, C. A1 - Taupitz, M. A1 - Biskup, K. A1 - Blanchard, V. A1 - Klein, O. A1 - Sack, I. A1 - Siegmund, B. A1 - Paclik, D. T1 - Visualization of inflammation in experimental colitis by magnetic resonance imaging using very small superparamagnetic iron oxide particles N2 - Inflammatory bowel diseases (IBD) comprise mainly ulcerative colitis (UC) and Crohn´s disease (CD). Both forms present with a chronic inflammation of the (gastro) intestinal tract, which induces excessive changes in the composition of the associated extracellular matrix (ECM). In UC, the inflammation is limited to the colon, whereas it can occur throughout the entire gastrointestinal tract in CD. Tools for early diagnosis of IBD are still very limited and highly invasive and measures for standardized evaluation of structural changes are scarce. To investigate an efficient non-invasive way of diagnosing intestinal inflammation and early changes of the ECM, very small superparamagnetic iron oxide nanoparticles (VSOPs) in magnetic resonance imaging (MRI) were applied in two mouse models of experimental colitis: the dextran sulfate sodium (DSS)-induced colitis and the transfer model of colitis. For further validation of ECM changes and inflammation, tissue sections were analyzed by immunohistochemistry. For in depth ex-vivo investigation of VSOPs localization within the tissue, Europium-doped VSOPs served to visualize the contrast agent by imaging mass cytometry (IMC). VSOPs accumulation in the inflamed colon wall of DSS-induced colitis mice was visualized in T2* weighted MRI scans. Components of the ECM, especially the hyaluronic acid content, were found to influence VSOPs binding. Using IMC, colocalization of VSOPs with macrophages and endothelial cells in colon tissue was shown. In contrast to the DSS model, colonic inflammation could not be visualized with VSOP-enhanced MRI in transfer colitis. VSOPs present a potential contrast agent for contrast-enhanced MRI to detect intestinal inflammation in mice at an early stage and in a less invasive manner depending on hyaluronic acid content. KW - Inflammation KW - Imaging KW - Immunohistochemistry KW - MRI KW - Nanoparticle KW - Extracellular matrix KW - Laser ablation KW - ICP-MS PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555395 DO - https://doi.org/10.3389/fphys.2022.862212 SN - 1664-042X VL - 13 IS - July 2022 SP - 1 EP - 15 PB - Frontiers Research Foundation CY - Lausanne AN - OPUS4-55539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Diener, S. A1 - Schubert, Hendrik A1 - Held, A. A1 - Katsikis, N. A1 - Günster, Jens A1 - Zocca, Andrea T1 - Influence of the dispersant on the parts quality in slurry-based binder jetting of SiC ceramics N2 - Binder jetting is establishing more and more in the ceramic industry to produce large complex shaped parts. A parameter with a great impact on the quality of the parts is the binder–powder interaction. The use of ceramic slurries as feedstock for this process, such as in the layerwise slurry deposition–print technology, allows a great flexibility in the composition. Such slurries are typically composed of ceramic powder, water, and small amounts of various additives. The understanding of the effect of these components on the printing quality is thus essential for the feedstock development. Four models were developed regarding the impact of additives, such as dispersants on printing. These models were confirmed or rebutted by experiments performed for an SiC slurry system with two different concentrations of a dispersant and a commercial phenolic resin used as a binder. It is shown that for this system the influence of the dispersant on the curing behavior and the clogging of the pores by dispersant can be neglected. The redispersion of the dispersant after the curing of the resin has no or only a minor effect. However, the wetting behavior determined by the surface energies of the system seem to be most crucial. In case the surface energy of the slurry additive is significantly lower than the surface energy of the binder, the strength of the green parts and the printing quality will be low. This was shown by inverse gas chromatography, contact angle measurement, rheological characterization, and mechanical tests with casted samples. KW - Additive Manufacturing KW - Binder Jetting KW - Layerwise slurry deposition KW - Silicon carbide KW - Wetting PY - 2022 DO - https://doi.org/10.1111/jace.18693 SN - 1551-2916 VL - 2022 SP - 1 EP - 15 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-55542 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Henning, L. M. A1 - Müller, J. T. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Schmidt, J. A1 - Bekheet, M. F. A1 - Gurlo, A. A1 - Simon, U. T1 - Hierarchically porous and mechanically stable monoliths from ordered mesoporous silica and their water filtration potential N2 - Mechanically stable structures with interconnected hierarchical porosity combine the benefits of both small and large pores, such as high surface area, pore volume, and good mass transport capabilities. Hence, lightweight micro-/meso-/macroporous monoliths are prepared from ordered mesoporous silica COK-12 by means of spark plasma sintering (SPS, S-sintering) and compared to conventionally (C-) sintered monoliths. A multi-scale model is developed to fit the small angle X-ray scattering data and obtain information on the hexagonal lattice parameters, pore sizes from the macro to the micro range, as well as the dimensions of the silica population. For both sintering techniques, the overall mesoporosity, hexagonal pore ordering, and amorphous character are preserved. The monoliths' porosity (77–49%), mesopore size (6.2–5.2 nm), pore volume (0.50–0.22 g cm-3 ), and specific surface area (451–180 m2 g-1) decrease with increasing processing temperature and pressure. While the difference in porosity is enhanced, the structural parameters between the C-and S-sintered monoliths are largely converging at 900 C, except for the mesopore size and lattice parameter, whose dimensions are more extensively preserved in the S-sintered monoliths, however, coming along with larger deviations from the theoretical lattice. Their higher mechanical properties (biaxial strength up to 49 MPa, 724 MPa HV 9.807 N) at comparable porosities and ability to withstand ultrasonic treatment and dead-end filtration up to 7 bar allow S-sintered monoliths to reach a high permeance (2634 L m-2 h-1 bar-1), permeability (1.25 x 10^-14 m2), and ability to reduce the chemical oxygen demand by 90% during filtration of a surfactant-stabilized oil in water emulsion, while indicating reasonable resistance towards fouling. KW - SAXS KW - Hierarchically porous KW - Silica KW - Water filtration PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555928 DO - https://doi.org/10.1039/D2NA00368F SN - 2516-0230 SP - 1 EP - 17 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-55592 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yao, J. A1 - Jiang, T. A1 - Ji, Y. A1 - An-Stepec, Biwen Annie A1 - Koerdt, Andrea A1 - Cai, Z. A1 - Dong, C. A1 - Ge, Y. A1 - Qi, Z. T1 - Water-Fueled Autocatalytic Bactericidal Pathway based on e-Fenton-Like Reactions Triggered by Galvanic Corrosion and Extracellular Electron Transfer N2 - Water is generally considered to be an undesirable substance in fuel system, which may lead to microbial contamination. The antibacterial strategies that can turn water into things of value with high disinfection efficacy have been urgently needed for fuel system. Here, we reveal a water-fueled autocatalytic bactericidal pathway comprised by bi-metal micro-electrode system, which can spontaneously produce reactive oxygen species (mainly H2O2 and O2•–) by the electron Fenton-like reaction in water medium without external energy., The respiratory chain component of bacteria and the galvanic corrosion on the coated metals were two electron sources in the system. The specific model of Ag-Ru water-fueled autocatalytic (WFA) microelectrode particles presents extremely high disinfection efficiency (>99.9999%) in less than one hour for three aerobic bacteria (Escherichia coli, Pseudomonas aeruginosa and Bacillus subtilis) in LB media and high disinfection efficiency for the anaerobic bacteria (Desulfovibrio alaskensis) in Postgate E media without natural light irradiation. Overall, the novel WFA Ag-Ru antibacterial material explored in this study has a high potential for sterilizing applications in fuel system and this work provides the potential for the development of non-chemical and water-based antibacterial materials, such as WFA Ag-Ru antibacterial coating on stainless steel. KW - Fenton-like reaction KW - Reactive oxygen species KW - Disinfection Fuel KW - Silver KW - Ruthenium KW - MIC PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555186 DO - https://doi.org/10.1016/j.jhazmat.2022.129730 SN - 0304-3894 VL - 440 SP - 1 EP - 11 PB - Elsevier CY - Amsterdam AN - OPUS4-55518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shaheen, Sabahat A1 - Hicke, Konstantin T1 - Geometric phase in distributed fiber optic sensing N2 - The geometric phase in the beat signal from coherent interference of two frequency-offset light beams is measured using a novel distributed optical fiber sensing setup. In a fiber optic medium, with changing beam intensities, to the best of our knowledge, ours is the first measurement of the mentioned geometric phase. Experimental results of applying a 100-Hz sinusoidal stimulus to a polarization scrambler and a piezoelectric transducer inline to an optical fiber are presented. The results may enable novel distributed fiber sensing techniques. KW - Distributed fiber optic sensing KW - Geometric phase measurement KW - Distributed vibration sensing KW - C-OTDR PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556053 DO - https://doi.org/10.1364/OL.464259 VL - 47 IS - 15 SP - 3932 EP - 3935 PB - Optica CY - Washington D.C., USA AN - OPUS4-55605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gook, S. A1 - Midik, A. A1 - Biegler, M. A1 - Gumenyuk, Andrey A1 - Rethmeier, Michael T1 - Joining 30 mm Thick Shipbuilding Steel Plates EH36 Using a Process Combination of Hybrid Laser Arc Welding and Submerged Arc Welding N2 - This article presents a cost-effective and reliable method for welding 30 mm thick sheets of shipbuilding steel EH36. The method proposes to perform butt welding in a two-run technique using hybrid laser arc welding (HLAW) and submerged arc welding (SAW). The HLAW is performed as a partial penetration weld with a penetration depth of approximately 25 mm. The SAWis carried out as a second run on the opposite side. With a SAWpenetration depth of 8 mm, the weld cross-section is closed with the reliable intersection of both passes. The advantages of the proposed welding method are: no need for forming of the HLAW root; the SAW pass can effectively eliminate pores in the HLAWroot; the high stability of the welding process regarding the preparation quality of the weld edges. Plasma cut edges can be welded without lack of fusion defects. The weld quality achieved is confirmed by destructive tests. KW - Shipbuilding steel KW - Hybrid laser arc welding KW - Submerged arc welding KW - Hardness KW - Bending test KW - Two-run welding technique KW - Microstructure PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556090 DO - https://doi.org/10.3390/jmmp6040084 SN - 2504-4494 VL - 6 IS - 4 SP - 1 EP - 11 PB - MDPI CY - Basel AN - OPUS4-55609 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heuser, Lina A1 - Nofz, Marianne T1 - Alkali and alkaline earth zinc and lead borate glasses: Structure and properties N2 - Low melting Li2O-PbO-B2O3, Me2O-ZnO-B2O3, Me = Li, Na, K, Rb and CaO-ZnO-B2O3 glasses were studied with Raman and infrared spectroscopies to advance the structural understanding of zinc borate glasses as potential candidates for substitution of lead containing glasses. Although the effect of type of alkali ions on the number (N4) of fourfold coordinated boron (B4) in the glasses is small, the alkali ions direct the type of borate groups, i.e., pentaborate in lithium, sodium, and calcium zinc borate glasses, as well as diborate in potassium and rubidium containing ones. Both groups were simultaneously found in Li2O-PbO-B2O3. Alkali ions are mainly responsible for the formation of B4-units and metaborate. Zinc ions favorably compensate non-bridging oxygen and partially form ZnO4. With decreasing N4 and field strength of the alkali ions the atomic packing density, glass transition temper ature and Young’s Modulus also decrease. The coefficient of thermal expansion increases with decreasing N4. KW - Raman spectroscopy KW - IR spectroscopy KW - Alkali zinc borate glasses KW - Lead borate glasses KW - Physical properties KW - Young’s Modulus PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556109 DO - https://doi.org/10.1016/j.nocx.2022.100109 SN - 2590-1591 VL - 15 SP - 1 EP - 12 PB - Elsevier CY - Amsterdam AN - OPUS4-55610 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klewe, Tim A1 - Völker, Tobias A1 - Götz, J. A1 - Landmann, M. A1 - Wilsch, Gerd A1 - Kruschwitz, Sabine T1 - Sorting of construction and demolition waste by combining LIBS with NIR spectroscopy N2 - In a joint project of partners from industry and research, the automated recycling of construction and demolition waste (CDW) is investigated and tested by combing laser-induced breakdown spectroscopy (LIBS) and near-infrared (NIR) spectroscopy. Joint processing of information (data fusion) is expected to significantly improve the sorting quality of various materials like concrete, main masonry building materials, organic components, etc., and may enable the detection and separation of impurities such as SO3-cotaining building materials (gypsum, aerated concrete, etc.). The project focuses primarily on the Berlin site to analyze the entire value chain, minimize economic/technological barriers and obstacles at the cluster level, and sustainably increase recovery and recycling rates. First measurements with LIBS and NIR spectroscopy show promising results in distinguishing various material types and indicate the potential for a successful combination. In addition, X-ray fluorescence (XRF) spectroscopy is being performed to obtain more information about the quantitative elemental composition of the different building materials. Future work will apply the developed sorting methodology in a fully automated measurement setup with CDW on a conveyor belt. T2 - NDT-CE 2022 CY - Zurich, Switzerland DA - 16.08.2022 KW - LIBS KW - NDT KW - Circular economy KW - Recycling KW - Material classification PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555531 UR - http://www.ndt.net/?id=27220 VL - 2022/09 SP - 1 EP - 9 PB - NDT.net CY - Bad Breisig AN - OPUS4-55553 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kimani, Martha Wamaitha A1 - Kislenko, Evgeniia A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Fluorescent molecularly imprinted polymer particles for glyphosate detection using phase transfer agents N2 - In this work, molecular imprinting was combined with direct fluorescence detection of the pesticide Glyphosate (GPS). Firstly, the solubility of highly polar GPS in organic solvents was improved by using lipophilic tetrabutylammonium (TBA+) and tetrahexylammonium (THA+) counterions. Secondly, to achieve fluorescence detection, a fluorescent crosslinker containing urea-binding motifs was used as a probe for GPS-TBA and GPS-THA salts in chloroform, generating stable complexes through hydrogen bond formation. The GPS/fluorescent dye complexes were imprinted into 2–3 nm fluorescent molecularly imprinted polymer (MIP) shells on the surface of sub-micron silica particles using chloroform as porogen. Thus, the MIP binding behavior could be easily evaluated by fluorescence titrations in suspension to monitor the spectral changes upon addition of the GPS analytes. While MIPs prepared with GPS-TBA and GPS-THA both displayed satisfactory imprinting following titration with the corresponding analytes in chloroform, GPS-THA MIPs displayed better selectivity against competing molecules. Moreover, the THA+ counterion was found to be a more powerful phase transfer agent than TBA+ in a biphasic assay, enabling the direct fluorescence detection and quantification of GPS in water. A limit of detection of 1.45 μM and a linear range of 5–55 μM were obtained, which match well with WHO guidelines for the acceptable daily intake of GPS in water (5.32 μM). KW - Glyphosate KW - Molecular imprinting KW - Core-shell particles KW - Fluorescent sensors PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555281 DO - https://doi.org/10.1038/s41598-022-16825-9 SN - 2045-2322 VL - 12 IS - 1 SP - 1 EP - 15 PB - Macmillan Publishers Limited CY - London AN - OPUS4-55528 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zabihi, Mohammadmasoud A1 - Krebber, Katerina T1 - Approach for Faster Signal Processing in Փ-OTDR Systems Based on Directional Measurement of Fiber Slices Interaction N2 - In this study, a signal processing approach for heterodyne Փ-OTDR and C-OTDR systems that can obtain external perturbation and its frequency content in a faster way is proposed. We can detect vibrations with the same or better SNR using this processing approach, only with a single step and fast calculation. Fig. 12 shows the comparison of the normalized measurement time for the gamma matrix method and the conventional method throughout the three experiments. The speed of processing using a gamma matrix is ~35%–50% faster compared to a conventional method in high frequency test (PZT), low frequency test (walking) and street monitoring test. The processing speed in low frequency test is normally a bit lower than the similar high frequency one, since we must use higher number of time frames. Also, in street test we have higher speed because we can select wider gauges. KW - Փ-OTDR PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560492 DO - https://doi.org/10.1364/OPTCON.456421 VL - 1 IS - 8 SP - 1837 EP - 1847 PB - Optica Publishing Group CY - Washington, DC AN - OPUS4-56049 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zabihi, Mohammadmasoud A1 - Krebber, Katerina T1 - Laser source frequency drift compensation in Φ-OTDR systems using multiple probe frequencies N2 - In this study, an approach for mitigation of LSFD in Φ-OTDR systems was proposed. By using one probe pulse as a reference in a system with two or more probe frequencies, we can remove unwanted low frequency noise that is originally caused by the laser source. Although LSFD is problematic issue, it is not the only source of low frequency noise. Change in temperature, humidity, physical surroundings, environment, etc., can result in such noises. The proposed method; however, is expected to highly suppresses all of these effects, regardless of their source, either in the time or frequency domain. For comparing reference and probe signals, there are sophisticated methods, rather than normal differentiation, available for use. Some of these methods have a close relationship with CPD methods and can further enhance the results. These methods can be further discussed in an independent research or future work. The proposed method is very helpful for increasing accuracy in passive and active seismic monitoring, reservoir monitoring, underwater monitoring, etc. It also helps using relatively simpler laser sources and make the whole system price-efficient, as well as processing data without lengthy compensation algorithms. KW - Frequency Drift KW - Փ-OTDR KW - LSFD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560517 DO - https://doi.org/10.1364/oe.460302 SN - 1094-4087 VL - 30 IS - 11 SP - 19990 EP - 19998 PB - Optica CY - Washington, DC AN - OPUS4-56051 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fritzsche, Sven A1 - Jaenisch, Gerd-Rüdiger A1 - Pavasaryte, Lina A1 - Funk, Alexander T1 - XCT and DLW: Synergies of Two Techniques at Sub-Micrometer Resolution N2 - Direct Laser Writing (DLW) and X-ray computed tomography (XCT) both offer unique possibilities in their respective fields. DLW produces full three-dimensional (3D) polymer structures on the microscale with resolutions below 100 nm. The fabricated structures can be analysed by XCT or X-ray microscopy (XRM), which incorporates additional X-ray lenses, in three dimensions down to a minimal basic spatial resolution of about 500 nm or 50 nm, respectively. In this work, two different DLW structures are analysed via XCT. Internal defects are detected and analysed for the purpose of quality control. Defects and structures with sizes down to 1.5 µm are successfully analysed. A 3D reconstruction and internal, hidden features of the fabricated structures are shown and discussed. In a first-of-its-kind study, we demonstrate the detectability of a single-voxel line inside a fabricated structure that would not be detectable with SEM or light microscopy. Furthermore, the direct fabrication on a PET substrate is shown to overcome the high X-ray absorbance of commonly used glass substrates. Attenuation spectra of SZ2080 and glass substrates are compared to a fabrication route direct on a 170 µm PET foil. The practical aspects of XCT measurements for DLW structures on different substrates will be discussed. KW - Non-destructive testing KW - Two-photon polymerization KW - X-ray microscopy KW - XCT KW - 2PP KW - Direct laser writing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560525 DO - https://doi.org/10.3390/app122010488 VL - 12 IS - 20 SP - 1 EP - 15 PB - MDPI CY - Basel AN - OPUS4-56052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Orf, I. A1 - Tenenboim, H. A1 - Omranian, N. A1 - Nikoloski, Z. A1 - Fernie, A. R. A1 - Lisec, Jan A1 - Brotman, Y. A1 - Bromke, M. A. T1 - Transcriptomic and Metabolomic Analysis of a Pseudomonas-Resistant versus a Susceptible Arabidopsis Accession N2 - Accessions of one plant species may show significantly different levels of susceptibility to stresses. The Arabidopsis thaliana accessions Col-0 and C24 differ significantly in their resistance to the pathogen Pseudomonas syringae pv. tomato (Pst). To help unravel the underlying mechanisms contributing to this naturally occurring variance in resistance to Pst, we analyzed changes in transcripts and compounds from primary and secondary metabolism of Col-0 and C24 at different time points after infection with Pst. Our results show that the differences in the resistance of Col-0 and C24 mainly involve mechanisms of salicylic-acid-dependent systemic acquired resistance, while responses of jasmonic-acid-dependent mechanisms are shared between the two accessions. In addition, arginine metabolism and differential activity of the biosynthesis pathways of aliphatic glucosinolates and indole glucosinolates may also contribute to the resistance. Thus, this study highlights the difference in the defense response strategies utilized by different genotypes. KW - Mass Spectrometry KW - Arabidopsis KW - Resistance PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559549 DO - https://doi.org/10.3390/ijms232012087 VL - 23 IS - 20 SP - 1 EP - 27 PB - MDPI AN - OPUS4-55954 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lüdicke, M. G. A1 - Hildebrandt, Jana A1 - Schindler, C. A1 - Sperling, R. A. A1 - Maskos, M. T1 - Automated QuantumDots Purification via Solid Phase Extraction N2 - The separation of colloidal nanocrystals from their original synthesis medium is an essential process step towards their application, however, the costs on a preparative scale are still a constraint. A new combination of approaches for the purification of hydrophobic Quantum Dots is presented, resulting in an efficient scalable process in regard to time and solvent consumption, using common laboratory equipment and low-cost materials. The procedure is based on a combination of solvent-induced adhesion and solid phase extraction. The platform allows the transition from manual handling towards automation, yielding an overall purification performance similar to one conventional batch precipitation/centrifugation step, which was investigated by thermogravimetry and gas chromatography. The distinct miscibility gaps between surfactants used as nanoparticle capping agents, original and extraction medium are clarified by their phase diagrams, which confirmed the outcome of the flow chemistry process. Furthermore, the solubility behavior of the Quantum Dots is put into context with the Hansen solubility parameters framework to reasonably decide upon appropriate solvent types. KW - Quantum Dots KW - Purification PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559590 DO - https://doi.org/10.3390/nano12121983 SN - 2079-4991 VL - 12 IS - 12 PB - MDPI CY - Basel AN - OPUS4-55959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wurzler, Nina A1 - Hidde, Gundula A1 - Schenderlein, Matthias A1 - Özcan Sandikcioglu, Özlem T1 - Effect of organic conditioning layers adsorbed on stainless steel AISI 304 on the attachment and biofilm formation of electroactive bacteria Shewanella putrefaciens CN32 N2 - The initial attachment and subsequent biofilm formation of electroactive bac-teriaShewanella putrefaciensCN32 was investigated to clarify the influence oforganic conditioning layers. A selection of macromolecules and self-assembledmonolayers (SAMs) of different chain lengths and functional groups were pre-pared and characterized by means of infrared spectroscopy in terms of theirchemistry. Surface energy and Zeta (ζ-) potential of the conditioning layers wasdetermined with contact angle and streaming current measurements. Amongthe studied surface parameters, a high polar component and a high ratio ofpolar-to-disperse components of the surface energy has emerged as a successfulindicator for the inhibition of the initial settlement ofS. putrefacienson stainlesssteel AISI 304 surfaces. Considering the negative surface charge of planktonicS. putrefacienscells, and the strong inhibition of cell attachment by positivelycharged polyethylenimine (PEI) conditioning layers, our results indicate thatelectrostatic interactions do play a subordinate role in controlling the attach-ment of this microorganism on stainless steel AISI 304 surfaces. For the biofilmformation, the organization of the SAMs affected the local distribution of thebiofilms. The formation of three-dimensional and patchy biofilm networks waspromoted with increasing disorder of the SAMs. KW - Bacterial attachment KW - Conditioning films KW - Self-assembled monolayers KW - Stainless steel PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559887 DO - https://doi.org/10.1002/eng2.12458 VL - 4 IS - 1 SP - 1 EP - 12 PB - Wiley online library AN - OPUS4-55988 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija A1 - Given, Joseph A1 - Rentala, V. K. A1 - Lehleitner, Johannes A1 - Kanzler, D. A1 - Heckel, Thomas A1 - Tkachenko, Viktoriya T1 - Human Factors in der POD - ist das möglich? N2 - Menschliche Faktoren sind ein häufig genanntes Thema, wenn wir über die Zuverlässigkeit der zerstörungsfreien Prüfung (ZfP) sprechen. Die Probability of Detection (POD), das üblicherweise verwendete Maß für die Zuverlässigkeit der ZfP, betrachtet jedoch nur die technische Fähigkeit eines ZfP-Systems, einen Fehler zu entdecken. Nach mehreren Jahrzehnten der Erforschung des Einflusses der menschlichen Faktoren auf die Zuverlässigkeit der ZfP gibt es immer noch keinen allgemein akzeptierten Ansatz, um menschliche Faktoren in der Zuverlässigkeitsbewertung sichtbar zu machen. Dieser Beitrag gibt einen Überblick über verschiedene verfügbare Methoden zur Einbeziehung menschlicher Faktoren in die Zuverlässigkeitsbewertung. Das Thema ist ein essenzieller Bestandteil des laufenden WIPANO-Projekts "normPOD", das sich als Ziel gesetzt hat, die Standardisierung der Zuverlässigkeitsbewertung in Deutschland voranzutreiben und im Vergleich zu den schon bekannten internationalen Normen einen Fokus auf den Umgang mit den menschlichen Faktoren zu legen. T2 - DGZfP Jahrestagung 2022 CY - Kassel, Germany DA - 23.05.2022 KW - Human factors KW - Zuverlässigkeit KW - POD KW - Probability of detection KW - Reliability PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559942 SP - 1 EP - 15 AN - OPUS4-55994 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gluth, Gregor A1 - Ke, X. A1 - Vollpracht, A. A1 - Weiler, L. A1 - Bernal, S. A. A1 - Cyr, M. A1 - Dombrowski-Daube, K. A1 - Geddes, D. A. A1 - Grengg, C. A1 - Le Galliard, C. A1 - Nedeljkovic, M. A1 - Provis, J. L. A1 - Valentini, L. A1 - Walkley, B. T1 - Carbonation rate of alkali-activated concretes and high-volume SCM concretes: a literature data analysis by RILEM TC 281-CCC N2 - The current understanding of the carbonation and the prediction of the carbonation rate of alkali-activated concretes is complicated inter alia by the wide range of binder chemistries used and testing conditions adopted. To overcome some of the limitations of individual studies and to identify general correlations between mix design parameters and carbonation resistance, the RILEM TC 281-CCC ‘Carbonation of Concrete with Supplementary Cementitious Materials’ Working Group 6 compiled and analysed carbonation data for alkali-activated concretes and mortars from the literature. For comparison purposes, data for blended Portland cement-based concretes with a high percentage of SCMs (≥ 66% of the binder) were also included in the database. The analysis indicates that water/CaO ratio and water/binder ratio exert an influence on the carbonation resistance of alkali-activated concretes; however, these parameters are not good indicators of the carbonation resistance when considered individually. A better indicator of the carbonation resistance of alkali-activated concretes under conditions approximating natural carbonation appears to be their water/(CaO + MgOeq + Na2Oeq + K2Oeq) ratio, where the subscript ‘eq’ indicates an equivalent amount based on molar masses. Nevertheless, this ratio can serve as approximate indicator at best, as other parameters also affect the carbonation resistance of alkali-activated concretes. In addition, the analysis of the database points to peculiarities of accelerated tests using elevated CO2 concentrations for low-Ca alkali-activated concretes, indicating that even at the relatively modest concentration of 1% CO2, accelerated testing may lead to inaccurate predictions of the carbonation resistance under natural exposure conditions. KW - Alkali-activated materials KW - Durability KW - Carbonation KW - Accelerated testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560037 DO - https://doi.org/10.1617/s11527-022-02041-4 VL - 55 IS - 8 SP - 1 EP - 15 PB - Springer Nature AN - OPUS4-56003 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jüngert, A. A1 - Heckel, Thomas A1 - Tkachenko, Viktoriya A1 - Bertovic, Marija A1 - Vrana, J. A1 - Kanzler, D. T1 - POD, aber wie? Konzeption und Herstellung von Testkörpersätzen und Prüfvorschriften für die experimentelle Zuverlässigkeitsbestimmung von ZfP-Prüfansätzen N2 - Im Rahmen des WIPANO Vorhabens „normPOD“ wird eine Richtlinie zur experimentellen und simulationsgestützten Zuverlässigkeitsbewertung erstellt. In der Richtlinie wird die Zuverlässigkeitsbewertung beispielhaft für zwei praktische Anwendungsfälle vorgestellt. Ein Anwendungsfall beschäftigt sich mit konventionellen Ultraschallprüfungen an ferritischen Stählen und deren Schweißnähten. Zur Berechnung von Probability-Of-Detection (POD)-Kurven ist es notwendig, dass ein geeigneter Testkörpersatz zur Verfügung steht, der sowohl leicht zu findende Fehlstellen als auch Fehlstellen, die an der Grenze der Detektierbarkeit liegen, enthält. Im Vorhaben kommen verschiedene Testkörper zum Einsatz, die entweder Ersatzfehler wie Nuten und Bohrungen oder künstlich eingebrachte realistische Fehlstellen wie Risse und Schweißfehler enthalten. Zur Erstellung eines möglichst allgemeinen Leitfadens zur Testkörperherstellung für die Zuverlässigkeitsbewertung werden verschiedene Möglichkeiten betrachtet. Es wird ein Testkörpersatz mit Ersatzfehlern hergestellt und durch Testkörper mit realistischen Fehlstellen ergänzt. Mit Hilfe von Simulationen mit CIVA sollen die optimalen Konfigurationen und Anordnung von realistischen Fehlstellen und Ersatzfehlern identifiziert, und anschließend mithilfe geeigneter Fertigungsverfahren eingebracht und validiert werden. Neben den Testkörpern, die gezielt für das Vorhaben hergestellt werden, kommen außerdem kommerziell erhältliche Testkörpersätze mit realistischen Fehlstellen zum Einsatz. Die Prüfaussage einer Ultraschallprüfung hängt weiterhin wesentlich von den Informationen ab, die dem Prüfpersonal vor Ort zur Verfügung steht. Es muss ein ausgewogenes Maß zwischen zu wenig und zu viel Informationen gefunden werden. Im letzten Schritt wird deshalb eine geeignete Vorlage für eine Prüfanweisung erstellt, die so formuliert ist, dass die Wahrscheinlichkeit menschlicher Fehler (z. B. Missverständnis, Fehlinterpretation, Überspringen von Schritten usw.) möglichst gering ist. T2 - DGZfP Jahrestagung 2022 CY - Kassel, Germany DA - 23.05.2022 KW - Zuverlässigkeit KW - POD KW - Testkörper KW - Ultraschallprüfung PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560103 SP - 1 EP - 9 AN - OPUS4-56010 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kanzler, D. A1 - Rentala, V. K. A1 - Bertovic, Marija A1 - Heckel, Thomas A1 - Tkachenko, Viktoriya A1 - Given, Joseph A1 - Keßler, S. A1 - Dethof, F. A1 - Jüngert, A. A1 - Vrana, J. T1 - Lasst uns mal POD standardisieren! N2 - Seit beinahe 50 Jahren werden Zuverlässigkeitsbewertungen zerstörungsfreier Prüfverfahren erfolgreich in unterschiedlichen Industriebranchen eingesetzt. Dennoch gibt es weiterhin viele Vorbehalte, da die Bewertungsgrundlage nicht standardisiert ist und konkrete Handlungsanweisungen fehlen. Dem gegenüber steht die Anerkennung in der ZfP-Community. Es ist bisher nur Wenigen bekannt, dass dem Wissen über die Zuverlässigkeit eines zerstörungsfreien Prüfverfahren eineSchlüsselfunktion für die ZfP 4.0 zukommt. Im Vortrag wird die Notwendigkeit für eine Norm oder eine Richtlinie zum Thema Zuverlässigkeitsbewertungen aufgezeigt. Es wird darauf eingegangen, warum es bisher (in Deutschland) noch keine Richtlinie gab und gibt und was der:die Anwender:innen aus einer Richtlinie zur Zuverlässigkeitsbewertung von ZfP-Prüfverfahren erwarten kann. Es werden konkrete Schritte und Vorgehensweisen zur Bewertung der Zuverlässigkeit eines Verfahrens aufgezeigt; von der Definition eines Anwendungsfalls, über die Herstellung geeigneter Testkörper bis hin zur Durchführung und Bewertung von Prüfungen unter Einbeziehung von menschlichen Einflüssen. Die Beispiele umfassen sowohl Anwendungen aus dem Bauwesen als auch aus dem Maschinen- und Anlagenbau. Der Vortrag fasst die bisherigen und geplanten Arbeiten in dem WIPANO Projekt „Normung für die probabilistische Bewertung der Zuverlässigkeit für zerstörungsfreie Prüfverfahren“ zusammen. T2 - DGZfP Jahrestagung 2022 CY - Kassel, Germany DA - 23.05.2022 KW - Zuverlässigkeit KW - POD KW - Probability of detection KW - Reliability KW - Human Factors KW - Simulation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560113 SP - 1 EP - 10 AN - OPUS4-56011 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija A1 - Given, Joseph A1 - Lehleitner, Johannes T1 - First insights into the human-related risks of tunnel inspection N2 - Whereas human factors (HF) in the non-destructive testing (NDT) of metallic components are a poorly investigated topic (in comparison to other industrial fields such as aviation), HF in the inspection of concrete components are even less known. Studies have shown that there is always some variability between individuals in their inspection results and that HF affect the reliability of NDT inspections. The aim of the ongoing WIPANO project is to draft a standard for a holistic reliability assessment, with concrete inspection as one case study. This includes also the HF. A human-oriented Failure Modes and Effects Analysis (FMEA) was carried out to do the following: a) identify possible human-related risks in tunnel inspection processes using a laser scan method (including data collection,evaluation, and assessment of tunnel damage) and b) evaluate these human-related risks as regards their possible causes, consequences and probability of occurrence – in addition with respect to existing and possible preventive measures. The results show that the causes for possible failures can lie within people, the physical environment, technology, organisation, and extra-organisational environment. Whereas current preventive measures rely mostly on the individual and quality management practices, there is potential for even larger improvement at the organisational and extra-organisational level. The FMEA results were also used to develop a quantification method to further understand the HF in tunnel inspection, which could possibly be included in the information into the overall reliability assessment. The usage of qualitative and quantitative data collected through the human-FMEA within the proposed quantification method shows promise that HF can be quantified and could offer broader understanding of HF influences on inspection in various industries T2 - The International Symposium on Nondestructive Testing in Civil Engineering CY - Zurich, Switzerland DA - 16.08.2022 KW - Human Factors KW - Failure Modes and Effects Analysis KW - FMEA KW - Tunnel Inspection KW - NDT Reliability KW - Quantification PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560138 SP - 1 EP - 5 AN - OPUS4-56013 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 Cupriavidus campinensis Strain G5, 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 G5 was determined by PacBio sequencing. Using the TYGS for taxonomic classification, strain G5 was assigned to the species Cupriavidus campinensis. KW - Polyethylene KW - Cupriavidus campinensis KW - Plastic degradation KW - Genome sequence PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557897 DO - https://doi.org/10.1128/mra.00553-22 SP - 1 EP - 2 PB - ASM AN - OPUS4-55789 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 - Data preparation KW - Quality assurance KW - Process monitoring PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555063 DO - https://doi.org/10.3390/app12083955 SN - 2076-3417 VL - 12 IS - 8 SP - 1 EP - 13 PB - MDPI CY - Basel AN - OPUS4-55506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Claudia A1 - Asna Ashari, Parsa A1 - Mirtsch, Mona A1 - Blind, K. A1 - Castka, P. T1 - Impact of the COVID-19 pandemic on accredited conformity assessment bodies: insights from a multinational study N2 - The COVID-19 pandemic posed new and manifold challenges to organizations and their operations worldwide. Conformity assessment bodies (CABs), such as testing or medical laboratories, certification, and inspection bodies, were also affected by the associated disruptions. Their role in this crisis is highly relevant, as CABs are essential pillars of the quality infrastructure: their activities ensure that products and services meet requirements as defined in standards and regulations, thereby contributing to their safety and reliability. The question arises of how CABs and their operations were affected by the pandemic and how they responded. To this end, we present the results of an international survey of 986 CABs of all types in Germany, the UK, Italy, and New Zealand. Overall, CABs reported, on average, a reduction in demand for their services during the pandemic, facing restrictions in all countries. In addition, the pandemic had an overall negative impact on the CABs’ investment and innovation activities. However, investments in digital infrastructure were increased as a countermeasure, with CABs reporting a higher need for digitalization. The paper highlights and discusses results from in-depth analyses relevant to policymakers and industry alike. KW - Quality Infrastructure KW - Digitalization KW - Testing laboratories KW - Conformity assessment KW - Certification KW - Conformity assessment body KW - Corona KW - Covid-19 KW - Resilience PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556396 DO - https://doi.org/10.1007/s00769-022-01514-x SP - 1 EP - 14 PB - Springer AN - OPUS4-55639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Straße, Anne A1 - Bakir, Nasim A1 - Gumenyuk, Andrey A1 - Rethmeier, Michael ED - Schmidt, M. ED - Vollertsen, F. ED - Schmidt, B. M. T1 - Preliminary study to investigate the applicability of optical strain measurement technique for the detection of hot cracks in laser metal deposited layers N2 - Laser metal deposition (LMD) as an additive manufacturing technique became increasingly important in recent years and thus the demand for component safety. This is the reason, for the need for reliable in-situ defect detection techniques. For laser beam weld seams an optical measurement technique based on an optical flow algorithm was successfully used to define the critical straining conditions that lead to hot cracking. This algorithm was adapted for bead-on-plate weld seams on LMD deposited layers of IN718 alloy while performing external strain on the specimen in an externally loaded hot cacking test facility. The resulting transversal hot cracks along the weld seam were localized via X-Ray inspection and the type of cracking confirmed by Scanning Electron Microscopy (SEM). The strain distribution was measured in the vicinity of the solidification front and correlated to the detected hot cracks. Based on the results this technique could be adopted for LMD experiments. T2 - 12th CIRP Conference on Photonic Technologies [LANE 2022] CY - Fürth, Germany DA - 04.09.2022 KW - Laser Metal Deposition (LMD) KW - Strain measurement KW - Optical flow KW - Critical strain PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556445 DO - https://doi.org/10.1016/j.procir.2022.08.034 VL - 111 SP - 335 EP - 339 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-55644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Solberg, S. A1 - Zimmermann, P. A1 - Wilhelmsen, Ø. A1 - Lamb, J. A1 - Bock, Robert A1 - Burheim, O. T1 - Heat to Hydrogen by Reverse Electrodialysis—Using a Non-Equilibrium Thermodynamics Model to Evaluate Hydrogen Production Concepts Utilising Waste Heat N2 - The reverse electrodialysis heat engine (REDHE) is a promising salinity gradient energy technology, capable of producing hydrogen with an input of waste heat at temperatures below 100 °C. A salinity gradient drives water electrolysis in the reverse electrodialysis (RED) cell, and spent solutions are regenerated using waste heat in a precipitation or evaporation unit. This work presents a non-equilibrium thermodynamics model for the RED cell, and the hydrogen production is investigated for KCl/water solutions. The results show that the evaporation concept requires 40 times less waste heat and produces three times more hydrogen than the precipitation concept. With commercial evaporation technology, a system efficiency of 2% is obtained, with a hydrogen production rate of 0.38 gH2 m−2h−1 and a waste heat requirement of 1.7 kWh g−1H2. The water transference coefficient and the salt diffusion coefficient are identified as membrane properties with a large negative impact on hydrogen production and system efficiency. Each unit of the water transference coefficient in the range tw=[0–10] causes a −7 mV decrease in unit cell electric potential, and a −0.3% decrease in system efficiency. Increasing the membrane salt diffusion coefficient from 10−12 to 10−11 leads to the system efficiency decreasing from 2% to 0.6% KW - Non-equilibrium thermodynamics KW - Hydrogen KW - Waste heat KW - RED PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556677 DO - https://doi.org/10.3390/en15166011 VL - 15 IS - 16 SP - 6011 PB - MDPI AN - OPUS4-55667 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bruno, Giovanni A1 - Maierhofer, Christiane T1 - Advanced Characterization and On-Line Process Monitoring of Additively Manufactured Materials and Components N2 - Additive manufacturing (AM) techniques have risen to prominence in many industrial sectors. This rapid success of AM is due to the freeform design, which offers enormous possibilities to the engineer, and to the reduction of waste material, which has both environmental and economic advantages. Even safety-critical parts are now being produced using AM. This enthusiastic penetration of AM in our daily life is not yet paralleled by a thorough characterization and understanding of the microstructure of materials and of the internal stresses of parts. The same holds for the understanding of the formation of defects during manufacturing. While simulation efforts are sprouting and some experimental techniques for on-line monitoring are available, still little is known about the propagation of defects throughout the life of a component (from powder to operando/service conditions). This Issue was aimed at collecting contributions about the advanced characterization of AM materials and components (especially at large-scale experimental facilities such as Synchrotron and Neutron sources), as well as efforts to liaise on-line process monitoring to the final product, and even to the component during operation. The goal was to give an overview of advances in the understanding of the impacts of microstructure and defects on component performance and life at several length scales of both defects and parts. KW - Non-destructive Testing KW - Additive Manufacturing KW - Materials Characterization KW - Online Monitoring KW - Residual Stress KW - Thermography KW - Computed Tomography PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556833 DO - https://doi.org/10.3390/met12091498 VL - 12 IS - 9 SP - 1 EP - 3 PB - MDPI CY - Basel, Schweiz AN - OPUS4-55683 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bruno, Giovanni T1 - Micro Non-Destructive Testing and Evaluation N2 - What is meant by ‘Micro Non-Destructive Testing and Evaluation’? This was the central subject of debate in this Special Issue. At present, sub-millimeter-size components or even assemblies are pervading the industrial and scientific world. Classic examples are electronic devices and watches (as well as parts thereof), but recent examples encompass additively manufactured lattice structures, stents, or other microparts. Moreover, most assemblies contain micro-components. Testing such components or their miniaturized parts would fit well within the topic of micro non-destructive testing and evaluation. In all cases, performance and integrity testing, quality control, and dimensional tolerances need to be measured at the sub-millimeter level (ideally with a spatial resolution of about a micron); most of the time, such features and components are embedded in much larger assemblies, which also need to be taken into account. The solution to this dilemma (i.e. measuring large parts with high resolution) depends on the part and on the problem under consideration. Another possible definition of micro non-destructive testing and evaluation can relate to the characterization of micro-features (e.g., the microstructure) in much larger specimens, such as damage in concrete cores or porosity in additively manufactured components. A further aspect is the use of microscopic probes to evaluate macroscopic properties. This is the case, for instance but not at all exclusively, in the use of diffraction techniques to determine macroscopic stress. The splits between testing and characterization at the micro-level (or of micro parts) from one side and handling of macroscopic assemblies on the other represent a great challenge for many fields of materials characterization. On top of that, including the use of microscopic methods to test integrity would add a further level of complexity. Imaging, mechanical testing, non-destructive testing, measurement of properties, structural health monitoring, and dimensional metrology all need to be re-defined if we want to cope with the multi-faceted topic of micro non-destructive testing and evaluation. The challenge has already been accepted by the scientific and engineering communities for a while but is still far from being universally tackled. This Special Issue yields an interesting answer to the questions posed above. It presents the progress made and the different aspects of the challenge as well as at indicates the paths for the future of NDT&E. KW - Ultrasound KW - Materials Characterization KW - Residual Stress KW - Thermography Computed KW - Tomography KW - Non-destructive Testing KW - Magnetic Methods PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556849 DO - https://doi.org/10.3390/ma15175923 VL - 15 IS - 17 SP - 1 EP - 3 PB - MDPI CY - Basel, Schweiz AN - OPUS4-55684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Falahat, A M A1 - Kardjilov, N A1 - Woracek, R A1 - Boin, M A1 - Markötter, Henning A1 - Kuhn, L T A1 - Makowska, M A1 - Strobl, M A1 - Pfretzschner, B A1 - Banhart, J A1 - Manke, I T1 - Temperature dependence in Bragg edge neutron transmission measurements N2 - A systematic study has been carried out to investigate the neutron transmission signal as a function of sample temperature. In particular, the experimentally determined wavelength-dependent neutron attenuation spectra for a martensitic steel at temperatures ranging from 21 to 700°C are compared with simulated data. A theoretical description that includes the Debye–Waller factor in order to describe the temperature influence on the neutron cross sections was implemented in the nxsPlotter software and used for the simulations. The analysis of the attenuation coefficients at varying temperatures shows that the missing contributions due to elastic and inelastic scattering can be clearly distinguished: while the elastically scattered intensities decrease with higher temperatures, the inelastically scattered intensities increase, and the two can be separated from each other by analysing unique sharp features in the form of Bragg edges. This study presents the first systematic approach to quantify this effect and can serve as a basis , for example, to correct measurements taken during in situ heat treatments, in many cases being a prerequisite for obtaining quantifiable results. KW - Neutron Bragg edge imaging KW - Debye–Waller factor KW - Temperature-dependent neutron transmission KW - Super martensitic stainless steel PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556896 DO - https://doi.org/10.1107/S1600576722006549 VL - 55 IS - Pt 4 SP - 919 EP - 928 PB - International Union of Crystallography AN - OPUS4-55689 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markötter, Henning A1 - Sintschuk, Michael A1 - Britzke, Ralf A1 - Dayani, Shahabeddin A1 - Bruno, Giovanni T1 - Upgraded imaging capabilities at the BAMline (BESSY II) N2 - The BAMline at the BESSY II synchrotron X-ray source has enabled research for more than 20 years in widely spread research fields such as materials science, biology, cultural heritage and medicine. As a nondestructive characterization method, synchrotron X-ray imaging, especially tomography, plays a particularly important role in structural characterization. A recent upgrade of key equipment of the BAMline widens its imaging capabilities: shorter scan acquisition times are now possible, in situ and operando studies can now be routinely performed, and different energy spectra can easily be set up. In fact, the upgraded double-multilayer monochromator brings full flexibility by yielding different energy spectra to optimize flux and energy resolution as desired. The upgraded detector (based on an sCMOS camera) also allows exploiting the higher flux with reduced readout times. Furthermore, an installed slip ring allows the sample stage to continuously rotate. The latter feature enables tomographic observation of processes occurring in the time scale of a few seconds. KW - Synchrotron radiation KW - Computed tomography KW - Double-multilayer monochromators KW - Pink beams KW - X-ray optics PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556907 DO - https://doi.org/10.1107/S1600577522007342 SN - 1600-5775 VL - 29 IS - Pt 5 SP - 1292 EP - 1298 PB - International Union of Crystallography CY - Chester AN - OPUS4-55690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cestari, F. A1 - Yang, Y. A1 - Wilbig, Janka A1 - Günster, Jens A1 - Motta, A. A1 - Sglavo, V. T1 - Powder 3D printing of bone scaffolds with uniform and gradient pore sizes using cuttlebone-derived calcium phosphate and glass-ceramic N2 - The pore geometry of bone scaffolds has a major impact on their cellular response; for this reason, 3D printing is an attractive technology for bone tissue engineering, as it allows for the full control and design of the porosity. Calcium phosphate materials synthesized from natural sources have recently attracted a certain interest because of their similarity to natural bone, and they were found to show better bioactivity than synthetic compounds. Nevertheless, these materials are very challenging to be processed by 3D printing due to technological issues related to their nanometric size. In this work, bone scaffolds with different pore geometries, with a uniform size or with a size gradient, were fabricated by binder jetting 3D printing using a biphasic calcium phosphate (BCP) nanopowder derived from cuttlebones. To do so, the nanopowder was mixed with a glass-ceramic powder with a larger particle size (45–100 µm) in 1:10 weight proportions. Pure AP40mod scaffolds were also printed. The sintered scaffolds were shown to be composed mainly by hydroxyapatite (HA) and wollastonite, with the amount of HA being larger when the nanopowder was added because BCP transforms into HA during sintering at 1150 ◦C. The addition of bio-derived powder increases the porosity from 60% to 70%, with this indicating that the nanoparticles slow down the glass-ceramic densification. Human mesenchymal stem cells were seeded on the scaffolds to test the bioactivity in vitro. The cells’ number and metabolic activity were analyzed after 3, 5 and 10 days of culturing. The cellular behavior was found to be very similar for samples with different pore geometries and compositions. However, while the cell number was constantly increasing, the metabolic activity on the scaffolds with gradient pores and cuttlebone-derived powder decreased over time, which might be a sign of cell differentiation. Generally, all scaffolds promoted fast cell adhesion and proliferation, which were found to penetrate and colonize the 3D porous structure. KW - Bioactivity KW - Cuttlefish KW - Biphasic calcium phosphate KW - Binder jetting KW - Scaffold geometry KW - Hausner ratio PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553627 DO - https://doi.org/10.3390/ma15155139 SN - 1996-1944 VL - 15 IS - 15 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-55362 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Matthias A1 - Mauch, Tatjana A1 - Riedel, Juliane T1 - Development of a Hydrazine-Based Solid-Phase Extraction and Clean-Up Method for Highly Selective Quantification of Zearalenone in Edible Vegetable Oils by HPLC-FLD N2 - Rapid, cost-efficient, and eco-friendly methods are desired today for routine analysis of the Fusarium mycotoxin zearalenone (ZEN) in edible vegetable oils. Liquid chromatography with fluorescence detection (HPLC-FLD) is commonly used to reliably control the specified ZEN maximum levels, which requires efficient sample clean-up to avoid matrix interferences. Therefore, a highly selective extraction and clean-up method based on reversible covalent hydrazine chemistry (RCHC) using hydrazine-functionalized silica was developed. This efficient solid-phase extraction (SPE) involves reversible hydrazone formation of ZEN with the hydrazine moiety covalently bound to a solid phase. Optimal conditions were achieved with 1 mL SPE cartridges filled with 400 mg of hydrazine-functionalized silica. The developed RCHC-SPE method was validated in an interlaboratory comparison study (ILC) with twelve participants analyzing six edible vegetable oils with a focus on maize oils. The derived method parameters (ZEN recovery 83%, repeatability 7.0%, and reproducibility 18%) meet the performance criteria of Commission Regulation (EC) No 401/2006. The developed RCHC-SPE-based HPLC-FLD method allows the reliable quantification of ZEN in the range of 47–494 μg/kg for different types of edible vegetable oils, also for matrix-reach native oils. Due to the high efficiency, the significantly reduced matrix load helps to extend the lifetime of analytical equipment. Furthermore, the re-useability of the RCHC-SPE cartridges contributes to an eco-friendly approach and reduced analysis costs. To our knowledge, this is the first report on ZEN quantification in edible vegetable oils based on manual RCHC-SPE cartridges. Due to its high performance, the developed RCHC-SPE method is a promising alternative to the current European standard method EN 16924:2017 (HPLC-FLD part). KW - Mycotoxin KW - Food KW - Reversible covalent hydrazine chemistry (RCHC) KW - Quantitative determination PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554812 DO - https://doi.org/10.3390/toxins14080549 VL - 14 IS - 8 PB - MDPI CY - Basel AN - OPUS4-55481 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mani, Deepak A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Diffraction Enhanced Imaging Analysis with Pseudo-Voigt Fit Function N2 - Diffraction enhanced imaging (DEI) is an advanced digital radiographic imaging technique employing the refraction of X-rays to contrast internal interfaces. This study aims at qualitatively and quantitatively evaluating images acquired using this technique and to assess how different fitting functions to the typical rocking curves (RCs) influence the quality of images. RCs are obtained for every image pixel. This allows the separate determination of the absorption and the refraction properties of the material in a position-sensitive manner. Comparison of various types of fitting functions reveals that the Pseudo-Voigt (PsdV) function is best suited to fit typical RCs. A robust algorithm was developed in the Python programming language, which reliably extracts the physically meaningful information from each pixel of the image. We demonstrate the potential of the algorithm with two specimens: a silicone gel specimen that has well-defined interfaces, and an additively manufactured polycarbonate specimen. KW - Diffraction Enhanced Imaging KW - Analyzer-Based Imaging KW - X-ray refraction KW - Non-Destructive Evaluation KW - Pseudo-Voigt fit function KW - Python PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553791 DO - https://doi.org/10.3390/jimaging8080206 SN - 2313-433X VL - 8 IS - 8 SP - 1 EP - 13 PB - MDPI CY - Basel, Switzerland AN - OPUS4-55379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Spitzer, Stefan A1 - Askar, Enis A1 - Hecht, Kristin A1 - Gabel, D. A1 - Zakel, S. A1 - Krietsch, Arne T1 - Requirements for a Hybrid Dust-Gas-Standard: Influence of the Mixing Procedure on Safety Characteristics of Hybrid Mixtures N2 - While developing a standard for the determination of safety characteristics for hybrid mixtures the authors discovered, that, beside the ignition source, the mixing procedure is the main difference between the single-phase standards for dusts and gases. The preparation of hybrid mixtures containing a flammable gas and a flammable dust in the 20 L-sphere can be realized in different ways. Either the flammable gas is filled only in the sphere or only in the dust container or in both. In previous works, almost always the first method is applied, without giving any information on the accuracy of the gas mixtures. In this work the accuracy of the gas mixtures and the results of the tests applying two methods of mixing were studied. No significant influence of the mixing method itself on the safety characteristics explosion pressure pex and the normalized rate of pressure rise (K-value) was found. Obviously, homogenization of the gas mixtures can be obtained sufficiently by the turbulence that is caused during the injection from the dust container into the explosion chamber within a short time. However, the mixing procedure has a great influence on the accuracy of the gas amount of the mixtures obtained. Without modifying the 20 L-sphere by installing precise pressure sensors, assuring its tightness and performing gas analysis, it must be expected, that the accuracy of the gas mixtures is very low. This has a significant influence on the measured safety characteristics and may lead to unsafe facilities or unnecessary expensive safety measures. KW - Hybrid mixtures KW - 20 L-sphere KW - Pre-ignition pressure rise KW - Post-injection pressure drop KW - Safety characteristics PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554610 DO - https://doi.org/10.3390/fire5040113 VL - 5 IS - 4 SP - 1 EP - 10 PB - MDPI CY - Basel AN - OPUS4-55461 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thuy, Maximilian A1 - Niebergall, Ute A1 - Oehler, H. A1 - Alig, I. A1 - Böhning, Martin T1 - Damaging effect of admixtures used in crop protection products on high density polyethylene packaging material N2 - The phenomenon of environmental stress cracking is still a major issue in materials engineering as well as from a scientific perspective. Especially in the case of packaging materials made of high-density polyethylene, assessing the potential of premature damage due to environmental stress cracking is complex because of the large number of components in possible liquid filling goods. As a first guideline, the well-known effect of detergents and dispersants is usually considered, but the interplay with other components, such as organic solvents is often unknown. Particularly challenging in this respect are crop protection products, consisting of several different admixtures in addition to the biologically active ingredients. This study is based on two model liquids representing these admixtures that were established for testing in this context. The model liquids as well as their constituting components were used as liquid media in the Full Notch Creep Test to characterize the environmental stress cracking behavior of a typical high-density polyethylene. Complementary to the time-to failure of a notched specimen obtained from these tests, the crack opening was monitored optically, and the fracture surface was analyzed post-failure by laser scanning microscopy as well as scanning electron microscopy. Based on the results, the effect of various surfactants as well as the influence of organic solvents on environmental stress cracking are discussed. KW - Environmental stress cracking KW - High-density polyethylene KW - Crop protection products KW - Full notch creep test KW - Fracture surface analysis KW - Crack opening displacement PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554631 DO - https://doi.org/10.1016/j.polymertesting.2022.107672 SN - 0142-9418 VL - 114 SP - 1 EP - 16 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-55463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Knoche, Lisa A1 - Lisec, Jan A1 - Koch, Matthias T1 - Analysis of electrochemical and liver microsomal transformation products of lasalocid by LC/HRMS N2 - Rationale: Lasalocid (LAS), an ionophore, is used in cattle and poultry farming as feed additive for its antibiotic and growth-promoting properties. Literature on transformation products (TP) resulting from LAS degradation is limited. So far, only hydroxylation is found to occur as the metabolic reaction during the LAS degradation. To investigate potential TPs of LAS, we used electrochemistry (EC) and liver microsome (LM) assays to synthesize TPs, which were identified using liquid chromatography high-resolution mass spectrometry (LC/HRMS). Methods: Electrochemically produced TPs were analyzed online by direct coupling of the electrochemical cell to the electrospray ionization (ESI) source of a Sciex Triple-TOF high resolution mass spectrometer. Then, EC-treated LAS solution was collected and analyzed offline using LC/HRMS to confirm stable TPs and improve their annotation with a chemical structure due to informative MS/MS spectra. In a complementary approach, TPs formed by rat and human microsomal incubation were investigated using LC/HRMS. The resulting data were used to investigate LAS modification reactions and elucidate the chemical structure of obtained TPs. Results: The online measurements identified a broad variety of TPs, resulting from modification reactions like (de-)hydrogenation, hydration, methylation, oxidation as well as adduct formation with methanol. We consistently observed different ion complexations of LAS and LAS-TPs (Na+; 2Na+ K+; NaNH4 +; KNH4 +). Two stable methylated EC-TPs were found, structurally annotated, and assigned to a likely modification reaction. Using LM incubation, seven TPs were formed, mostly by oxidation/hydroxylation. After the identification of LM-TPs as Na+-complexes, we identified LM-TPs as K+-complexes. Conclusion: We identified and characterized TPs of LAS using EC- and LM-based methods. Moreover, we found different ion complexes of LAS-based TPs. This knowledge, especially the different ion complexes, may help elucidate the metabolic and environmental degradation pathways of LAS. KW - Mass Spectrometry KW - Electrochemistry KW - ECR KW - Lasalocid KW - Ionophore KW - Transformation products PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553919 DO - https://doi.org/10.1002/rcm.9349 VL - 36 IS - 18 SP - 1 EP - 10 PB - Wiley online library AN - OPUS4-55391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shapovalov, O. A1 - Heckel, Thomas A1 - Gaal, Mate A1 - Weiß, S. T1 - External Acoustical Damping on a Metallic Angle Wedge in a High Temperature Resistant Ultrasonic Probe N2 - Ultrasonic probes for high-temperature applications are provided with metallic wedges, which can withstand the contact with the high temperature of the inspected structure. The ultrasonic signal travels within the wedge and gets reflected from its boundaries, causing interference signals called “ghost echoes”. The current work presents an investigation of the additional damping effect provided by porous sintered metal plates applied onto the surface of the wedge. In particular, the study evaluates the effect of damping plate thickness on the interference signal level at different transmission frequencies. Damping plates made of sintered metal SIKA-R 15 AX were attached to a wedge prototype made of steel 1.4301. The study revealed, that the most effective thickness of damping plates in the selected frequency interval of 1 to 4 MHz is equal to 4 mm. The evaluation of the interference signal has shown that the application of such damping plates to the wedge surface contributes to an additional attenuation of an interference signal of 10 to 30 dB after 500 μs of signal propagation. KW - Ultrasonic testing KW - High temperature KW - Acoustical damping KW - Angle wedge KW - Ultrasonic probe PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553920 DO - https://doi.org/10.1007/s40857-022-00270-9 SN - 0814-6039 SP - 1 EP - 11 PB - Springer AN - OPUS4-55392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scharf-Wildenhain, R. A1 - Hälsig, A. A1 - Hensel, J. A1 - Wandtke, Karsten A1 - Schröpfer, Dirk A1 - Kromm, Arne A1 - Kannengießer, Thomas T1 - Influence of Heat Control on Properties and Residual Stresses of Additive-Welded High-Strength Steel Components N2 - This contributed to the knowledge regarding the safe avoidance of cold cracking. In addition to a thermophysical simulation using a dilatometer of different high-strength steels with subsequent tensile testing, reference WAAM specimens (open hollow cuboids) were welded while utilizing a high-strength filler metal (ultimate tensile strength > 790 MPa). The heat control was varied by means of the heat input and interlayer temperature such that the Dt8/5 cooling times corresponded to the recommended processing range (approx. 5 s to 20 s). For the heat input, significant effects were exhibited, in particular on the local residual stresses in the component. Welding with an excessive heat input or deposition rate may lead to low cooling rates, and hence to unfavorable microstructure and component properties, but at the same time, is intended to result in lower tensile residual stress levels. Such complex interactions must ultimately be clarified to provide users with easily applicable processing recommendations and standard specifications for an economical WAAM of high-strength steels. These investigations demonstrated a major influence of the heat input on both the cooling conditions and the residual stresses of components manufactured withWAAM using high-strength filler materials. A higher heat input led to longer cooling times (Dt8/5) and approx. 200 MPa lower residual stresses in the surface of the top layer. KW - WAAM KW - Additive manufacturing KW - Heat control KW - High-strength filler metals KW - Residual stress PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553982 UR - https://www.mdpi.com/2075-4701/12/6/951 DO - https://doi.org/10.3390/met12060951 VL - 12 IS - 6 SP - 951 PB - MDPI AN - OPUS4-55398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Tim A1 - Delgado Arroyo, Diego A1 - Börner, Andreas A1 - Schröpfer, Dirk A1 - Rhode, Michael A1 - Lindner, T. A1 - Löbel, M. A1 - Preuß, B. A1 - Lampke, T. T1 - Ultrasonic assisted milling of a CoCrFeNi medium entropy alloy N2 - Medium and High Entropy Alloys (MEA/HEA) are recently developed material classes, providing manifold applications, e.g., due to extraordinary structural properties. In that connection, the machinability as important issue for the processing of these materials was not in the scientific focus. This study focusses on experimental analysis of milling process conditions including ultrasonic assisted milling (USAM) and their effects on the resulting surface integrity of equiatomic CoCrFeNi-MEA specimens. For that reason, milling parameters (cutting speed, feed per cutting edge) were systematically varied for both conventional milling and USAM. The surface integrity was analyzed in terms of topography, defects, and residual stresses. Especially USAM leads to a decrease of occurring cutting forces and, hence, to an improvement of the surface integrity. Beneficial effects were observed in terms of lower tensile residual stresses at high cutting speed and feed per cutting edge. KW - Medium entropy alloy KW - Ultrasonic Assisted Machining KW - Surface Integrity PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554458 DO - https://doi.org/10.1016/j.procir.2022.05.203 VL - 108 SP - 879 EP - 884 PB - Elsevier B.V. AN - OPUS4-55445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Binder, F. A1 - Bircher, B. A1 - Laquai, René A1 - Küng, A. A1 - Bellon, Carsten A1 - Meli, F. A1 - Deresch, A. A1 - Ulrich Neuschaefer-Rube, U. A1 - Hausotte, T. T1 - Methodologies for model parameterization of virtual CTs for measurement uncertainty estimation N2 - X-ray computed tomography (XCT) is a fast-growing technology for dimensional measurements in industrial applications. However, traceable and efficient methods to determine measurement uncertainties are not available. Guidelines like the VDI/VDE 2630 Part 2.1 suggest at least 20 repetitions of a specific measurement task, which is not feasible for industrial standards. Simulation-based approaches to determine task specific measurement uncertainties are promising, but require closely adjusted model parameters and an integration of error sources like geometrical deviations during a measurement. Unfortunately, the development of an automated process to parameterize and integrate geometrical deviations into XCT models is still an open issue. In this work, the whole processing chain of dimensional XCT measurements is taken into account with focus on the issues and requirements to determine suitable parameters of geometrical deviations. Starting off with baseline simulations of different XCT systems, two approaches are investigated to determine and integrate geometrical deviations of reference measurements. The first approach tries to iteratively estimate geometric deviation parameter values to match the characteristics of the missing error sources. The second approach estimates those values based on radiographs of a known calibrated reference object. In contrast to prior work both approaches only use a condensed set of parameters to map geometric deviations. In case of the iterative approach, some major issues regarding unhandled directional dependencies have been identified and discussed. Whereas the radiographic method resulted in task specific expanded measurements uncertainties below one micrometre even for bi-directional features, which is a step closer towards a true digital twin for uncertainty estimations in dimensional XCT. KW - Geometrical deviation KW - X-ray computed tomography KW - Uncertainty estimation KW - Virtual CT PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553263 DO - https://doi.org/10.1088/1361-6501/ac7b6a VL - 33 IS - 10 SP - 1 EP - 15 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-55326 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eissel, A. A1 - Engelking, Lorenz A1 - Treutler, K. A1 - Wesling, V. A1 - Schröpfer, Dirk A1 - Kannengießer, Thomas T1 - Modification of Co–Cr alloys to optimize additively welded microstructures and subsequent surface finishing N2 - Cobalt chromium alloys are often used in turbine and plant construction. This is based on their high thermal and mechanical stress resistance as well as their high wear resistance to corrosive and abrasive loads. However, cobalt is a cost-intensive material that is difficult to machine. Moreover, increasingly complex structures and the optimisation of resource efficiency also require additive manufacturing steps for the production or repair of components in many sectors. 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. As a result of the high stresses on the components and requirements for a high surface quality, a complementary use of additive and machining manufacturing processes is necessary. Thereby, Co–Cr alloys are extremely challenging for machining with geometrically defined cutting edges because of their low thermal conductivity combined with high strength and toughness. An approach to solve this problem is to refine and homogenise the microstructure. This is achieved by modifying the alloy with elements zirconium and hafnium, which are added up to a maximum of 1 wt.-%. A reduction of the process forces and stresses on the tool and work piece surface is also achievable via hybrid milling processes. There are already studies on the combined use of additive and machining manufacturing processes based on laser technology. However, knowledge based on powder and wire-based arc processes is important, as these processes are more widespread. Furthermore, the effects on the surface zone of additively manufactured components by hybrid finish milling have not yet been a subject of research. The results show that the structural morphology could be significantly influenced with the addition of zirconium and hafnium. KW - Alloy modification KW - Ultrasonic-assisted milling KW - Plasma-transferred arc welding KW - Co-Cr-alloy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554182 DO - https://doi.org/10.1007/s40194-022-01334-0 SN - 0043-2288 SN - 1878-6669 SP - 1 EP - 13 PB - Springer CY - Heidelberg AN - OPUS4-55418 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Völker, Tobias T1 - Intrinsic Performance of Monte Carlo Calibration-Free Algorithm for Laser-Induced Breakdown Spectroscopy N2 - The performance of the Monte Carlo (MC) algorithm for calibration-free LIBS was studied on the example of a simulated spectrum that mimics a metallurgical slag sample. The underlying model is that of a uniform, isothermal, and stationary plasma in local thermodynamical equilibrium. Based on the model, the algorithm generates from hundreds of thousands to several millions of simultaneous configurations of plasma parameters and the corresponding number of spectra. The parameters are temperature, plasma size, and concentrations of species. They are iterated until a cost function, which indicates a difference between synthetic and simulated slag spectra, reaches its minimum. After finding the minimum, the concentrations of species are read from the model and compared to the certified values. The algorithm is parallelized on a graphical processing unit (GPU) to reduce computational time. The minimization of the cost function takes several minutes on the GPU NVIDIA Tesla K40 card and depends on the number of elements to be iterated. The intrinsic accuracy of the MC calibration-free method is found to be around 1% for the eight elements tested. For a real experimental spectrum, however, the efficiency may turn out to be worse due to the idealistic nature of the model, as well as incorrectly chosen experimental conditions. Factors influencing the performance of the method are discussed. KW - Laser induced breakdown spectroscopy KW - Calibration-free analysis KW - Monte Carlo algorithm PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-558016 DO - https://doi.org/10.3390/s22197149 VL - 22 IS - 19 SP - 7149 PB - MDPI AN - OPUS4-55801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Tobias A1 - Gornushkin, Igor B. T1 - Importance of physical units in the Boltzmann plot method N2 - The Boltzmann plot is one of the most widely used methods for determining the temperature in different types of laboratory plasmas. It operates on the logarithm as a function of the dimensional argument, which assumes that the correct physical units are used. In many works using the Boltzmann method, there is no analysis of the dimension of this argument, which may be the cause of a potential error. This technical note offers a brief description of the method and shows how to correctly use physical units when using transcendental functions like the logarithm. KW - Boltzmann plot KW - Laser induced plasma PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-558039 DO - https://doi.org/10.1039/d2ja00241h SP - 1 EP - 3 PB - Royal Society of Chemistry AN - OPUS4-55803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Deumer, J. A1 - Pauw, Brian Richard A1 - Marguet, S. A1 - Skroblin, D. A1 - Taché, O. A1 - Krumrey, M. A1 - Gollwitzer, C. T1 - Small-angle X-ray scattering: characterization of cubic Au nanoparticles using Debye’s scattering formula N2 - A versatile software package in the form of a Python extension, named CDEF (computing Debye’s scattering formula for extraordinary form factors), is proposed to calculate approximate scattering profiles of arbitrarily shaped nanoparticles for small-angle X-ray scattering (SAXS). CDEF generates a quasi-randomly distributed point cloud in the desired particle shape and then applies the open-source software DEBYER for efficient evaluation of Debye’s scattering formula to calculate the SAXS pattern (https://github.com/j-from-b/CDEF). If self-correlation of the scattering signal is not omitted, the quasi-random distribution provides faster convergence compared with a true-random distribution of the scatterers, especially at higher momentum transfer. The usage of the software is demonstrated for the evaluation of scattering data of Au nanocubes with rounded edges, which were measured at the four-crystal monochromator beamline of PTB at the synchrotron radiation facility BESSY II in Berlin. The implementation is fast enough to run on a single desktop computer and perform model fits within minutes. The accuracy of the method was analyzed by comparison with analytically known form factors and verified with another implementation, the SPONGE, based on a similar principle with fewer approximations. Additionally, the SPONGE coupled to McSAS3 allows one to retrieve information on the uncertainty of the size distribution using a Monte Carlo uncertainty estimation algorithm. KW - X-ray scattering KW - SAXS KW - Non-spherical nanoparticles KW - Nanoparticles KW - Nanomaterials KW - Debye scattering equation KW - Simulation KW - Data fitting PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557652 DO - https://doi.org/10.1107/S160057672200499X VL - 55 IS - Pt 4 SP - 993 EP - 1001 PB - International Union of Crystallography CY - Chester, England AN - OPUS4-55765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bachmann, Marcel A1 - Meng, Xiangmeng A1 - Artinov, Antoni A1 - Rethmeier, Michael T1 - Evaluation of narrowed weld pool shapes and their effect on resulting potential defects during deep penetration laser beam welding N2 - This study presents mechanisms of the evolution of a narrowed region in the weld pool center during deep penetration laser beam welding. In numerous numerical studies presented in this study, it was also found that the local reduction of the weld pool size can cause detrimental effects on the melt flow behavior and the resulting properties of the welds. A particularly large influence of this effect was identified in three aspects. First, the local variation of the solidification sequence of the weld pool causes an increase in the hot-cracking susceptibility due to a locally delayed solidification. Second, it was proven that a change in the local length and width of the weld pool is associated with an adverse impact on the potential flow routes of the molten material that induces stronger local variations of its solidification. Thus, the element mixing, e.g., during the welding with filler materials, is blocked. This leads to a non-homogeneous chemical composition of the final weld and can cause undesired effects on the final material properties. Finally, another observed effect is related to the reduced ability of process pores to reach the top surface. As this type of porosity is usually produced around the keyhole tip, the change of the fluid flow regime above this area plays a significant role in determining the final path of the pores until the premature solidification in the middle of the weld pool captures them. This study summarizes mainly numerical results that were supported by selected experimental validation results. KW - Weld pool shape KW - Laser beam welding KW - Solidification KW - Porosity KW - Numerical process simulation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557759 DO - https://doi.org/10.2351/7.0000733 SN - 1042-346X VL - 34 IS - 4 SP - 1 EP - 7 PB - Laser Institute of America CY - Orlando, Fla. AN - OPUS4-55775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gluth, Gregor A1 - Grengg, C. A1 - Ukrainczyk, N. A1 - Mittermayr, F. A1 - Dietzel, M. T1 - Acid resistance of alkali-activated materials: Recent advances and research needs N2 - Cementitious materials are frequently applied in environments in which they are exposed to acid attack, e.g., in sewer systems, biogas plants, and agricultural/food-related industries. Alkali-activated materials (AAMs) have repeatedly been shown to exhibit a remarkably high resistance against attack by organic and inorganic acids and, thus, are promising candidates for the construction and the repair of acid-exposed structures. However, the reaction mechanisms and processes affecting the acid resistance of AAMs have just recently begun to be understood in more detail. The present contribution synthesises these advances and outlines potentially fruitful avenues of research. The interaction between AAMs and acids proceeds in a multistep process wherein different aspects of deterioration extend to different depths, complicating the overall determination of acid resistance. Partly due to this indistinct definition of the ‘depth of corrosion’, the effects of the composition of AAMs on their acid resistance cannot be unambiguously identified to date. Important parallels exist between the deterioration of low-Ca AAMs and the weathering/corrosion of minerals and glasses (dissolution-reprecipitation mechanism). Additional research requirements relate to the deterioration mechanism of high-Ca AAMs; how the character of the corroded layer influences the rate of deterioration; the effects of shrinkage and the bond between AAMs and substrates. KW - Alkali-activated materials KW - Acid attack KW - Acid resistance KW - Concrete repair KW - MIC PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557376 DO - https://doi.org/10.21809/rilemtechlett.2022.157 SN - 2518-0231 VL - 7 SP - 58 EP - 67 PB - RILEM Publications SARL CY - Paris AN - OPUS4-55737 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jauregui-Correa, J. C. A1 - Morales-Velazquez, L. A1 - Otremba, Frank A1 - Hurtado-Hurtado, G. T1 - Method for predicting dynamic loads for a health monitoring system for subway tracks N2 - This paper presents a method for processing acceleration data registered on a train and determining the health condition of a subway’s substructure. The acceleration data was converted into a dynamic deformation by applying a transfer function defined using the Empirical Mode Decomposition Method. The transfer function was constructed using data produced on an experimental rig, and it was scaled to an existing subway system. The equivalent deformation improved the analysis of the dynamic loads that affect the substructure of the subway tracks because it is considered the primary load that acts on the track and substructure. The acceleration data and the estimated deformations were analyzed with the Continues Wavelet Transform. The equivalent deformation data facilitated the application of a health monitoring system and simplified the development of predictive maintenance programs for the subway or railroad operators. This method better identified cracks in the substructure than using the acceleration data. KW - Health monitoring KW - Transfer function KW - Railroad KW - Substructure failures KW - Dynamic loads PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557480 DO - https://doi.org/10.3389/fmech.2022.858424 SN - 2297-3079 VL - 8 SP - 1 EP - 16 PB - Frontiers Media CY - Lausanne AN - OPUS4-55748 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dubey, A. A1 - Hon Keat, C. A1 - Shvartsman, V. A1 - Yusenko, Kirill A1 - Escobar, M. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Hagemann, U. A1 - Kovalenko, S. A1 - Stächler, J. A1 - Lupascu, D. T1 - Mono-, Di-, and Tri-valent Cation Doped BiFe0.95Mn0.05O3 Nanoparticles: Ferroelectric Photocatalysts N2 - The ferroelectricity of multivalent co-doped Bismuth ferrite (BiFeO3; BFO) nanoparticles (NPs) is revealed and utilized for light photocatalysis exploiting their narrow electronic band gap. The photocatalytic activity of ferroelectric photocatalysts BiFe0.95Mn0.05O3 (BFM) NPs and mono-, di-, or tri-valent cations (Ag+, Ca2+, Dy3+; MDT) co-incorporated BFM NPs are studied under ultrasonication and in acidic conditions. We find that such doping enhances the photocatalytic activity of the ferroelectric NPs approximately three times. The correlation of the photocatalytic activity with structural, optical, and electrical properties of the doped NPs is established. The increase of spontaneous polarization by the mono- and tri-valent doping is one of the major factors in enhancing the photocatalytic performance along with other factors such as stronger light absorption in the visible range, low recombination rate of charge carriers and larger surface area of NPs. A-site doping of BFO NPs by divalent elements suppresses the polarization, whereas trivalent (Dy3+) and monovalent (Ag+) cations provide an increase of polarization. The depolarization field in these single domain NPs acts as a driving force to mitigate recombination of the photoinduced charge carriers. KW - Piezoresponse KW - Bismuth Ferrite KW - Nanoparticles KW - Photocatalysis KW - Ferroelectric KW - Polarization PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557230 DO - https://doi.org/10.1002/adfm.202207105 SN - 1616-301X SP - 1 EP - 16 PB - Wiley AN - OPUS4-55723 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nehring, Grzegorz A1 - Gordon, Nehemia A1 - Rabin, Ira T1 - Distinguishing between seemingly identical inks using scanning μXRF and heat maps N2 - This study will present a new approach to distinguishing writing inks that have the same elemental compositions and visual appearances. The approach is based on displaying the intensity of elemental distributions as heat maps that represent data recorded with a scanning μX-ray fluorescence spectrometer. The heat maps present the data so as to facilitate digitally identifying and distinguishing between inks used to produce, correct, and reink two medieval Torah scrolls. As ritual objects, Torah scrolls had to be written in accordance with exacting standards that evolved over time. This requirement led to successive stages of modifications, sometimes over centuries. Both vitriolic and non-vitriolic inks used to modify Torah scrolls can be visually identical to each other. Furthermore, different non-vitriolic inks usually have an identical elemental composition. The solid material analysis evidence and its presentation as heat maps made it possible to discriminate between original and altered portions of text that in some cases would have been impossible. Our interdisciplinary work brought together conservation, material science, paleog-raphy, and philology to enable the identification of complex stratigraphy in multiple stages of production, correction, and reinking. ©2 0 2 2 Published by Elsevier Masson SAS. KW - Spectroscopy KW - Scanning micro-X-ray fluorescence KW - Vitriolic iron-gall inks KW - Non-vitriolic iron-gall inks KW - Heat maps KW - Torah scrolls KW - Scribal corrections PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557271 DO - https://doi.org/10.1016/j.culher.2022.07.007 SN - 1296-2074 VL - 57 SP - 142 EP - 148 PB - Elsevier Masson SAS AN - OPUS4-55727 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sichler, Theresa Constanze A1 - Adam, Christian A1 - Barjenbruch, M. A1 - Montag, D. A1 - Mauch, Tatjana A1 - Sommerfeld, Thomas A1 - Ehm, J.H. T1 - Variation of the element composition of municipal sewage sludges in the context of new regulations on phosphorus recovery in Germany N2 - Phosphorus (P) recovery is obligatory for all sewage sludges with more than 20 g P/kg dry matter (DM) from 2029 in Germany. Nine wastewater treatment plants (WWTPs) were chosen to investigate variations of phosphorus contents and other parameters in sewage sludge over the year. Monthly sewage sludge samples from each WWTP were analyzed for phosphorus and other matrix elements (C, N, H, Ca, Fe, Al, etc.), for several trace elements (As, Cr, Mo, Ni, Pb, Sn) and loss of ignition. Among the nine WWTPs, there are four which have phosphorus contents both above and below the recovery limit of 20 g/kg DM along the year. Considering the average phosphorus content over the year, only one of them is below the limit. Compared to other matrix elements and parameters, phosphorus fuctuations are low with an average of 7% over all nine WWTPs. In total, only hydrogen and carbon are more constant in the sludge. In several WWTPs with chemical phosphorus elimination, phosphorus fuctuations showed similar courses like iron and/or aluminum. WWTPs with chamber flter presses rather showed dilution efects of calcium dosage. As result of this study, monthly phosphorus measurement is highly recommended to determine whether a WWTP is below the 20 g/kg DM limit. KW - Sewage sludge KW - Phosphorus recovery KW - Wastewater KW - Phosphorus elimination PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557499 DO - https://doi.org/10.1186/s12302-022-00658-4 SN - 2190-4707 VL - 34 IS - 1 SP - 1 EP - 12 PB - Springer Nature CY - Berlin AN - OPUS4-55749 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen A1 - Scheliga, F. T1 - Ring-opening polymerizations of L-Lactide catalyzed by zinc caprylate: Syntheses of cyclic and linear poly(L-lactide)s N2 - Alcohol-initiated ring-opening polymerizations (ROPs) of L-Lactide (LA) were conducted in bulk at 130 °C catalyzed by Zn acetate (ZnAc2), lactate (ZnLac2), or caprylate (ZnCap2). 11-undecenol (UND), 1-hydroxymethylnaphtalene (HMN), and 4-nitrobenzylalcohol (4NB) were used as alcohols. Whereas variation of the alcohols had little effect, the usefulness of the catalysts increased in the order: acetate < lactate < caprylate. Hence, further alcohol-initiated polymerizations were performed with ZnCap2 alone and with variation of the lactide/catalyst (LA/Cat) ratio. With increasing LA/Cat ratio higher fractions of cyclic poly(L-lactide) (PLA) were found, so that the measured degree of polymerization (DP) is considerably lower than the theoretical value (i.e., 2 x LA/alcohol). With neat ZnCap2 cyclic PLAs were the largely prevailing reaction products. For these cyclic PLAs weight average molar masses (Mw) up to 134,000 were obtained and an optical purity around 99% was indicated by 13C NMR spectroscopy and DSC measurements even after 48 h at 150 or 160 °C. KW - Cyclization KW - Lactide KW - Ring opening polymerization KW - Transesterification KW - Zinc catalyst KW - MALDI PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557565 DO - https://doi.org/10.1002/pol.20220328 SN - 2642-4150 SP - 1 EP - 10 PB - Wiley AN - OPUS4-55756 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rautenberg, Max A1 - Bhattacharya, Biswajit A1 - Witt, Julia A1 - Jain, Mohit A1 - Emmerling, Franziska T1 - In situ time-resolved monitoring of mixed-ligand metal–organic framework mechanosynthesis N2 - The mechanism of mixed-ligand metal–organic framework (MOF) formation, and the possible role of intermediate single-ligand metal complexes during mechanosynthesis, have not been explored yet. For the first time, we report here in situ real-time monitoring of the mechanochemical formation mechanism of mixed-ligand MOFs. Our results show that binary phases can act as intermediates or competing products in one-pot and stepwise synthesis. KW - Mechanochemistry KW - Metal-organic-frameworks KW - In situ X-ray diffraction KW - Mixed-ligand MOFs PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-558167 DO - https://doi.org/10.1039/D2CE00803C SP - 1 EP - 4 PB - Royal Society of Chemistry AN - OPUS4-55816 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pacheco, V. A1 - Marattukalam, J. J. A1 - Karlsson, D. A1 - Dessieux, L. A1 - Tran, K. V. A1 - Beran, P. A1 - Manke, I. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Sahlberg, M. A1 - Woracek, R. T1 - On the relationship between laser scan strategy, texture variations and hidden nucleation sites for failure in laser powder-bed fusion N2 - While laser powder-bed fusion has overcome some of the design constraints of conventional manufacturing methods, it requires careful selection of process parameters and scan strategies to obtain favorable properties. Here we show that even simple scan strategies, complex ones being inevitable when printing intricate designs, can inadvertently produce local alterations of the microstructure and preferential grain orientation over small areas – which easily remain unnoticed across the macroscale. We describe how a combined usage of neutron imaging and electron backscatter diffraction can reveal these localized variations and explain their origin within cm-sized parts. We explain the observed contrast variations by linking the neutron images to simulated data, pole figures and EBSD, providing an invaluable reference for future studies and showing that presumably minor changes of the scan strategy can have detrimental effects on the mechanical properties. In-situ tensile tests reveal that fracture occurs in a region that was re-melted during the building process. KW - Laser powder-bed fusion KW - Texture KW - Preferential orientation KW - Diffraction contrast neutron imaging KW - Bragg-edge PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568054 DO - https://doi.org/10.1016/j.mtla.2022.101614 VL - 26 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-56805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Engelking, Lorenz A1 - Schröpfer, Dirk A1 - Kannengießer, Thomas A1 - Eissel, A. A1 - Treutler, K. A1 - Wesling, V. T1 - Alloy modification for additive manufactured Ni alloy components Part II: Effect on subsequent machining properties N2 - Alloy 36 (1.3912) is an alloy with 36% nickel and 64% iron and is generally classified as a difficult-to-cut material. Increasingly complex structures and the optimization of resource efficiency are making additive manufacturing (AM) more and more attractive for the manufacture or repair of components. Subsequent machining of AM components is unavoidable for its final contour. By using modern, hybrid machining processes, e.g., ultrasonic-assisted milling (US), it is possible to improve the cutting situation regarding the resulting surface integrity as well as the cutting force. Part I deals with the influence of the alloying elements Ti, Zr, and Hf on the microstructure and the hardness of the initial alloy 36. Part II focusses on the effect of the alloy modifications and the ultrasonic assistance on machinability as well as on the surface integrity after finish-milling. The results show a highly significant influence of the ultrasonic assistance. The cutting force during the US is reduced by over 50% and the roughness of approx. 50% compared to conventional milling (CM) for all materials investigated. Moreover, the US causes a defect-free surface and induces near-surface compressive residual stresses. CM leads to a near-surface stress state of approx. 0 MPa. T2 - 75th IIW Annual Assembly CY - Tokyo, Japan DA - 17.07.2022 KW - Alloy 36 KW - Ultrasonic-assisted milling KW - Surface integrity KW - Modification of structural morphology PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-566609 DO - https://doi.org/10.1007/s40194-022-01438-7 SP - 1 EP - 8 PB - Springer CY - Heidelberg AN - OPUS4-56660 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Witte, Julien A1 - Schröpfer, Dirk A1 - Hamacher, M. A1 - Michels, H. A1 - Hamm, C. A1 - Appelt, M. A1 - Börner, Andreas A1 - Kannengießer, Thomas T1 - Tool development for hybrid finishing milling of iron aluminides N2 - The importance of high-temperature materials made of iron aluminides (FeAl) has been increasing in light weight applications, e.g., airplane turbines, due to the high material’s specific strength. However, the highly economic production by means of permanent mold casting involves special microstructures for Fe26Al4Mo0.5Ti1B alloy components leading to difficult machinability for subsequent finishing milling and low surface qualities. Major effects of tool and machining parameter variation incorporating ultrasonic assistance on the milling process and surface integrity are shown. Loads for tool and component surface are significantly adjustable to enable an economic process chain regarding the surface integrity of safety-relevant components. KW - Ultrasonic-assisted milling KW - Iron aluminide KW - Surface integrity KW - Tool wear PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-566294 DO - https://doi.org/10.1016/j.procir.2022.03.123 SN - 2212-8271 VL - 108 SP - 793 EP - 798 PB - Elsevier B.V. AN - OPUS4-56629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scharf-Wildenhain, R. A1 - Hälsig, A. A1 - Hensel, J. A1 - Wandtke, Karsten A1 - Schröpfer, Dirk A1 - Kannengießer, Thomas T1 - Heat control and design‑related effects on the properties and welding stresses in WAAM components of high‑strength structural steels N2 - Commercial high-strength fller metals for wire arc additive manufacturing (WAAM) are already available. However, widespread industrial use is currently limited due to a lack of quantitative knowledge and guidelines regarding welding stresses and component safety during manufacture and operation for WAAM structures. In a joint research project, the process- and material-related as well as design infuences associated with residual stress formation and the risk of cold cracking are being investigated. For this purpose, reference specimens are welded fully automated with defned dimensions and systematic variation of heat control using a special, high-strength WAAM fller metal (yield strength>790 MPa). Heat control is varied by means of heat input (200–650 kJ/m) and interlayer temperature (100–300 °C). The ∆t8/5 cooling times correspond with the recommendations of fller metal producers (approx. 5–20 s). For this purpose, additional thermo-physical forming simulations using a dilatometer allowed the complex heat cycles to be reproduced and the resulting ultimate tensile strength of the weld metal to be determined. Welding parameters and AM geometry are correlated with the resulting microstructure, hardness, and residual stress state. High heat input leads to a lower tensile stress in the component and may cause unfavorable microstructure and mechanical properties. However, a sufciently low interlayer temperature is likely to be suitable for obtaining adequate properties at a reduced tensile stress level when welding with high heat input. The component design afects heat dissipation conditions and the intensity of restraint during welding and has a signifcant infuence on the residual stress. These complex interactions are analyzed within this investigation. The aim is to provide easily applicable processing recommendations and standard specifcations for an economical, appropriate, and crack-safe WAAM of high-strength steels. KW - GMA welding KW - Additive manufacturing KW - Residual stresses KW - High-strength steel KW - Cold cracking safety KW - Heat control KW - Wind energy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567397 DO - https://doi.org/10.1007/s40194-022-01450-x SN - 1878-6669 VL - 2022 SP - 1 EP - 11 PB - Springer CY - Berlin AN - OPUS4-56739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Menga, D. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Wagner, F. A1 - Fellinger, Tim-Patrick T1 - Evaluation of the Specific Activity of MNCs and the Intrinsic Activity of Tetrapyrrolic FeN4 Sites for the Oxygen Reduction Reaction N2 - M−N−C electrocatalysts are considered pivotal to replace expensive precious group metal-based materials in electrocatalytic conversions. However, their development is hampered by the limited availability of methods for the evaluation of the intrinsic activity of different active sites, like pyrrolic FeN4 sites within Fe−N−Cs. Currently, new synthetic procedures based on active-site imprinting followed by an ion exchange reaction, e.g. Zn-to-Fe, are producing single-site M−N−Cs with outstanding activity. Based on the same replacement principle, we employed a conservative iron extraction to partially remove the Fe ions from the N4 cavities in Fe−N−Cs. Having catalysts with the same morphological properties and Fe ligation that differ solely in Fe content allows for the facile determination of the decrease in density of active sites and their turn-over frequency. In this way, insight into the specific activity of M−N−Cs is obtained and for single-site catalysts the intrinsic activity of the site is accessible. This new approach surpasses limitations of methods that rely on probe molecules and, together with those techniques, offers a novel tool to unfold the complexity of Fe−N−C catalyst and M−N−Cs in general. KW - Fe-N-C catalysts KW - M-N-C catalysts KW - Fuel Cells PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567406 DO - https://doi.org/10.1002/anie.202207089 SN - 1433-7851 VL - 61 IS - 50 SP - 1 EP - 6 PB - Wiley-VHC AN - OPUS4-56740 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Buzolin, R. H. A1 - Richter, Tim A1 - Pixner, F. A1 - Rhode, Michael A1 - Schroepfer, Dirk A1 - Enzinger, N. T1 - Microstructure characterisation of multi-principal element alloys welds produced by electron beam welding N2 - This work explores the feasibility of producing bead-on-plate welds of a CrCoNi medium entropy alloy and a CrMnFeCoNi high entropy alloy using electron beam welding. The alloys were welded in two states: one in an as-cold-rolled condition and the other in an annealed condition. In addition, the materials are welded with two different parameters. The FCC microstructure of the welds is investigated using scanning electron microscopy assisted by energy-dispersive X-ray spectroscopy and electron-backscattered diffraction. The impact of the weld on the microstructure is discussed. The heat-affected zone is negligible for the annealed condition of both medium and high entropy alloys since there is no driving force for recrystallisation and the exposure time to high temperature is insufficient for grain coarsening. The texture formed in the fusion zone is also discussed and compared to the texture in the base metal and the heat-affected zone. Although the grain growth along the (100) crystallographic direction is preferential in all cases, the crystallographic texture type differs from each weld. Higher hardness values are measured in the medium entropy alloy’s base metal and fusion zone than in the high entropy alloy. KW - Multi-principal element alloy KW - Electron backscattered diffraction KW - Electron beam welding KW - High-entropy alloy KW - Microstructure characterization PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568129 DO - https://doi.org/10.1016/j.matdes.2023.111609 SN - 1873-4197 VL - 225 SP - 1 EP - 14 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-56812 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pakrashy, S. A1 - Mandal, P. K. A1 - Goswami, J. N. A1 - Dey, S. K. A1 - Choudhury, S. M. A1 - Bhattacharya, Biswajit A1 - Emmerling, Franziska A1 - Alasmary, F. A. A1 - Dolai, M. T1 - Bioinformatics and Network Pharmacology of the First Crystal Structured Clerodin: Anticancer and Antioxidant Potential against Human Breast Carcinoma Cell N2 - Clerodin was isolated from the medicinal plant Clerodendrum infortunatum, and CSD search showed the first crystal structure of clerodin by a single-crystal X-ray diffraction study. We checked its binding potential with target proteins by docking and conducted network pharmacology analysis, ADMET analysis, in silico pathway analysis, normal mode analysis (NMA), and cytotoxic activity studies to evaluate clerodin as a potential anticancer agent. The cell viability studies of clerodin on the human breast carcinoma cell line (MCF-7) showed toxicity on MCF-7 cells but no toxicity toward normal human lymphocyte cells (HLCs). The anticancer mechanism of clerodin was validated by its enhanced capacity to produce intracellular reactive oxygen species (ROS) and to lower the reduced glutathione content in MCF-7 cells. KW - Anticancer KW - Clerodin PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567600 DO - https://doi.org/10.1021/acsomega.2c07173 SN - 2470-1343 VL - 7 IS - 51 SP - 48572 EP - 48582 PB - ACS Publ. CY - Washington, DC AN - OPUS4-56760 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rockenhäuser, Christian A1 - von Hartrott, P. A1 - Skrotzki, Birgit T1 - Brinell-Hardness data (HBW 2.5/62.5) of aluminum alloy EN AW-2618A after different aging times and temperatures N2 - The article covers data on the Brinell hardness of the forged precipitation-hardened aluminum alloy EN AW-2618A in the initial T61 condition (i. e. slightly underaged) and after isothermal aging for up to 25,0 0 0 h at aging temperatures between 160 °C and 350 °C. In addition, the hardness was determined on specimens after creep testing at 190 °C and various stresses. The hardness decreases with increasing ag- ing time due to the microstructural evolution of the harden- ing precipitates. The drop occurs faster the higher the aging temperature. Aging under creep load additionally accelerates the hardness decrease. KW - Aluminum alloy KW - EN AW-2618A KW - Brinell hardness KW - Aging KW - Creep KW - Ostwald ripening KW - Reheating PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567611 DO - https://doi.org/10.1016/j.dib.2022.108830 SN - 2352-3409 VL - 46 PB - Elsevier Inc. AN - OPUS4-56761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pittner, Andreas A1 - Rethmeier, Michael T1 - Life Cycle Assessment of Fusion Welding Processes - A Case Study of Resistance Spot Welding Versus Laser Beam Welding N2 - The high amount of resource consumption of fusion welding processes offers the potential to reduce their environmental impact. While the driving forces are known froma qualitative perspective, the quantitative assessment of the crucial parameters is not a trivial task. Therefore, herein, a welding-specific methodology to utilize life cycle assessment as a tool for evaluating the environmental impact of fusion welding processes is presented. In this context, two welding processes, resistance spot welding and laser beam welding, are analyzed for two different use cases. These comprise the welding of shear test specimens and a cap profile made of electrogalvanized sheets of DC 05þ ZE (1.0312) as representative of an automotive application. For both welding processes, the main influences on the resulting environmental impact categories are evaluated and compared. The requirements for ecological efficient welding processes are discussed and implemented. KW - Resistance spot welding KW - Carbon dioxide footprint KW - Environmental impact categories KW - Laser beam welding KW - Life cycle assessment PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-566458 DO - https://doi.org/10.1002/adem.202101343 SN - 1438-1656 VL - 24 IS - 6 SP - 1 EP - 14 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56645 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Tim A1 - Schröpfer, Dirk A1 - Rhode, Michael T1 - Residual stresses in a high- and a medium-entropy alloy due to TIG and friction stir welding N2 - The new alloying concept of multi-element systems with defined entropy (HEA—high-entropy alloy; MEA—medium-entropy alloy) is gaining increasing importance in materials research. Significantly improved properties or combinations of properties are shown by some HEA/MEA systems. Thus, primarily the production and resulting microstructures of HEA, as well as its properties, have been investigated so far. Furthermore, processing is a main issue in transferring HEA systems from the laboratory to real components. Since welding is the most important joining process for metals, it is crucial to investigate the influence of welding to guarantee component integrity. Welding leads to residual stresses, which significantly affect the component integrity. Hence, the focus of this study is the residual stress formation and distribution in a CoCrFeMnNi HEA and ternary CoCrNi MEA using two different welding processes: tungsten inert gas (TIG) welding and solid-state friction stir welding (FSW). As a pathway for the application of HEA in this investigation, for the first time, residual stress analyses in realistic near-component specimens were performed. The residual stresses were determined by X-ray diffraction (XRD) on the surfaces of top and root weld side. The results were correlated with the local welding microstructures. The results show that both FSW and TIG generate significant tensile residual stresses on the weld surfaces in, and transverse to, the welding direction. In the case of FSW of the CoCrFeMnNi HEA, the longitudinal residual stresses are in the range of the yield strength of approx. 260 MPa in the weld zone. KW - High entropy alloy KW - Welding KW - Residual stresses KW - Microstructure PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567039 DO - https://doi.org/10.3390/jmmp6060147 SN - 2504-4494 VL - 6 IS - 6 SP - 1 EP - 11 PB - MDPI CY - Basel AN - OPUS4-56703 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -