TY - CONF A1 - Kanzler, D. A1 - Bertovic, Marija A1 - Dethof, F. A1 - Heckel, Thomas A1 - Jüngert, A. A1 - Keßler, S. A1 - Rentala, V. A1 - Rosenthal, Martina A1 - Stolz, R. A1 - Vrana, J. T1 - Die deutschen Bestrebungen zur Normierung der Fähigkeits- und Zuverlässigkeitsbewertung der zerstörungsfreien Prüfung N2 - Seit 1999 existiert das MIL-HDBK 1823, die us-amerikanische Leitfaden zur Erstellung einer Probability of Detection (POD; Fehlerdetektionswahrscheinlichkeit). Obwohl das Dokument als internationaler Stand der Technik angesehen wird, ist die allgemeine Anwendung in der ZfP-Praxis von einigen Nachteilen begleitet: 1. Die beschriebenen POD‘s bilden ausschließlich die Grundlagen-POD ab, jeweils mit nur einem Fehlerparameter und einem Signalparameter. Modernere Ansätze werden hier nicht adressiert. 2. Die aktuelle Version verzichtet fast vollständig auf konkrete mathematische Formulierungen. 3. Die Richtlinie richtet sich hauptsächlich an die militärische Luftfahrt. 4. Das Dokument ist nur in englischer Sprache verfügbar. Mit Hilfe eines BMWi-Förderprojekts wird ein weiterführendes Regelwerk auf Basis der MIL-HDBK 1823 unter deutscher Federführung erarbeitet, welches die Anwendung der POD-Berechnung auf eine breitere Basis stellt und die oben genannten Nachteile der MIL-HDBK 1823 behebt. Das vorgestellte Projekt „normPOD“ wird eine normative, branchenübergreifend einsetzbare Beschreibung des Vorgehens bei der Berechnung einer POD zur Zuverlässigkeitsbewertung zerstörungsfreier Prüfungen entwickeln. Hierbei wird Klarheit über unterschiedliche POD-Ansätze geschaffen und anhand praktischer Beispiele aus Maschinenbau und Bauwesen ein Leitfaden für den Praxiseinsatz erarbeitet. Das Poster gibt einen Überblick über die geplanten Arbeiten innerhalb des Projekts und lädt die Beteiligten der DGZfP-Jahrestagung zur Diskussion ein, um eine breite Basis und Akzeptanz für die entwickelten Berechnungsverfahren zu schaffen, insbesondere in Hinblick auf ZfP 4.0 und Digitalisierung. T2 - Jahrestagung der DGZfP CY - Online meeting DA - 10.05.2021 KW - Zerstörungsfreie Prüfung KW - ZfP KW - Zuverlässigkeit KW - Standardisierung KW - Human Factors PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-535628 UR - www.ndt.net/article/dgzfp2021/papers/P40.pdf SP - 1 EP - 8 AN - OPUS4-53562 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Michalchuk, Adam A1 - Rudic, S. A1 - Pulham, C. A1 - Morrison, C. T1 - Predicting the impact sensitivity of a polymorphic high explosive: the curious case of FOX-7 N2 - The impact sensitivity (IS) of FOX-7 polymorphs is predicted by phonon up-pumping to decrease as layers of FOX-7 molecules flatten. Experimental validation proved anomalous owing to a phase transition during testing, raising questions regarding Impact sensitivity measurement and highlighting the need for models to predict IS of polymorphic energetic materials. KW - Energetic materials KW - Density functional theory KW - Inelastic Neutron Scattering Spectroscopy KW - Impact Sensitivity PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-535558 DO - https://doi.org/10.1039/d1cc03906g SN - 1364-548X VL - 57 IS - 85 SP - 11213 EP - 11216 PB - Royal Society of Chemistry AN - OPUS4-53555 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Climent Terol, Estela A1 - Rurack, Knut A1 - Hecht, Mandy T1 - Loading and Release of Charged and Neutral Fluorescent Dyes into and from Mesoporous Materials: A Key Role for Sensing Applications N2 - The aim of this study is to determine the efficiency of loading and release of several zwitterionic, neutral, anionic and cationic dyes into/from mesoporous nanoparticles to find the optimum loading and release conditions for their application in detection protocols. The loading is carried out for MCM-41 type silica supports suspended in phosphate-buffered saline (PBS) buffer (pH 7.4) or in acetonitrile, involving the dyes (rhodamine B chloride, rhodamine 101 chloride, rhodamine 101 perchlorate, rhodamine 101 inner salt, meso-(4-hydroxyphenyl)-boron–dipyrromethene (BODIPY), sulforhodamine B sodium salt and fluorescein 27). As a general trend, rhodamine-based dyes are loaded with higher efficiency, when compared with BODIPY and fluorescein dyes. Between the rhodamine-based dyes, their charge and the solvent in which the loading process is carried out play important roles for the amount of cargo that can be loaded into the materials. The delivery experiments carried out in PBS buffer at pH 7.4 reveal for all the materials that anionic dyes are more efficiently released compared to their neutral or cationic counterparts. The overall best performance is achieved with the negatively charged sulforhodamine B dye in acetonitrile. This material also shows a high delivery degree in PBS buffer. KW - Mesoporous materials KW - Charged dyes KW - Neutral dyes KW - Dye loading optimisation KW - Dye release PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522596 UR - https://www.mdpi.com/2072-666X/12/3/249 DO - https://doi.org/10.3390/mi12030249 VL - 12 IS - 3 SP - 249 PB - MDPI AN - OPUS4-52259 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Denkler, Tilman T1 - Accreditation in Europe: Benchmarking the operations of European accreditation bodies using an innovative management tool N2 - Accreditation is one of the pillars of a national Quality Infrastructure, as the competence of conformity assessment bodies is assured through accreditation performed by accreditation bodies. To compare the operation of accreditation bodies in Europe and to identify best practices, a management tool, the Process Maturity Benchmarking Tool, was developed and validated by applying it to European accreditation bodies. The benchmarking project comprised two major phases: In the first phase, the processes of accreditation bodies were systematically analyzed. A process map was developed, and processes of special relevance were identified and underpinned by indicators. In the second phase, the practical applicability of the theoretical model was demonstrated by analyzing the processes of eight European accreditation bodies. The results of this comparative assessment were subsequently discussed in a workshop with experts from those accreditation bodies, giving the opportunity to identify best practices. This article has a twofold objective. First, to present a method to benchmark European accreditation bodies, based on the European Foundation for Quality Management excellence model. The successful application of the Process Maturity Benchmarking Tool gives evidence that it is a suitable and capable management tool to assess the processes of the European accreditation bodies and to benchmark them. Second, the article presents the results of the first adaption of the Process Maturity Benchmarking Tool. A general trend of process maturity was identified: While processes based on stakeholder involvement tend to have an overall lower maturity on average, internal processes are more mature. KW - Accreditation KW - Benchmarking KW - Quality Infrastructure KW - EFQM Excellence Modell KW - Total Quality Management KW - Akkreditierung PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521706 DO - https://doi.org/10.1007/s00769-021-01459-7 VL - 26 IS - 1 SP - 47 EP - 57 PB - Springer Nature CY - Jersey City, NJ 07302, USA AN - OPUS4-52170 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Long, Lijia A1 - Alcover, I. F. A1 - Thöns, Sebastian T1 - Utility analysis for SHM durations and service life extension of welds on steel bridge deck N2 - Optimization of the duration of Structural Health Monitoring (SHM) campaigns is rarely performed. This article provides a utility-based solution to posteriorly determine: i) optimal monitoring Durations and ii) the extension of the service life of the welds on a steel bridge deck. The approach is Illustrated with a case study focusing on remaining fatigue life estimation of the welds on the orthotropic steel deck of the Great Belt Bridge, in Denmark. The identification of the optimal monitoring duration and the decision about extending the service life of the welds are modelled by maximizing the expected benefits and minimizing the structural risks. The results are a parametric analysis, mainly on the effect of the target probability, benefit, cost of failure, cost of rehabilitation, cost of monitoring and Discount rate on the posterior utilities of monitoring strategies and the choice of service life considering the risk variability and the costs and benefits models. The results show that the decision on short-term monitoring, i.e., 1 week every six months, is overall the most valued SHM strategy. In addition, it is found that the target probability is the most sensitive parameter affecting the optimal SHM Durations and service life extension of the welds. KW - Fatigue KW - Monitoring strategy KW - Orthotropic steel deck KW - Structural health monitoring KW - Utility and decision theory PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521719 DO - https://doi.org/10.1080/15732479.2020.1866026 SN - 1573-2479 VL - 18 IS - 4 SP - 492 EP - 504 PB - Taylor Francis Online AN - OPUS4-52171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Anzt, H. A1 - Bach, F. A1 - Druskat, S. A1 - Löffler, F. A1 - Loewe, A. A1 - Renard, B. Y. A1 - Seemann, G. A1 - Struck, A. A1 - Achhammer, E. A1 - Aggarwal, P. A1 - Appel, F. A1 - Bader, M. A1 - Brusch, L. A1 - Busse, C. A1 - Chourdakis, G. A1 - Dabrowski, P. W. A1 - Ebert, P. A1 - Flemisch, B. A1 - Friedl, S. A1 - Fritzsch, B. A1 - Funk, M. D. A1 - Gast, V. A1 - Goth, F. A1 - Grad, J. A1 - Hegewald, J. A1 - Hermann, S. A1 - Hohmann, F. A1 - Janosch, S. A1 - Kutra, D. A1 - Linxweiler, J. A1 - Muth, Thilo A1 - Peters-Kottig, W. A1 - Rack, F. A1 - Raters, F. H. C. A1 - Rave, S. A1 - Reina, G. A1 - Reißig, M. A1 - Ropinski, T. A1 - Schaarschmidt, J. A1 - Seibold, H. A1 - Thiele, J. P. A1 - Uekermann, B. A1 - Unger, S. A1 - Weeber, R. T1 - An environment for sustainable research software in Germany and beyond: current state, open challenges, and call for action N2 - Research software has become a central asset in academic research. It optimizes existing and enables new research methods, implements and embeds research knowledge, and constitutes an essential research product in itself. Research software must be sustainable in order to understand, replicate, reproduce, and build upon existing research or conduct new research effectively. In other words, software must be available, discoverable, usable, and adaptable to new needs, both now and in the future. Research software therefore requires an environment that supports sustainability. Hence, a change is needed in the way research software development and maintenance are currently motivated, incentivized, funded, structurally and infrastructurally supported, and legally treated. Failing to do so will threaten the quality and validity of research. In this paper, we identify challenges for research software sustainability in Germany and beyond, in terms of motivation, selection, research software engineering personnel, funding, infrastructure, and legal aspects. Besides researchers, we specifically address political and academic decision-makers to increase awareness of the importance and needs of sustainable research software practices. In particular, we recommend strategies and measures to create an environment for sustainable research software, with the ultimate goal to ensure that software-driven research is valid, reproducible and sustainable, and that software is recognized as a first class citizen in research. This paper is the outcome of two workshops run in Germany in 2019, at deRSE19 - the first International Conference of Research Software Engineers in Germany - and a dedicated DFG-supported follow-up workshop in Berlin. KW - Research Software KW - Sustainable Software Development KW - Academic Software KW - Software Infrastructure KW - Software Training KW - Software Licensing PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522029 DO - https://doi.org/10.12688/f1000research.23224.2 VL - 9 SP - 1 EP - 35 AN - OPUS4-52202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pech, S. A1 - Rehberg, M. A1 - Janke, R. A1 - Benndorf, D. A1 - Genzel, Y. A1 - Muth, Thilo A1 - Sickmann, A. A1 - Rapp, E. A1 - Reichl, U. T1 - Tracking changes in adaptation to suspension growth for MDCK cells: cell growth correlates with levels of metabolites, enzymes and proteins N2 - Adaptations of animal cells to growth in suspension culture concern in particular viral vaccine production, where very specific aspects of virus-host cell interaction need to be taken into account to achieve high cell specific yields and overall process productivity. So far, the complexity of alterations on the metabolism, enzyme, and proteome level required for adaptation is only poorly understood. In this study, for the first time, we combined several complex analytical approaches with the aim to track cellular changes on different levels and to unravel interconnections and correlations. Therefore, a Madin-Darby canine kidney (MDCK) suspension cell line, adapted earlier to growth in suspension, was cultivated in a 1-L bioreactor. Cell concentrations and cell volumes, extracellular metabolite concentrations, and intracellular enzyme activities were determined. The experimental data set was used as the input for a segregated growth model that was already applied to describe the growth dynamics of the parental adherent cell line. In addition, the cellular proteome was analyzed by liquid chromatography coupled to tandem mass spectrometry using a label-free protein quantification method to unravel altered cellular processes for the suspension and the adherent cell line. Four regulatory mechanisms were identified as a response of the adaptation of adherent MDCK cells to growth in suspension. These regulatory mechanisms were linked to the proteins caveolin, cadherin-1, and pirin. Combining cell, metabolite, enzyme, and protein measurements with mathematical modeling generated a more holistic view on cellular processes involved in the adaptation of an adherent cell line to suspension growth. KW - MDCK cell KW - Proteome KW - Metabolism KW - Enzyme activity KW - Suspension growth PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522070 DO - https://doi.org/10.1007/s00253-021-11150-z VL - 105 IS - 5 SP - 1861 EP - 1874 PB - Springer AN - OPUS4-52207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ziesche, R. F. A1 - Robinson, J. B. A1 - Markötter, Henning A1 - Bradbury, R. A1 - Tengattini, A. A1 - Lenoir, N. A1 - Helfen, L. A1 - Kockelmann, W. A1 - Kardjilov, N. A1 - Manke, I. A1 - Brett, D. J. L. A1 - Shearing, P. R. T1 - Editors’ Choice—4D Neutron and X-ray Tomography Studies of High Energy Density Primary Batteries: Part II. Multi-Modal Microscopy of LiSOCl2 Cells N2 - The ability to track electrode degradation, both spatially and temporally, is fundamental to understand performance loss during operation of lithium batteries. X-ray computed tomography can be used to follow structural and morphological changes in electrodes; however, the direct detection of electrochemical processes related to metallic lithium is difficult due to the low sensitivity to the element. In this work, 4-dimensional neutron computed tomography, which shows high contrast for lithium, is used to directly quantify the lithium diffusion process in spirally wound Li/SOCl2 primary cells. The neutron dataset enables the quantification of the lithium transport from the anode and the accumulation inside the SOCl2 cathode to be locally resolved. Complementarity between the collected neutron and X-ray computed tomographies is shown and by applying both methods in concert we have observed lithium diffusion blocking by the LiCl protection layer and identified all cell components which are difficult to distinguish using one of the methods alone. KW - Lithium-ion battery KW - Room-temperature KW - Thermal runaway KW - Gas evolution KW - Cells PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520890 DO - https://doi.org/10.1149/1945-7111/abbfd9 VL - 167 SP - 140509 PB - IOP Science AN - OPUS4-52089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bevilacqua, N. A1 - Asset, T. A1 - Schmid, M. A. A1 - Markötter, Henning A1 - Manke, I. A1 - Atanassov, P. A1 - Zeis, R. T1 - Impact of catalyst layer morphology on the operation of high temperature PEM fuel cells N2 - Electrochemical impedance spectroscopy (EIS) is a well-established method to analyze a polymer electrolyte membrane fuel cell (PEMFC). However, without further data processing, the impedance spectrum yields only qualitative insight into the mechanism and individual contribution of transport, kinetics, and ohmic losses to the overall fuel cell limitations. The distribution of relaxation times (DRT) method allows quantifying each of these polarization losses and evaluates their contribution to a given electrocatalyst's depreciated performances. We coupled this method with a detailed morphology study to investigate the impact of the 3D-structure on the processes occurring inside a high-temperature polymer electrolyte membrane fuel cell (HT-PEMFC). We tested a platinum catalyst (Pt/C), a platinum-cobalt alloy catalyst (Pt3Co/C), and a platinum group metal-free iron-nitrogen-carbon (Fe–N–C) catalyst. We found that the hampered mass transport in the latter is mainly responsible for its low performance in the MEA (along with its decreased intrinsic performances for the ORR reaction). The better performance of the alloy catalyst can be explained by both improved mass transport and a lower ORR resistance. Furthermore, single-cell tests show that the catalyst layer morphology influences the distribution of phosphoric acid during conditioning. KW - High-temperature polymer electrolyte membrane fuel cell KW - Platinum-free catalyst KW - Mass transport KW - Oxygen reduction reaction KW - Distribution of relaxation times analysis PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520917 DO - https://doi.org/10.1016/j.powera.2020.100042 VL - 7 SP - 100042 PB - Elsevier Ltd. AN - OPUS4-52091 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Niebergall, Ute A1 - Marschall, Niklas A1 - Alig, I. A1 - Böhning, Martin T1 - A phenomenological criterion for an optical assessment of PE-HD fracture surfaces obtained from FNCT N2 - The full-notch creep test (FNCT) is a common test method to evaluate the environmental stress cracking (ESC) behavior of high-density polyethylene (PE-HD), e.g. for container materials. The test procedure as specified in ISO 16770 provides a comparative measure of the resistance against ESC using the time to failure of PE-HD specimens under constant mechanical load in a well-defined liquid test environment. Since the craze-crack damage mechanism underlying the ESC phenomenon is associated with brittle failure, the occurrence of a predominantly brittle fracture surface is a prerequisite to consider an FNCT measurement as representative for ESC, i.e. a time to failure dominated by craze-crack propagation. The craze-crack propagation continuously reduces the effective residual cross-sectional area of the specimen during the test, which results in a corresponding increase of the effective mechanical stress. Thus, a transition to ductile shear deformation is inevitable at later stages of the test, leading usually to a pronounced central ligament. Therefore, an optical evaluation of FNCT fracture surfaces concerning their brittleness is essential. An enhanced imaging analysis of FNCT fracture surfaces enables a detailed assessment of craze-crack Propagation during ESC. In this study, laser scanning microscopy (LSM) was employed to evaluate whether FNCT fracture surfaces are representative with respect to craze-crack propagation and ESC. Based on LSM height data, a phenomenological criterion is proposed to assess the validity of distinct FNCT measurements. This criterion is supposed to facilitate a quick evaluation of FNCT results in practical routine testing. Its applicability is verified on a sample basis for seven different commercial PE-HD container materials. KW - Environmental stress cracking (ESC) KW - Full notch creep test (FNCT) KW - Laser scanning microscopy (LSM) KW - Fracture surfaces KW - Optical criterion of brittleness PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521012 DO - https://doi.org/10.1016/j.polymertesting.2020.107002 VL - 94 SP - 107002 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-52101 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Meyer, A. A1 - Weidner, Steffen T1 - High Tm Poly(l-lactide)s by Means of Bismuth Catalysts? N2 - One series of BiSub-catalyzed ring-opening polymerizations (ROPs) is per-formed at 160 °C for 3 days with addition of difunctional cocatalysts to find out, if poly(l-lactide) crystallizes directly from the reaction mixture. An analogous series is performed with monofunctional cocatalysts. High Tm crystal-lites (Tm > 190 °C) are obtained from all bifunctional cocatalysts, but not from all monofunctional ones. It is shown by means of SAXS measurements that the high Tm values are mainly a consequence of a transesterification–homogenization process across the lamellar surfaces resulting in thickness and smoothing of the surfaces. An unusual enthalpy-driven modification of the molecular weight distribution is found for samples that have crystallized during the polymerization. A third series of ROPs is performed at 170 °C for 2 h followed by annealing at 120 °C (2 h) to induce crystallization. Complete transformation of the resulting low Tm crystallites (Tm < 180 °C) into the high Tm crystallites by annealing at 170 °C for 1 d is not achieved, despite variation of the cocatalyst. KW - Polylactide KW - MALDI-TOF MS KW - Crystallization PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522777 DO - https://doi.org/10.1002/macp.202100019 SN - 1022-1352 VL - 222 IS - 8 SP - 19 PB - Wiley AN - OPUS4-52277 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen T1 - Polymerization of L-lactide with SnCl2: A Low Toxic and Eco-friendly Catalyst N2 - Polymerizations of L-lactide catalyzed either by neat SnCl2 or by SnCl2 + difunctional cocatalysts were conducted in bulk at 180, 160 and 140 °C with variation of the Lac/Cat ratio and time. With neat SnCl2 poly(L-lactide) having weight average molecular weights (uncorrected Mw’s) up to 190 000 g mol−1 were obtained mainly consisting of linear chains. Addition of salicylic acid or 1,1-bisphenol yielded a higher fraction of cyclic polylactides but lower molecular weights. Furthermore, SnCl2 was compared with Bu2SnCl2 and various other metal chlorides and the best results were obtained with SnCl2. With ethyl L-lactate as initiator SnCl2-catalyzed ROPs were performed at 120 °C and the lac/initiator ratio was varied. All these experiments were conducted under conditions allowing for comparison with ROPs catalyzed with neat Sn(II)-2-ethyhexanoate. Such a comparison was also performed with ε-caprolactone as monomer. KW - Catalyst KW - Polylactide KW - MALDI-TOF MS KW - Polycondensation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520517 DO - https://doi.org/10.1007/s10924-020-02042-w SN - 1566-2543 SP - 1 EP - 13 PB - Springer Nature AN - OPUS4-52051 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rühle, Bastian A1 - Krumrey, Julian Frederic A1 - Hodoroaba, Vasile-Dan T1 - Workflow towards automated segmentation of agglomerated, non‑spherical particles from electron microscopy images using artificial neural networks N2 - We present a workflow for obtaining fully trained artificial neural networks that can perform automatic particle segmentations of agglomerated, non-spherical nanoparticles from scanning electron microscopy images “from scratch”, without the need for large training data sets of manually annotated images. The whole process only requires about 15 minutes of hands-on time by a user and can typically be finished within less than 12 hours when training on a single graphics card (GPU). After training, SEM image analysis can be carried out by the artificial neural network within seconds. This is achieved by using unsupervised learning for most of the training dataset generation, making heavy use of generative adversarial networks and especially unpaired image-to-image translation via cycle-consistent adversarial networks. We compare the segmentation masks obtained with our suggested workflow qualitatively and quantitatively to state-of-the-art methods using various metrics. Finally, we used the segmentation masks for automatically extracting particle size distributions from the SEM images of TiO2 particles, which were in excellent agreement with particle size distributions obtained manually but could be obtained in a fraction of the time. KW - Electron microscopy KW - Neural networks KW - Artificial intelligence KW - Image segmentation KW - Automated image analysis PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522454 DO - https://doi.org/10.1038/s41598-021-84287-6 VL - 11 IS - 1 SP - 4942 PB - Springer Nature AN - OPUS4-52245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schutjajew, K. A1 - Pampel, Jonas A1 - Zhang, W. A1 - Antonietti, M. A1 - Oschatz, M. T1 - Influence of pore architecture and chemical structure on the sodium storage in nitrogen‐doped hard carbons N2 - Hard carbon is the material of choice for sodium ion battery anodes. Capacities comparable to those of lithium/graphite can be reached, but the understanding of the underlying sodium storage mechanisms remains fragmentary. A two‐step process is commonly observed, where sodium first adsorbs to polar sites of the carbon (“sloping region”) and subsequently fills small voids in the material (“plateau region”). To study the impact of nitrogen functionalities and pore geometry on sodium storage, a systematic series of nitrogen‐doped hard carbons is synthesized. The nitrogen content is found to contribute to sloping capacity by binding sodium ions at edges and defects, whereas higher plateau capacities are found for materials with less nitrogen content and more extensive graphene layers, suggesting the formation of 2D sodium structures stabilized by graphene‐like pore walls. In fact, up to 84% of the plateau capacity is measured at potentials less than 0 V versus metallic Na, that is, quasimetallic sodium can be stabilized in such structure motifs. Finally, gas physisorption measurements are related to charge discharge data to identify the energy storage relevant pore architectures. Interestingly, these are pores inaccessible to probe gases and electrolytes, suggesting a new view on such “closed pores” required for efficient sodium storage. KW - Sodium Ion Batteries KW - Hard Carbon KW - Storage Mechanism KW - Anode PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522529 DO - https://doi.org/10.1002/smll.202006767 VL - 17 IS - 48 SP - 2006767 PB - Wiley Online Library AN - OPUS4-52252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weimann, Karin A1 - Adam, Christian A1 - Buchert, M. A1 - Sutter, J. T1 - Environmental Evaluation of Gypsum Plasterboard Recycling N2 - Gypsum is widely used in the construction sector and its worldwide consumption has been increasing for several decades. Depending on the life-time of the used gypsum products, an increase of gypsum in construction and demolition waste follows. Especially against the background of a circular economy, the recycling of waste gypsum is of growing importance. However, the use of recycled gypsum makes only sense if it is environmentally friendly. Therefore, an evaluation of the environmental impacts of an industrial-scale processing for the recycling of post-consumer gypsum waste was conducted. The evaluation was performed with an established life cycle assessment software. Original data provided by industry and complementary data from a database for life cycle assessments were used for the calculations. Two scenarios for recycled gypsum with different transportation distances were calculated. These results are compared with results of the environmental evaluation of gypsum derived from coal-fired power plants (FGD gypsum) and natural gypsum. The results show that utilization of recycled gypsum can be environmentally advantageous compared to the use of natural gypsum or FGD gypsum, especially in the impact categories land transformation and resource consumption (abiotic depletion potential). For most environmental impact categories the specific transportation distances have a strong influence. KW - Gypsum plasterboards KW - Gypsum waste KW - Recycled gypsum KW - Environmental evaluation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522321 DO - https://doi.org/10.3390/min11020101 SN - 2075-163X VL - 11 IS - 2 SP - 101 PB - MDPI CY - Basel, Schweiz AN - OPUS4-52232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Legall, Herbert A1 - Bonse, Jörn A1 - Krüger, Jörg T1 - Review of x-ray exposure and safety issues arising from ultra-short pulse laser material processing N2 - Laser processing with ultra-short laser pulses enables machining of materials with high accuracy and throughput. The development of novel laser Technologies with laser pulse repetition rates up to the MHz range opened the way for industrial manufacturing processes. From a radiological point of view this evolution is important, because x-ray radiation can be generated as an unwanted side effect in laser material processing. Even if the emitted x-ray dose per pulse is comparably low, the x-ray dose can become hazardous to health at high laser repetition rates. Therefore, radiation protection must be considered. This article provides an overview on the generation and detection of x-rays in laser material processing, as well as on the handling of this radiation risk in the framework of radiological protection. KW - Ultra-short pulse laser processing KW - Laser-induced x-ray emission KW - Radiation protection PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522376 DO - https://doi.org/10.1088/1361-6498/abcb16 VL - 41 IS - 1 SP - R28 EP - R42 AN - OPUS4-52237 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Plarre, Rüdiger A1 - Zocca, Andrea A1 - Spitzer, Andrea A1 - Benemann, Sigrid A1 - Gorbushina, Anna A1 - Li, Y. A1 - Waske, Anja A1 - Funk, Alexander A1 - Wilgig, Janka A1 - Günster, Jens T1 - Searching for biological feedstock material: 3D printing of wood particles from house borer and drywood termite frass N2 - Frass (fine powdery refuse or fragile perforated wood produced by the activity of boring insects) of larvae of the European house borer (EHB) and of drywood termites was tested as a natural and novel feedstock for 3D-printing of wood-based materials. Small particles produced by the drywood termite Incisitermes marginipennis and the EHB Hylotrupes bajulus during feeding in construction timber, were used. Frass is a powdery material of particularly consistent quality that is essentially biologically processed wood mixed with debris of wood and faeces. The filigree-like particles flow easily permitting the build-up of woodbased structures in a layer wise fashion using the Binder Jetting printing process. The Quality of powders produced by different insect species was compared along with the processing steps and properties of the printed parts. Drywood termite frass with a Hausner Ratio HR = 1.1 with ρBulk = 0.67 g/cm3 and ρTap = 0.74 g/cm3 was perfectly suited to deposition of uniformly packed layers in 3D printing. We suggest that a variety of naturally available feedstocks could be used in environmentally responsible approaches to scientific material sciences/additive manufacturing. KW - 3D printing KW - X-ray tomographic KW - SEM micrography KW - Drywood termite PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521517 DO - https://doi.org/10.1371/journal.pone.0246511 VL - 16 IS - 2 SP - e0246511 AN - OPUS4-52151 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kupsch, Andreas A1 - Laquai, René A1 - Müller, Bernd R. A1 - Paciornik, S. A1 - Horvath, J. A1 - Tushtev, K. A1 - Rezwan, K. A1 - Bruno, Giovanni T1 - Evolution of Damage in All-Oxide Ceramic Matrix Composite After Cyclic Loading N2 - While structural ceramics usually display a brittle mechanical behavior, their composites may show nonlinearities, mostly due to microcracking. Herein, the stiffness evolution of a sandwich-like laminate of an Al2O3 15%vol. ZrO2 matrix reinforced with Nextel 610 fibers is studied as a function of number of cycles N in tension. The stiffness of the composite degrades with increasing N, indicating microcracking. However, synchrotron X-ray refraction radiography shows that the internal specific surface of such cracks varies differently. A modeling strategy is developed for the calculation of the equivalent stiffness of mixtures (first the matrix and then the sandwich), based on the Voigt and Reuß schemes. The Bruno–Kachanov model is then used to estimate the initial microcrack density in the matrix (due to the thermal expansion mismatch) and the amount of microcracking increase upon cyclic loading. The stiffness in the composite degrades dramatically already after 20 000 cycles but then remains nearly constant. The combination of mechanical testing, quantitative imaging analysis, and modeling provides insights into the damage mechanisms acting: microcrack propagation is more active than microcrack initiation upon cyclic loading, but the second also occurs. This scenario is similar but not equal to previous results on porous and microcracked ceramics. KW - Ceramic matrix composites KW - Homogenization schemes KW - Microcracking KW - Nonlinear behavior KW - Synchrotron X-ray refraction radiography PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534541 DO - https://doi.org/10.1002/adem.202100763 SN - 1527-2648 SN - 1438-1656 VL - 24 IS - 6 SP - 2100763 -1 EP - 2100763 -13 PB - VCH GmbH CY - Weinheim AN - OPUS4-53454 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Marklein, B. A1 - Jenning, M. A1 - Konthur, Zoltán A1 - Häupl, T. A1 - Welzel, F. A1 - Nonhoff, U. A1 - Krobitsch, S. A1 - Mulder, D. M. A1 - Koenders, M. I. A1 - Joshua, V. A1 - Cope, A. P. A1 - Shlomchik, M. J. A1 - Anders, H.-J. A1 - Burmester, G. R. A1 - Hensvold, A. A1 - Catrina, A. I. A1 - Rönnelid, J. A1 - Steiner, G. A1 - Skriner, K. T1 - The citrullinated/native index of autoantibodies against hnRNP-DL predicts an individual "window of treatment success" in RA patients N2 - Background: There is a need for biomarker to identify patients “at risk” for rheumatoid arthritis (risk-RA) and to better predict the therapeutic response and in this study we tested the hypothesis that novel native and citrullinated heterogeneous nuclear ribonucleoprotein (hnRNP)-DL autoantibodies could be possible biomarkers. Methods: Using protein macroarray and ELISA, epitope recognition against hnRNP-DL was analysed in sera from different developed RA disease and diagnosed SLE patients. Toll-like receptor (TLR) 7/9 and myeloid Differentiation primary response gene 88 (MyD88)-dependency were studied in sera from murine disease models. HnRNP-DL expression in cultivated cells and synovial tissue was analysed by indirect immunofluorescence, immunoblot and immunohistochemistry. KW - Citrullinated KW - Rheumatoid arthritis KW - Protein-modification KW - Autoantibodies KW - Antigens PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533682 DO - https://doi.org/10.1186/s13075-021-02603-x SN - 1478-6362 VL - 23 SP - 1 EP - 16 PB - BioMed Central CY - London AN - OPUS4-53368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fritsch, Tobias A1 - Farahbod-Sternahl, L. A1 - Serrano Munoz, Itziar A1 - Léonard, F. A1 - Haberland, C. A1 - Bruno, Giovanni T1 - 3D Computed Tomography Quantifies the Dependence of Bulk Porosity, Surface Roughness, and Re-Entrant Features on Build Angle in Additively Manufactured IN625 Lattice Struts N2 - Layer-by-layer additive manufacturing (AM) by means of laser-powder bed Fusion (L-PBF) offers many prospects regarding the design of lattice structures used, for example, in gas turbines. However, defects such as bulk porosity, Surface roughness, and re-entrant features are exacerbated in nonvertical structures, such as tilted struts. The characterization and quantification of these kinds of defects are essential for the correct estimation of fracture and fatigue properties. Herein, cylindrical struts fabricated by L-PBF are investigated by means of X-ray computed tomography (XCT), with the aim of casting light on the dependence of the three kinds of defects (bulk porosity, surface roughness, and re-entrant features) on the build angle. Innovative analysis methods are proposed to correlate shape and position of pores, to determine the angular-resolved Surface roughness, and to quantify the amount of re-entrant surface features, q. A meshing of the XCT surface enables the correlation of q with the classical Surface roughness Pa. This analysis leads to the conclusion that there is a linear correlation between q and Pa. However, it is conjectured that there must be a threshold of surface roughness, below which no re-entrant features can be build. KW - Additive manufacturing KW - Laser powder bed fusion KW - Computed tomography KW - Surface roughness analysis KW - Re-entrant surface feature PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534728 DO - https://doi.org/10.1002/adem.202100689 IS - 2100689 SP - 1 EP - 8 PB - Wiley-VCH Verlag AN - OPUS4-53472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kardjilov, N A1 - Manke, I A1 - Hilger, A A1 - Arlt, T A1 - Bradbury, R A1 - Markötter, Henning A1 - Woracek, R A1 - Strobel, M A1 - Treimer, W A1 - Banhart, J T1 - The Neutron Imaging Instrument CONRAD — Post‐Operational Review N2 - The neutron imaging instrument CONRAD was operated as a part of the user program of the research reactor BER‐II at Helmholtz‐Zentrum Berlin (HZB) from 2005 to 2020. The Instrument was designed to use the neutron flux from the cold source of the reactor, transported by a curved neutron guide. The pure cold neutron spectrum provided a great advantage in the use of different neutron optical components such as focusing lenses and guides, solid‐state polarizers, Monochromators and phase gratings. The flexible setup of the instrument allowed for implementation of new methods including wavelength‐selective, dark‐field, phase‐contrast and imaging with polarized neutrons. In summary, these developments helped to attract a large number of scientists and industrial customers, who were introduced to neutron imaging and subsequently contributed to the Expansion of the neutron imaging community. KW - Neutron imaging KW - Neutron scattering KW - Neutron instrument KW - Tomography PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534190 DO - https://doi.org/10.3390/ jimaging7010011 VL - 7 IS - 11 SP - 7010011 PB - MDPI AN - OPUS4-53419 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauzon, C. A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Dubiez-Le Goff, S. A1 - Murugesan, S. A1 - Bruno, Giovanni A1 - Hryha, E. T1 - Residual stresses and porosity in Ti-6Al-4V produced by laser powder bed fusion as a function of process atmosphere and component design N2 - The influence of the process gas, laser scan speed, and sample thickness on the build-up of residual stresses and porosity in Ti-6Al-4V produced by laser powder bed fusion was studied. Pure argon and helium, as well as a mixture of those (30% helium), were employed to establish process atmospheres with a low residual Oxygen content of 100 ppm O2. The results highlight that the subsurface residual stresses measured by X-ray diffraction were significantly lower in the thin samples (220 MPa) than in the cuboid samples (645 MPa). This difference was attributed to the shorter laser vector length, resulting in heat accumulation and thus in-situ stress relief. The addition of helium to the process gas did not introduce additional subsurface residual stresses in the simple geometries, even for the increased scanning speed. Finally, larger deflection was found in the cantilever built under helium (after removal from the baseplate), than in those produced under argon and an argon-helium mixture. This result demonstrates that complex designs involving large scanned areas could be subjected to higher residual stress when manufactured under helium due to the gas’s high thermal conductivity, heat capacity, and thermal diffusivity. KW - Additive manufacturing KW - Ti-6Al-4V KW - Residual stress KW - Process atmosphere KW - Helium PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534209 DO - https://doi.org/10.1016/j.addma.2021.102340 VL - 47 SP - 2340 PB - Elsevier B.V. AN - OPUS4-53420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Haeckel, A. A1 - Ascher, Lena A1 - Beindorff, N. A1 - Prasad, S. A1 - Garczynska, K. A1 - Guo, J. A1 - Schellenberger, E. T1 - Long‑circulating XTEN864‑annexin A5 fusion protein for phosphatidylserine‑related therapeutic applications N2 - Annexin A5 (anxA5) is a marker for apoptosis, but has also therapeutic potential in cardiovascular diseases, cancer, and, due to apoptotic mimicry, against dangerous viruses, which is limited by the short blood circulation. An 864-amino-acid XTEN polypeptide was fused to anxA5. XTEN864-anxA5 was expressed in Escherichia coli and purified using XTEN as tag. XTEN864-anxA5 was coupled with DTPA and indium-111. After intravenous or subcutaneous injection of 111In-XTEN864-anxA5, mouse blood samples were collected for blood half-life determination and organ samples for biodistribution using a gamma counter. XTEN864-anxA5 was labeled with 6S-IDCC to confirm binding to apoptotic cells using flow cytometry. To demonstrate targeting of atherosclerotic plaques, XTEN864-anxA5 was labeled with MeCAT(Ho) and administered intravenously to atherosclerotic ApoE−/−mice. MeCAT(Ho)-XTEN864-anxA5 was detected together with MeCAT(Tm)-MAC-2 macrophage antibodies by imaging mass cytometry (CyTOF) of aortic root sections. The ability of anxA5 to bind apoptotic cells was not affected by XTEN864. The blood half-life of XTEN864-anxA5 was 13 h in mice after IV injection, markedly longer than the 7-min half-life of anxA5. 96 h after injection, highest amounts of XTEN864-anxA5 were found in liver, spleen, and kidney. XTEN864-anxA5 was found to target the adventitia adjacent to atherosclerotic plaques. XTEN864-anxA5 is a long-circulating fusion protein that can be efficiently produced in E. coli and potentially circulates in humans for several days, making it a promising therapeutic drug. KW - Programmed cell death KW - LA/ICP-MS Imaging KW - Medicinal application PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533811 DO - https://doi.org/10.1007/s10495-021-01686-w VL - 26 IS - 9-10 SP - 534 EP - 547 PB - Springer AN - OPUS4-53381 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fink, Friedrich A1 - Emmerling, Franziska A1 - Falkenhagen, Jana T1 - Identification and Classification of Technical Lignins by means of Principle Component Analysis and k-Nearest Neighbor Algorithm N2 - The characterization of technical lignins is a key step for the efficient use and processing of this material into valuable chemicals and for quality control. In this study 31 lignin samples were prepared from different biomass sources (hardwood, softwood, straw, grass) and different pulping processes (sulfite, Kraft, organosolv). Each lignin was analysed by attenuated total reflectance Fourier transform infrared (ATR-FT-IR) spectroscopy. Statistical analysis of the ATR-FT-IR spectra by means of principal component analysis (PCA) showed significant differences between the lignins. Hence, the samples can be separated by PCA according to the original biomass. The differences observed in the ATR-FT-IR spectra result primarily from the relative ratios of the p-hydroxyphenyl, guaiacyl and syringyl units. Only limited influence of the pulping process is reflected by the spectral data. The spectra do not differ between samples processed by Kraft or organosolv processes. Lignosulfonates are clearly distinguishable by ATR-FT-IR from the other samples. For the classification a model was created using the k-nearest neighbor (k NN) algorithm. Different data pretreatment steps were compared for k=1…20. For validation purposes, a 5-fold cross-validation was chosen and the different quality criteria Accuracy (Acc), Error Rate (Err), Sensitivity (TPR) and specificity (TNR) were introduced. The optimized model for k=4 gives values for Acc = 98.9 %, Err = 1.1 %, TPR = 99.2 % and TNR = 99.6 %. KW - Classification KW - PCA KW - K-nearest neighbor KW - FT-IR KW - Technical lignin PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533855 DO - https://doi.org/10.1002/cmtd.202100028 VL - 1 IS - 8 SP - 350 EP - 396 PB - Wiley-VCH GmbH AN - OPUS4-53385 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hildebrand, G. A1 - Sänger, Johanna Christiane A1 - Schirmer, U. A1 - Mantei, W. A1 - Dupuis, Y. A1 - Houbertz, R. A1 - Liefeith, K. T1 - Process Development for Additive Manufacturing of Alumina Toughened Zirconia for 3D Structures by Means of Two-Photon Absorption Technique N2 - Additive manufacturing is well established for plastics and metals, and it gets more and more implemented in a variety of industrial processes. Beside these well-established material platforms, additive manufacturing processes are highly interesting for ceramics, especially regarding resource conservation and for the production of complex three-dimensional shapes and structures with specific feature sizes in the µm and mm range with high accuracy. The usage of ceramics in 3D printing is, however, just at the beginning of a technical implementation in a continuously and fast rising field of research and development. The flexible fabrication of highly complex and precise 3D structures by means of light-induced photopolymerization that are difficult to realize using traditional ceramic fabrication methods such as casting and machining is of high importance. Generally, slurry-based ceramic 3D printing technologies involve liquid or semi-liquid polymeric systems dispersed with ceramic particles as feedstock (inks or pastes), depending on the solid loading and viscosity of the system. This paper includes all types of photo-curable polymer-ceramic-mixtures (feedstock), while demonstrating our own work on 3D printed alumina toughened zirconia based ceramic slurries with light induced polymerization on the basis of two-photon absorption (TPA) for the first time. As a proven exemplary on cuboids with varying edge length and double pyramids in the µm-range we state that real 3D micro-stereolithographic fabrication of ceramic products will be generally possible in the near future by means of TPA. This technology enables the fabrication of 3D structures with high accuracy in comparison to ceramic technologies that apply single-photon excitation. In sum, our work is intended to contribute to the fundamental development of this technology for the representation of oxide-ceramic components (proof-of-principle) and helps to exploit the high potential of additive processes in the field of bio-ceramics in the medium to long-term future. KW - Additive manufacturing KW - Ceramics 3D printing KW - Two-photon adsorption KW - Polymer-ceramic mixtures KW - Bio-ceramic engineering PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526672 DO - https://doi.org/10.3390/ceramics4020017 VL - 4 IS - 2 SP - 224 EP - 239 PB - MDPI CY - Basel AN - OPUS4-52667 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Bernd R. A1 - Mack, D. E. A1 - Laquai, René A1 - Kupsch, Andreas A1 - Helle, O. A1 - Sebold, D. A1 - Vaßen, R. A1 - Bruno, Giovanni T1 - Charakterisierung der Porositäts- und Rissdichteentwicklung in Wärmedämmschichten von Gasturbinenschaufeln mittels Synchrotron Refraktions Radiographie N2 - Die Degradation von Wärmedämmschichten(thermal barrier coatings - TBCs) in Gasturbinen durch glasartige Calcium-Magnesium-Aluminiumsilikat (CMAS)Ablagerungen aus verschiedenen Quellen istseit vielen Jahren ein anhaltendes Problem. In dieser Studie wurde mit Hilfe derSynchrotron-Röntgen-Refraktions-Radiographie (SXRR), und vergleichend mit der Elektronenmikroskopie, das Eindringen von CMAS in die poröse Struktur von atmosphärisch plasmagespritzten (APS)TBCs sowie die Bildung und das Wachstum von Rissen unter thermisch zyklischer Belastung untersucht. Die Ergebnisse deuten darauf hin, dass die Infiltration sowie deren Kinetik im Brenner-Teststand wesentlich vom Benetzungsverhalten des CMAS beeinflusst werden. Trotz desoffensichtlichen Angriffs von CMAS auf die Korngrenzen hat die Wechselwirkung von Yttriumdioxid-stabilisiertem Zirkoniumdioxid (YSZ) mit intrudiertem CMAS keinen unmittelbaren Einfluss auf die Struktur und Dichte der innen Oberflächen(Risse, Poren). In einem späteren Stadium wird die Bildung von Rissen senkrecht zur äußeren Oberfläche in einer breiteren Zone der TBC-Schicht beobachtet. T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - CMAS - Calcium-Magnesium-Aluminiumsilikat KW - SXRR - Synchrotron X-ray Refraction Radiography KW - TBC - Thermal barrier coatings PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526732 UR - https://jahrestagung.dgzfp.de/Programm#P32 SP - 1 EP - 15 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-52673 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wosniok, Aleksander A1 - Jansen, R. A1 - Cheng, L. A1 - Chruscicki, Sebastian T1 - Ortsaufgelöste Zustandsüberwachung von Brückenbauwerken mittels faseroptischer Sensoren N2 - In der vorliegenden Studie wurde der Einfluss der statischen Verkehrsbelastung auf die geringen Durchbiegungseffekte in der Betonkonstruktion einer bestehenden Brücke mittels ortsauflösender faseroptischer Sensoren untersucht. Dabei tragen die Ergebnisse der an der Amsterdamer Brücke 705 durchgeführten Belastungstests wesentlich zum Verständnis des Strukturverhaltens bei. Das Konzept der statischen Belastung basierte auf dem Einsatz von zwei 36-Tonnen-Lastwagen, die an mehreren vorbestimmten Stellen auf der Brücke anhielten. Die auf diese Weise aufgebrachte Last führte zu ortsabhängigen kleinen Durchbiegungseffekten, die als lokale Längsdehnung der an der Unterseite der Brücke integrierten Sensorfaser aufgezeichnet wurden. Die reflektometrischen Messungen beruhten auf dem Prinzip genannt TW-COTDR (Tunable Wavelength Coherent Optical Time Domain Reflectometry). Die Messgenauigkeit lag im Bereich von 0,5 µm/m. T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Frequenzbereichsreflektometrie KW - Ortsaufgelöste Fasersensorik KW - Rayleigh-Streuung PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526752 UR - https://jahrestagung.dgzfp.de/Programm#P73 SP - 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-52675 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fahmy, Alaa A1 - Saied, M. A. A. A1 - Morgan, N. A1 - Abdelbary, H. A1 - Bahy, S. M. A1 - Schönhals, Andreas A1 - Friedrich, J. F. T1 - Modified polyvinyl chloride membrane grafted with an ultra-thin polystyrene film: structure and electrochemical properties N2 - The work explores the synthesis and the properties of a novel composite membrane System based on modified polystyrene (PS) grafted onto a polyvinyl chloride (PVC) membrane. PVC membranes were prepared by solution-casting followed by exposure to an atmospheric pressure dielectric barrier discharge (DBD) with O2 to obtain an activated Surface for grafting PS to it. Moreover, the thus prepared membranes were chemically modified furthermore by amination with polyethyleneimine or sulfonation with 4 M sulfuric acid. The membrane surface characteristics such as wettability, structure and morphology were investigated using water contact angle measurements, attenuated total reflection Fourier transform infrared spectroscopy and scanning electron microscopy experiments. The thermogravimetric stability and electrolytic responses of the membranes were studied utilizing TGA, ion exchange capacity (IEC), and solvent uptake. A significant result of plasma and chemical modification was to produce a membrane material with low permeability. Thus, the methanol permeability of the sulfonated membranes measured for 12 h was measured to 2.34$10� 8 cm2 s� 1 compared to 177.00$10� 8 cm2 s� 1 of Nafion 117®which is considered as a benchmark. This result indicates that the prepared sulfonated samples are an innovative and effective material for decreasing the methanol crossover in fuel cells to a great extent. This makes the PVC-g-St membranes are promising and attractive as new materials for polyelectrolyte membrane for fuel cells. KW - Electrolyte membrane KW - Fuell cells PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526794 DO - https://doi.org/10.1016/j.jmrt.2021.04.018 VL - 12 SP - 2273 EP - 2284 PB - Elsevier B.V. AN - OPUS4-52679 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pohl, P. A1 - Kümmel, F. A1 - Schunk, C. A1 - Serrano Munoz, Itziar A1 - Markötter, Henning A1 - Göken, M. A1 - Höppel, H. W. T1 - About the Role of Interfaces on the Fatigue Crack Propagation in Laminated Metallic Composites N2 - The influence of gradients in hardness and elastic properties at interfaces of dissimilar materials in laminated metallic composites (LMCs) on fatigue crack propagation is investigated experimentally for three different LMC systems: Al/Al-LMCs with dissimilar yield stress and Al/Steel-LMCs as well as Al/Ti/Steel-LMCs with dissimilar yield stress and Young’s modulus, respectively. The damage tolerant fatigue behavior in Al/Al-LMCs with an alternating layer structure is enhanced significantly compared to constituent monolithic materials. The prevalent toughening mechanisms at the interfaces are identified by microscopical methods and synchrotron X-ray computed tomography. For the soft/hard transition, crack deflection mechanisms at the vicinity of the interface are observed, whereas crack bifurcation mechanisms can be seen for the hard/soft transition. The crack propagation in Al/Steel-LMCs was studied conducting in-situ scanning electron microscope (SEM) experiments in the respective low cycle fatigue (LCF) and high cycle fatigue (HCF) regimes of the laminate. The enhanced resistance against crack propagation in the LCF regime is attributed to the prevalent stress redistribution, crack deflection, and crack bridging mechanisms. The fatigue properties of different Al/Ti/Steel-LMC systems show the potential of LMCs in terms of an appropriate selection of constituents in combination with an optimized architecture. The results are also discussed under the aspect of tailored lightweight applications subjected to cyclic loading. KW - Laminated metallic composites KW - Toughening mechanisms KW - Interfaces KW - Fatigue crack propagation KW - Fatigue crack growth PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526531 DO - https://doi.org/10.3390/ma14102564 VL - 14 IS - 10 SP - 2564 PB - MDPI AN - OPUS4-52653 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Omar, Hassan A1 - Smales, Glen Jacob A1 - Henning, S. A1 - Li, Z. A1 - Wang, D.-Y. A1 - Schönhals, Andreas A1 - Szymoniak, Paulina T1 - Calorimetric and Dielectric Investigations of Epoxy-Based Nanocomposites with Halloysite Nanotubes as Nanofillers N2 - Epoxy nanocomposites are promising materials for industrial applications (i.e., aerospace, marine and automotive industry) due to their extraordinary mechanical and thermal properties. Here, the effect of hollow halloysite nanotubes (HNT) on an epoxy matrix (Ep) was the focus of the study. The structure and molecular mobility of the nanocomposites were investigated using a combination of X-ray scattering, calorimetry (differential (DSC) and fast scanning calorimetry (FSC)) and dielectric spectroscopy. Additionally, the effect of surface modification of HNT (polydopamine (PDA) and Fe(OH)3 nanodots) was considered. For Ep/HNT, the glass transition temperature (Tg) is was de-creased due to a nanoparticle-related decrease of the crosslinking density. For the modified system, Ep/m-HNT, the surface modification resulted in enhanced filler–matrix interactions leading to higher Tg values than the pure epoxy in some cases. For Ep/m-HNT, the amount of interface formed between the nanoparticles and the matrix ranged from 5% to 15%. Through BDS measurements, localized fluctuations were detected as a β- and γ-relaxation, related to rotational fluctuations of phenyl rings and local reorientations of unreacted components. A combination of calorimetry and BDS dielectric spectroscopy revealed a dynamic and structural heterogeneity of the matrix, as confirmed by two glassy dynamics in both systems, related to regions with different crosslinking densities. KW - Rigid amorphous fraction KW - Epoxy nanocomposites KW - Halloysite nanotubes KW - X-ray scattering KW - Differential scanning calorimetry KW - Broadband dielectric spectroscopy KW - Flash DSC PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526668 DO - https://doi.org/10.3390/polym13101634 VL - 13 IS - 10 SP - 1634 PB - MDPI AN - OPUS4-52666 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heisterkamp, I. A1 - Ratte, M. A1 - Schoknecht, Ute A1 - Gartiser, S. A1 - Kalbe, Ute A1 - Ilvonen, O. T1 - Ecotoxicological evaluation of construction products: inter-laboratory test with DSLT and percolation test eluates in an aquatic biotest battery N2 - Background A European inter-laboratory test with 29 participating laboratories investigated whether a battery of four ecotoxicological tests is suitable for assessing the environmental compatibility of construction products. For this purpose, a construction product was investigated with the dynamic surface leaching test (DIN CEN/TS 16637-2) and the percolation test (DIN CEN/TS 16637-3). The eluates were produced centrally by one laboratory and were tested by the participants using the following biotests: algae test (ISO 8692), acute daphnia test (ISO 6341), luminescent bacteria test (DIN EN ISO 11348), and fish egg test (DIN EN ISO 15088). As toxicity measures, EC50 and LID values were calculated. Results Toxic effects of the eluates were detected by all four biotests. The bacteria test was by far the most sensitive, followed by the algae test and the daphnia test; the fish egg test was the least sensitive for eluates of both leaching tests. The toxicity level of the eluates was very high in the bacteria, daphnia, and algae test, with lowest ineffective dilution values of LID = 70 to LID = 13,000 and corresponding EC50 values around or even below 1 volume percent. The reproducibility (approximated by interlaboratory variability) of the biotests was good (< 53%) to very good (< 20%), regardless of the toxicity level of the eluates. The reproducibility of the algae test was up to 80%, and thus still acceptable. Conclusion It can be confirmed that the combination of leaching and ecotoxicity tests is suitable to characterize with sufficient reproducibility the environmental impact posed by the release of hazardous substances from construction products. KW - Inter-laboratory test KW - Construction products KW - Leaching tests KW - Ecotoxicity tests KW - Grouts PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529198 DO - https://doi.org/10.1186/s12302-021-00514-x VL - 33 IS - 1 SP - Article number: 75 PB - Springer AN - OPUS4-52919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mirabella, Francesca A1 - Müllner, M. A1 - Touzalin, T. A1 - Riva, M. A1 - Jakub, Z. A1 - Kraushofer, F. A1 - Schmid, M. A1 - Koper, M. T. M. A1 - Parkinson, G. S. A1 - Diebold, U. T1 - Ni-modified Fe3O4(001) surface as a simple model system for understanding the oxygen evolution reaction N2 - Electrochemical water splitting is an environmentally friendly technology to store renewable energy in the form of chemical fuels. Among the earth-abundant first-row transition metal-based catalysts, mixed Ni-Fe oxides have shown promising performance for effective and low-cost catalysis of the oxygen evolution reaction (OER) in alkaline media, but the synergistic roles of Fe and Ni cations in the OER mechanism remain unclear. In this work, we report how addition of Ni changes the reactivity of a model iron oxide catalyst, based on Ni deposited on and incorporated in a magnetite Fe3O4(001) single crystal, using a combination of surface science techniques in ultra-high vacuum such as low energy electron diffraction (LEED), x-ray photoelectron spectroscopy (XPS), low-energy ion scattering (LEIS), and scanning tunneling microscopy (STM), as well as atomic force microscopy (AFM) in air, and electrochemical Methods such as cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) in alkaline media. A significant improvement in the OER activity is observed when the top surface presents an iron fraction among the cations in the range of 20-40%, which is in good agreement with what has been observed for powder catalysts. Furthermore, a decrease in the OER overpotential is observed following surface aging in electrolyte for three days. At higher Ni load, AFM shows the growth of a new phase attributed to an (oxy)-hydroxide phase which, according to CV measurements, does not seem to correlate with the surface activity towards OER. EIS suggests that the OER precursor species observed on the clean and Ni-modified surfaces are similar and Fe-centered, but form at lower overpotentials when the surface Fe:Ni ratio is optimized. We propose that the well-defined Fe3O4(001) surface can serve as a model System for understanding the OER mechanism and establishing the structure-reactivity relation on mixed Fe-Ni oxides. KW - OER KW - Fe-Ni oxides KW - Surface science KW - Electrochemistry KW - Water splitting PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529231 UR - https://www.sciencedirect.com/science/article/pii/S0013468621009282?via%3Dihub DO - https://doi.org/10.1016/j.electacta.2021.138638 VL - 389 SP - 138638 PB - Elsevier Ltd. AN - OPUS4-52923 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Rabin, Ira ED - Raggetti, L. T1 - Material Studies of Historic Inks: Transition from Carbon to Iron-Gall Inks N2 - This chapter offers observations and considerations concerning black writing inks encountered in writing supports transmitting documentary and literary texts of the late Antiquity and early Middle Ages. It discusses different types of inks, the Methods of their detection and their use in different times and geographical areas. KW - Material analysis KW - Writing inks KW - Ink fingerprint PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528057 DO - https://doi.org/10.1163/9789004444805_006 SP - 70 EP - 78 PB - Brill CY - Leiden AN - OPUS4-52805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Boaretto, E. A1 - Newman, H. A1 - Shevchuk, I. A1 - Breterniz, S. A1 - Rabin, Ira T1 - Date, Materiality and Historical Significance of P.Köln Inv. 5941 N2 - The paper presents the results of the radiocarbon dating and ink analysis of a leather fragment bearing an important liturgical text in Hebrew from the early centuries of the common era. The work initiated by the scholarly interest in the text stresses the importance of the date and materiality of the manuscripts and closes with an appeal to the curators of manuscript collections. KW - Mixed ink KW - Radiocarbon KW - Leather PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528063 DO - https://doi.org/10.25592/uhhfdm.8471 VL - 6/2 SP - 173 EP - 186 AN - OPUS4-52806 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wurzler, Nina A1 - Schütter, Jan David A1 - Wagner, R. A1 - Dimper, Matthias A1 - Hodoroaba, Vasile-Dan A1 - Lützenkirchen-Hecht, D. A1 - Özcan Sandikcioglu, Özlem T1 - Preconditioning of AISI 304 stainless steel surfaces in the presence of flavins—Part II: Effect on biofilm formation and microbially influenced corrosion processes N2 - Biofilm formation and microbially influenced corrosion of the iron-reducing microorganism Shewanella putrefaciens were investigated on stainless steel surfaces preconditioned in the absence and presence of flavin molecules by means of XANES (X-ray absorption near-edge structure) analysis and electrochemical methods. The results indicate that biofilm formation was promoted on samples preconditioned in electrolytes containing minute amounts of flavins. On the basis of the XANES results, the corrosion processes are controlled by the iron-rich outer layer of the passive film. Biofilm formation resulted in a cathodic shift of the open circuit potential and a protective effect in terms of pitting corrosion. The samples preconditioned in the absence of flavins have shown delayed pitting and the samples preconditioned in the presence of flavins did not show any pitting in a window of −0.3- to +0.0-V overpotential in the bacterial medium. The results indicate that changes in the passive film chemistry induced by the presence of minute amounts of flavins during a mild anodic polarization can change the susceptibility of stainless steel surfaces to microbially influenced corrosion. KW - Biofilms KW - XANES KW - Microbially influenced corrosion (MIC) PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528130 DO - https://doi.org/10.1002/maco.202012192 VL - 72 IS - 6 SP - 983 EP - 994 PB - Wiley AN - OPUS4-52813 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wipfler, B. A1 - Bradler, S. A1 - Büsse, S. A1 - Hammel, J. A1 - Müller, Bernd R. A1 - Pass, G. T1 - Evolutionary morphology of the antennal heart in stick and leaf insects (Phasmatodea) and webspinners (Embioptera) (Insecta: Eukinolabia) N2 - The morphology of the antennal hearts in the head of Phasmatodea and Embioptera was investigated with particular reference to phylogenetically relevant key taxa. The antennal circulatory organs of all examined species have the same basic construction: they consist of antennal vessels that are connected to ampullae located in the head near the antenna base. The ampullae are pulsatile due to associated muscles, but the points of attachment differ between the species studied. All examined Phasmatodea species have a Musculus (M.) interampullaris which extends between the two ampullae plus a M. ampulloaorticus that runs from the ampullae to the anterior end of the aorta; upon contraction, all these muscles dilate the lumina of both ampullae at the same time. In Embioptera, only the australembiid Metoligotoma has an M. interampullaris. All other studied webspinners instead have a M. ampullofrontalis which extends between the ampullae and the frontal region of the head capsule; these species do not have M. ampulloaorticus. Outgroup comparison indicates that an antennal heart with a M. interampullaris is the plesiomorphic character state among Embioptera and the likely ground pattern of the taxon Eukinolabia. Antennal hearts with a M. ampullofrontalis represent a derived condition that occurs among insects only in some embiopterans. These findings help to further clarify the controversially discussed internal phylogeny of webspinners by supporting the view that Australembiidae are the sister group of the remaining Embioptera. KW - Phylogeny KW - Polyneoptera KW - Metoligotoma PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527795 DO - https://doi.org/10.1007/s00435-021-00526-4 SN - 1432-234X VL - 140 IS - 3 SP - 331 EP - 340 PB - Springer AN - OPUS4-52779 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xu, R. A1 - Teich, W. A1 - Frenzel, Florian A1 - Hoffmann, Katrin A1 - Radke, J. A1 - Rösler, J. A1 - Faust, K. A1 - Blank, A. A1 - Brandenburg, S. A1 - Misch, M. A1 - Vajkoczy, P. A1 - Onken, J. S. A1 - Resch-Genger, Ute T1 - Optical characterization of sodium fluorescein in vitro and ex vivo N2 - Objective: The utilization of fluorescein-guided biopsies and resection has been recently discussed as a suitable strategy to improve and expedite operative techniques for the resection of central nervous system (CNS) tumors. However, little is known about the optical properties of sodium fluorescein (NaFl) in human tumor tissue and their potential impact on ex vivo analyses involving fluorescence-based methods. Methods: Tumor tissue was obtained from a study cohort of an observational study on the utilization of fluorescein-guided biopsy and resection (n=5). The optical properties of fluorescein-stained tissue were compared to the optical features of the dye in vitro and in control samples consisting of tumor tissue of high-grade glioma patients (n=3) without intravenous (i.v.) application of NaFl. The dye-exposed tumor tissues were used for optical measurements to confirm the detectability of NaFl emission ex vivo. The tissue samples were fixed in 4%PFA, immersed in 30% sucrose, embedded in Tissue-Tek OCT compound, and cut to 10 mm cryosections. Spatially resolved emission spectra from tumor samples were recorded on representative slides with a Confocal Laser Scanning Microscope FV1000 (Olympus GmbH, Hamburg, Germany) upon excitation with lexc = 488 nm. Results: Optical measurements of fluorescein in 0.9% sodium chloride (NaCl) under in vitro conditions showed an absorption maximum of lmax abs = 479 nm as detected with spectrophotometer Specord 200 and an emission peak at lmax em = 538 nm recorded with the emCCD detection system of a custom-made microscope-based single particle setup using a 500 nm long-pass filter. Further measurements revealed pH- and concentration-dependent emission spectra of NaFl. Under ex vivo conditions, confocal laser scanning microscopy of fluorescein tumor samples revealed a slight bathochromic shift and a broadening of the emission band. Conclusion: Tumor uptake of NaFl leads to changes in the optical properties – a bathochromic shift and broadening of the emission band – possibly caused by the dye’s high pH sensitivity and concentration-dependent reabsorption acting as an innerfilter of the dye’s emission, particularly in the short wavelength region of the Emission spectrum where absorption and fluorescence overlap. Understanding the ex vivo optical properties of fluorescein is crucial for testing and validating its further applicability as an optical probe for intravital microscopy, immunofluorescence localization studies, and flow cytometry analysis. KW - Fluorescence KW - Optical probe KW - Sensor KW - Fluorescein KW - PH KW - Imaging KW - Tissue KW - Cancer KW - Medical diagnostics KW - Tumor KW - In vivo KW - Ex vivo KW - Quantum yield KW - Dye KW - Quality assurance KW - Microscopy PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527843 DO - https://doi.org/10.3389/fonc.2021.654300 SN - 2234-943X VL - 11 SP - 1 EP - 8 PB - Frontiers Media CY - Lausanne AN - OPUS4-52784 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fürst, Richard A1 - Fürst, E. A1 - Vlach, T. A1 - Repka, J. A1 - Pokorny, M. A1 - Mozer, V. T1 - Use of Cement Suspension as an Alternative Matrix Material for Textile-Reinforced Concrete N2 - Textile-reinforced concrete (TRC) is a material consisting of high-performance concrete (HPC) and tensile reinforcement comprised of carbon roving with epoxy resin matrix. However, the problem of low epoxy resin resistance at higher temperatures persists. In this work, an alternative to the epoxy resin matrix, a non-combustible cement suspension (cement milk) which has proven stability at elevated temperatures, was evaluated. In the first part of the work, microscopic research was carried out to determine the distribution of particle sizes in the cement suspension. Subsequently, five series of plate samples differing in the type of cement and the method of textile reinforcement saturation were designed and prepared. Mechanical experiments (four-point bending tests) were carried out to verify the properties of each sample type. It was found that the highest efficiency of carbon roving saturation was achieved by using finer ground cement (CEM 52.5) and the pressure saturation method. Moreover, this solution also exhibited the best results in the four-point bending test. Finally, the use of CEM 52.5 in the cement matrix appears to be a feasible variant for TRC constructions that could overcome problems with its low temperature resistance. KW - Textile-reinforced concrete KW - High-performance concrete KW - Carbon fibers KW - Cement matrix PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527100 DO - https://doi.org/10.3390/ma14092127 SN - 1996-1944 VL - 14 IS - 9 SP - 2127 PB - MDPI CY - Basel AN - OPUS4-52710 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reuter, T. A1 - Plotzki, David A1 - Borges de Oliveira, F. A1 - Hausotte, T. T1 - Simulative Untersuchung des Einflusses von Bildrauschen auf dimensionelle Messungen mit industriellen Computertomografen N2 - Die industrielle Röntgen-Computertomografie (CT) etabliert sich für die Anwendung in der dimensionellen Messtechnik. Sie bietet als zerstörungsfreies Messverfahren das Potential, sowohl innen- als auch außenliegende Merkmale holistisch zu erfassen. Für die Bestimmung der Güte eines Messwerts muss die dem Messwert zugeordnete Messunsicherheit ermittelt werden. Dabei kann, nach derzeitigem Stand der Technik und Normung, die aufgabenspezifische Messunsicherheit nach VDI/VDE 2630 Blatt 2.1 nur unter hohem Aufwand mit einer Vielzahl an experimentellen Wiederholmessungen ermittelt werden. Ziel diverser Forschungs-projekte zu diesem Thema ist es daher, eine numerische Messunsicherheitsbestimmung zu erreichen. Dafür ist es notwendig, alle signifikanten Einflussgrößen zu erfassen, deren Unsicherheitsbeiträge zu bestimmen und zu bewerten. In diesem Beitrag wird der Einfluss des Bildrauschens auf verschiedene dimensionelle Messgrößen simulativ untersucht. Mithilfe eines prismatischen Prüfkörpers, der eine Vielzahl an Geometrieelementen aufweist, werden verschiedene Messgrößen unterschiedlicher Komplexität betrachtet. Ziel ist es, für diese Messgrößen zu testen, wie diese auf das Bildrauschen reagieren. Dieses wird dabei durch das Signal-Rausch-Verhältnis (SNR) der Projektionsgrauwerte beschrieben und variiert. Es werden Wiederholsimulationen durchgeführt, damit eine statistische Aussage über die Verteilung der Messwerte möglich ist und der Einfluss des Rauschens auf verschiedene Messgrößen individuell beurteilt werden kann. Das Simulationsszenario wird so gestaltet, dass lediglich das Bildrauschen Einfluss auf die Messung hat. Die berechneten Verteilungsbreiten lassen mit sinkendem SNR eine deutliche Zunahme erkennen, insbesondere bei der Bestimmung von Formabweichungen. Simuliert wird mit der Software aRTist 2.10 (BAM). T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Rauschen KW - Computertomografie KW - Dimensionelle Messung KW - Simulation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527144 SP - 1 EP - 11 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung e.V. (DGZfP) CY - Berlin AN - OPUS4-52714 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schwabe, M. A1 - Griep, S. A1 - Schmidtberg, H. A1 - Plarre, Rüdiger A1 - Goesmann, A. A1 - Vilcinskas, A. A1 - Vogel, H. A1 - Brinkrolf, K. T1 - Next-Generation Sequencing Analysis of the Tineola bisselliella Larval Gut Transcriptome Reveals Candidate Enzymes for Keratin Digestion N2 - The clothes moth Tineola bisselliella is one of a few insects that can digest keratin, leading to the destruction of clothing, textiles and artwork. The mechanism of keratin digestion is not yet fully understood, partly reflecting the lack of publicly available genomic and transcriptomic data. Here we present a high-quality gut transcriptome of T. bisselliella generated from larvae reared on keratin-rich and keratin-free diets. The overall transcriptome consists of 428,221 contigs that were functionally annotated and screened for candidate enzymes involved in keratin utilization. As a mechanism for keratin digestion, we identified cysteine synthases, cystathionine β-synthases and cystathionine γ-lyases. These enzymes release hydrogen sulfite, which may reduce the disulfide bonds in keratin. The dataset also included 27 differentially expressed contigs with trypsin domains, among which 20 were associated with keratin feeding. Finally, we identified seven collagenases that were upregulated on the keratin-rich diet. In addition to this enzymatic repertoire potentially involved in breaking down keratin, our analysis of poly(A)-enriched and poly(A)-depleted transcripts suggested that T. bisselliella larvae possess an unstable intestinal microbiome that may nevertheless contribute to keratin digestion KW - Insect biotechnology KW - Gene expression KW - RNA-Sequencing KW - Transcriptomics KW - Tineola bisselliella KW - Keratin PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529902 DO - https://doi.org/10.3390/genes12081113 VL - 12 IS - 8 SP - 1113 PB - MDPI AN - OPUS4-52990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaeger, Carsten A1 - Ritter, D. A1 - Goeritzer, M. A1 - Thiele, A. A1 - Blumrich, A. A1 - Beyhoff, N. A1 - Luettges, K. A1 - Smeir, E. A1 - Kasch, J. A1 - Grune, J. A1 - Müller, O. A1 - Klopfleisch, R. A1 - Foryst-Ludwig, A. A1 - Kintscher, U. T1 - Liver X Receptor Agonist AZ876 Induces Beneficial Endogenous Cardiac Lipid Reprogramming and Protects Against Isoproterenol-Induced Cardiac Damage N2 - Background - It is known that dietary intake of polyunsaturated fatty acids may improve cardiac function. However, relatively high daily doses are required to achieve sufficient cardiac concentrations of beneficial omega‐3 fatty acids. The liver X receptor (LXR) is a nuclear hormone receptor and a crucial regulator of lipid homeostasis in mammals. LXR activation has been shown to endogenously reprogram cellular lipid profiles toward increased polyunsaturated fatty acids levels. Here we studied whether LXR lipid reprogramming occurs in cardiac tissue and exerts cardioprotective actions. Methods and Results - Male 129SV mice were treated with the LXR agonist AZ876 (20 µmol/kg per day) for 11 days. From day 6, the mice were injected with the nonselective β‐agonist isoproterenol for 4 consecutive days to induce diastolic dysfunction and subendocardial fibrosis while maintaining systolic function. Treatment with isoproterenol led to a marked impairment of global longitudinal strain and the E/e' ratio of transmitral flow to mitral annular velocity, which were both significantly improved by the LXR agonist. Histological examination showed a significant reduction in isoproterenol‐induced subendocardial fibrosis by AZ876. Analysis of the cardiac lipid composition by liquid chromatography‐high resolution mass spectrometry revealed a significant increase in cardiac polyunsaturated fatty acids levels and a significant reduction in saturated fatty acids by AZ876. Conclusions - The present study provides evidence that the LXR agonist AZ876 prevents subendocardial damage, improves global longitudinal strain and E/e' in a mouse model of isoproterenol‐induced cardiac damage, accompanied by an upregulation of cardiac polyunsaturated fatty acids levels. Cardiac LXR activation and beneficial endogenous cardiac lipid reprogramming may provide a new therapeutic strategy in cardiac disease with diastolic dysfunction. KW - Heart failure KW - Lipids KW - Liver X receptor KW - Diastolic dysfunction KW - Nuclear receptor PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529352 DO - https://doi.org/10.1161/JAHA.120.019473 VL - 10 IS - 14 SP - e019473 AN - OPUS4-52935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friberg, I. A1 - Clark, A. H. A1 - Ho, P. A1 - Sadokhina, N. A1 - Smales, Glen Jacob A1 - Woo, J. A1 - Auray, X. A1 - Ferri, D. A1 - Nachtegaal, M. A1 - Krocher, O. A1 - Olsson, L. T1 - Structure and performance of zeolite supported Pd for complete methane oxidation N2 - The influence of zeolite support materials and their impact on CH4 oxidation activity was studied utilizing Pd supported on H-beta and H-SSZ-13. A correlation between CH4 oxidation activity, Si/Al ratio (SAR), the type of zeolite framework, reduction-oxidation behaviour, and Pd species present was found by combining catalytic activity measurements with a variety of characterization methods (operando XAS, NH3-TPD, SAXS, STEM and NaCl titration). Operando XAS analysis indicated that catalysts with high CH4 oxidation activity experienced rapid transitions between metallic- and oxidized-Pd states when switching between rich and lean conditions. This behaviour was exhibited by catalysts with dispersed Pd particles. By contrast, the formation of ion-exchanged Pd2+ and large Pd particles appeared to have a detrimental effect on the oxidation-reduction behaviour and the conversion of CH4. The formation of ion-exchanged Pd2+ and large Pd particles was limited by using a highly siliceous beta zeolite support with a low capacity for cation exchange. The same effect was also found using a small-pore SSZ-13 zeolite due to the lower mobility of Pd species. It was found that the zeolite support material should be carefully selected so that the well-dispersed Pd particles remain, and the formation of ion-exchanged Pd2+ is minimized. KW - SAXS KW - Zeolites KW - Methane Oxidation KW - XAS KW - Catalysis PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529606 DO - https://doi.org/10.1016/j.cattod.2020.11.026 VL - 382 SP - 3 EP - 12 PB - Elsevier B.V. AN - OPUS4-52960 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Christoph A1 - Firdous, R. A1 - Kruschwitz, Sabine A1 - Stephan, D. T1 - Sequential learning to accelerate discovery of alkali-activated binders N2 - Alkali-activated binders (AAB) can provide a clean alternative to conventional cement in terms of CO2 emissions. However, as yet there are no sufficiently accurate material models to effectively predict the AAB properties, thus making optimal mix design highly costly and reducing the attractiveness of such binders. This work adopts sequential learning (SL) in high-dimensional material spaces (consisting of composition and processing data) to find AABs that exhibit desired properties. The SL approach combines machine learning models and feedback from real experiments. For this purpose, 131 data points were collected from different publications. The data sources are described in detail, and the differences between the binders are discussed. The sought-after target property is the compressive strength of the binders after 28 days. The success is benchmarked in terms of the number of experiments required to find materials with the desired strength. The influence of some constraints was systematically analyzed, e.g., the possibility to parallelize the experiments, the influence of the chosen algorithm and the size of the training data set. The results show the advantage of SL, i.e., the amount of data required can potentially be reduced by at least one order of magnitude compared to traditional machine learning models, while at the same time exploiting highly complex information. This brings applications in laboratory practice within reach. KW - Alkali-activated binders KW - Machine learning KW - Sequential learning KW - Materials by design KW - Materials informatics PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531376 DO - https://doi.org/10.1007/s10853-021-06324-z SN - 0022-2461 SN - 1573-4803 VL - 56 SP - 15859 EP - 15881 PB - Springer CY - Dordrecht AN - OPUS4-53137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reichelt, Manuel A1 - Cappella, Brunero T1 - Micro- and nanowear of self-mated steel generated and studied with an AFM at the single asperity level N2 - We show for the first time tribotests performed with self-mated 100Cr6 steel, taking advantage of an AFM, employed as a tribometer for the tribotests as well as for the inspection of wear of both tribopartners. Emphasis is put on the morphology of the scars, on wear particles, and on wear of the “colloidal” particles glued on the AFM cantilever. Measurements demonstrate the possibility of characterizing single asperity events leading to very small wear. We highlight several phenomena, which are elementary key constituents of tribological processes. Such phenomena, probably occurring also at the macroscale, can be detected, identified, and characterized with high spatial and time resolution only at the nanoscale, thus giving insight into conditions and causes of their emergence. KW - Nanowear KW - Atomic force microscope KW - 100Cr6 (AISI 52100) steel KW - Wear particles KW - Single asperity contact KW - Particle transfer KW - Zero wear PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531389 DO - https://doi.org/10.3389/fmech.2021.722434 SN - 2297-3079 VL - 7 SP - 1 EP - 16 PB - Frontiers Media CY - Lausanne AN - OPUS4-53138 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mirtsch, Mona A1 - Blind, K. A1 - Koch, Claudia A1 - Dudek, Gabriele T1 - Information security management in ICT and non-ICT sector companies: A preventive innovation perspective N2 - Despite the growing dependence of companies on information technology and the increasingly negative impact of security incidents worldwide, there is little research on the management of information security at the company level. This paper seeks to expand knowledge on the implementation of an information security management system based on the widely used international standard ISO/IEC 27001. We present motives, experienced impacts, and obstacles related to ISO/IEC 27001 implementation using data from a survey of 125 ISO/IEC 27001 certified companies in Germany. Since adoption rates vary between ICT and non-ICT sector companies, we highlight sector-related variations. We classify the adoption of this standard as a preventive organizational innovation and apply Structural Equation Modeling to unearth explanations for the comparatively low adoption of this management system standard among companies outside the ICT sector. We, therefore, derive recommendations for policymakers, standardization, and certification bodies to foster its diffusion. KW - Information Security KW - ISO/IEC 27001 KW - Management system standard KW - Certification KW - Information security management system (ISMS) KW - Preventive Innovation KW - Resource-based-view KW - Institutional theory PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531037 DO - https://doi.org/10.1016/j.cose.2021.102383 SN - 0167-4048 VL - 109 IS - 10 SP - 1 EP - 23 PB - Elsevier Ltd. AN - OPUS4-53103 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Magkos, Sotirios A1 - Kupsch, Andreas A1 - Bruno, Giovanni T1 - Suppression of Cone-Beam Artefacts with Direct Iterative Reconstruction Computed Tomography Trajectories (DIRECTT) N2 - The reconstruction of cone-beam computed tomography data using filtered back-projection algorithms unavoidably results in severe artefacts. We describe how the Direct Iterative Reconstruction of Computed Tomography Trajectories (DIRECTT) algorithm can be combined with a model of the artefacts for the reconstruction of such data. The implementation of DIRECTT results in reconstructed volumes of superior quality compared to the conventional algorithms. KW - DIRECTT KW - Iterative method KW - Signal processing KW - X-ray imaging KW - Computed tomography PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531085 DO - https://doi.org/10.3390/jimaging7080147 SN - 2313-433X) VL - 7 IS - 8 SP - 147 - 1 EP - 147 -9 PB - MDPI CY - Basel, Switzerland AN - OPUS4-53108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martynec, T. A1 - Karapanagiotis, Christos A1 - Klapp, S. H. L. A1 - Kowarik, S. T1 - Machine learning predictions of surface migration barriers in nucleation and non-equilibrium growth N2 - Machine learning is playing an increasing role in the discovery of new materials and may also facilitate the search for optimum growth conditions for crystals and thin films. Here, we perform kinetic Monte-Carlo simulations of sub-monolayer growth. We consider a generic homoepitaxial growth scenario that covers a wide range of conditions with different diffusion barriers (0.4–0.55 eV) and lateral binding energies (0.1–0.4 eV). These simulations are used as a training data set for a convolutional neural network that can predict diffusion barriers and binding energies. Specifically, a single Monte-Carlo image of the morphology is sufficient to determine the energy barriers with an accuracy of approximately 10 meV and the neural network is tolerant to images with noise and lower than atomic-scale resolution. We believe this new machine learning method will be useful for fundamental studies of growth kinetics and growth optimization through better knowledge of microscopic parameters. KW - Machine learning KW - Surface migration barriers KW - Material engineering PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532523 UR - https://www.nature.com/articles/s43246-021-00188-1 DO - https://doi.org/10.1038/s43246-021-00188-1 SN - 2662-4443 VL - 2 SP - 1 EP - 9 PB - Springer Nature CY - London AN - OPUS4-53252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, Z. A1 - Villa Santos, C. A1 - Legrand, A. A1 - Haase, F. A1 - Hara, Y. A1 - Kanamori, K. A1 - Aoyama, T. A1 - Urayama, K. A1 - Doherty, C. M. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Colon, Y. J. A1 - Furukawa, S. T1 - Multiscale structural control of linked metal–organic polyhedra gel by aging-induced linkage-reorganization N2 - Assembly of permanently porous metal–organic polyhedra/cages (MOPs) with bifunctional linkers leads to soft supramolecular networks featuring both porosity and processability. However, the amorphous nature of such soft materials complicates their characterization and thus limits rational structural control. Here we demonstrate that aging is an effective strategy to control the hierarchical network of supramolecular gels, which are assembled from organic ligands as linkers and MOPs as junctions. Normally, the initial gel formation by rapid gelation leads to a kinetically trapped structure with low controllability. Through a controlled post-synthetic aging process, we show that it is possible to tune the network of the linked MOP gel over multiple length scales. This process allows control on the molecular-scale rearrangement of interlinking MOPs, mesoscale fusion of colloidal particles and macroscale densification of the whole colloidal network. In this work we elucidate the relationships between the gel properties, such as porosity and rheology, and their hierarchical structures, which suggest that porosity measurement of the dried gels can be used as a powerful tool to characterize the microscale structural transition of their corresponding gels. This aging strategy can be applied in other supramolecular polymer systems particularly containing kinetically controlled structures and shows an opportunity to engineer the structure and the permanent porosity of amorphous materials for further applications. KW - SAXS KW - Metal-organic polyhedra KW - Structural control PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532309 DO - https://doi.org/10.1039/d1sc02883a SN - 1478-6524 SN - 1742-2183 VL - 12 IS - 38 SP - NIL_1 EP - NIL_9 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-53230 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Khrapov, D. A1 - Kozadayeva, M. A1 - Manabaev, K. A1 - Panin, A. A1 - Sjöström, W. A1 - Koptyug, A. A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Meinel, Dietmar A1 - Bruno, Giovanni A1 - Cheneler, D. A1 - Surmenev, R. A1 - Surmeneva, M. T1 - Different approaches for manufacturing Ti-6Al-4V alloy with triply periodic minimal surface sheet-based structures by electron beam melting N2 - Targeting biomedical applications, Triply Periodic Minimal Surface (TPMS) gyroid sheet-based structures were successfully manufactured for the first time by Electron Beam Melting in two different production Themes, i.e., inputting a zero (Wafer Theme) and a 200 µm (Melt Theme) wall thickness. Initial assumption was that in both cases, EBM manufacturing should yield the structures with similar mechanical properties as in a Wafer-mode, as wall thickness is determined by the minimal beam spot size of ca 200 µm. Their surface morphology, geometry, and mechanical properties were investigated by means of electron microscopy (SEM), X-ray Computed Tomography (XCT), and uniaxial tests (both compression and tension). Application of different manufacturing Themes resulted in specimens with different wall thicknesses while quasi-elastic gradients for different Themes was found to be of 1.5 GPa, similar to the elastic modulus of human cortical bone tissue. The specific energy absorption at 50% strain was also similar for the two types of structures. Finite element simulations were also conducted to qualitatively analyze the deformation process and the stress distribution under mechanical load. Simulations demonstrated that in the elastic regime wall, regions oriented parallel to the load are primarily affected by deformation. We could conclude that gyroids manufactured in Wafer and Melt Themes are equally effective in mimicking mechanical properties of the bones. KW - Electron beam melting KW - Scaffold KW - Lightweight structures KW - Computed tomography PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531595 DO - https://doi.org/10.3390/ma14174912 SN - 1996-1944 VL - 14 IS - 17 SP - 1 EP - 21 PB - MDPI CY - Basel AN - OPUS4-53159 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schraut, Katharina A1 - Kargl, F. A1 - Adam, Christian A1 - Ivashko, O. T1 - In situ synchrotron XRD measurements during solidification of a melt in the CaO–SiO2 system using an aerodynamic levitation system N2 - Phase formation and evolution was investigated in the CaO–SiO2 system in the range of 70–80 mol% CaO. The samples were container-less processed in an aerodynamic levitation system and crystallization was followed in situ by synchrotron x-ray diffraction at the beamline P21.1 at the German electron synchrotron (DESY). Modification changes of di- and tricalcium silicate were observed and occurred at lower temperatures than under equilibrium conditions. Despite deep sample undercooling, no metastable phase formation was observed within the measurement timescale of 1 s. For the given cooling rates ranging from 300 K s−1 to about 1 K s−1, no decomposition of tricalcium silicate was observed. No differences in phase evolution were observed between reducing and oxidizing conditions imposed by the levitation gas (Ar and Ar + O2). We demonstrate that this setup has great potential to follow crystallization in refractory oxide liquids in situ. For sub-second primary phase formation faster detection and for polymorph detection adjustments in resolution have to be implemented. KW - Aerodynamic levitation KW - Calcium silicate KW - Phase formation KW - Oxide melts KW - In situ synchrotron x-ray diffraction PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526952 DO - https://doi.org/10.1088/1361-648X/abf7e1 VL - 33 IS - 26 SP - 264003 (12pp) PB - IOP Publishing AN - OPUS4-52695 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Rhode, Michael A1 - Wetzel, Annica A1 - Oczan, Ozlem A1 - Nietzke, Jonathan A1 - Richter, Tim A1 - Schröpfer, Dirk T1 - Corrigendum: Hydrogen diffusion and local Volta potential in high- and medium-entropy alloys (2020 IOP Conf. Ser.: Mater. Sci. Eng. 882 012015) N2 - In the sub-section “2.1 Investigated materials” the chemical composition of Co, Cr and Mn was in wrong order for both HEA and MEA. The content of table 1 is here included in the correct version. PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527050 DO - https://doi.org/10.1088/1757-899X/882/1/012027 VL - 882 SP - 1 EP - 2 PB - IOP Publishing CY - Bristol AN - OPUS4-52705 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kauss, Norman A1 - Heyn, A. A1 - Michael, O. A1 - Schymura, M. A1 - Rosemann, P. T1 - Application limits and sensitisation behaviour of the manganese- and nitrogen-alloyed austenitic stainless steel P2000 (X13CrMnMoN18-14-3) N2 - Nickel‐free high‐nitrogen‐alloyed stainless steels like the P2000 (X13CrMnMoN18‐14‐3) were developed to enhance the strength and corrosion resistance of austenitic stainless steels like 304 and 316 while keeping the typical high ductility. The mechanical and corrosive properties of P2000 were investigated and compared with 304 and 316 to highlight the application opportunities of this new alloy. The microstructure of the solution‐annealed condition was characterised by electron backscatter diffraction and the mechanical properties were studied by uniaxial tensile tests, Charpy impact tests and hardness measurements. The passivation behaviour was analysed using the electrochemical potentiodynamic reactivation, whereas the pitting corrosion resistance was compared by pitting potentials and pitting temperatures. However, secondary thermal influences or suboptimal heat treatment can impair the corrosion resistance due to the precipitation of secondary phases and the resulting sensitisation. Thermodynamic calculations and artificial ageing treatment in the range of 500–900°C for up to 100 h were used to determine critical time–temperature parameters for sensitisation. The microstructure of the various aged states was evaluated by scanning electron microscopy and compared with the degrading corrosion resistance characterised by the KorroPad method. KW - Austenitic stainless steel KW - Electrochemical methods KW - High‐nitrogen steel KW - Mechanical properties KW - Corrosion resistance PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527925 DO - https://doi.org/10.1002/maco.202112450 VL - 71 IS - 10 SP - 1656 EP - 1667 PB - Wiley-VCH GmbH AN - OPUS4-52792 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulze-Makuch, D. A1 - Lipus, D. A1 - Arens, F. L. A1 - Baque, M. A1 - Bornemann, T. L. V. A1 - de Vera, J. P. A1 - Flury, M. A1 - Froesler, J. A1 - Heinz, J. A1 - Hwang, Y. A1 - Kounaves, S. P. A1 - Mangelsdorf, K. A1 - Meckenstock, R. U. A1 - Pannekens, M. A1 - Probst, A. J. A1 - Saenz, J. S. A1 - Schirmack, J. A1 - Schloter, M. A1 - Schmitt-Kopplin, P. A1 - Schneider, Beate A1 - Uhl, J. A1 - Vestergaard, G. A1 - Valenzuela, B. A1 - Zamorano, P. A1 - Wagner, D. T1 - Microbial hotspots in lithic microhabitats inferred from DNA fractionation and metagenomics in the Atacama Desert N2 - The existence of microbial activity hotspots in temperate regions of Earth is driven by soil heterogeneities, especially the temporal and spatial availability of nutrients. Here we investigate whether microbial activity hotspots also exist in lithic microhabitats in one of the most arid regions of the world, the Atacama Desert in Chile. While previous studies evaluated the total DNA fraction to elucidate the microbial communities, we here for the first time use a DNA separation approach on lithic microhabitats, together with metagenomics and other analysis methods (i.e., ATP, PLFA, and metabolite analysis) to specifically gain insights on the living and potentially active microbial community. Our results show that hypolith colonized rocks are microbial hotspots in the desert environment. In contrast, our data do not support such a conclusion for gypsum crust and salt rock environments, because only limited microbial activity could be observed. The hypolith community is dominated by phototrophs, mostly Cyanobacteria and Chloroflexi, at both study sites. The gypsum crusts are dominated by methylotrophs and heterotrophic phototrophs, mostly Chloroflexi, and the salt rocks (halite nodules) by phototrophic and halotolerant endoliths, mostly Cyanobacteria and Archaea. The major environmental constraints in the organic-poor arid and hyperarid Atacama Desert are water availability and UV irradiation, allowing phototrophs and other extremophiles to play a key role in desert ecology. KW - Desert ecology KW - Extremophile KW - Hyperarid PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527959 DO - https://doi.org/10.3390/microorganisms9051038 SN - 2076-2607 VL - 9 IS - 5 SP - 1038 PB - MDPI CY - Basel AN - OPUS4-52795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, Xin A1 - Niederleithinger, Ernst A1 - Hindersmann, Iris T1 - The installation of embedded ultrasonic transducers inside a bridge to monitor temperature and load influence using coda wave interferometry technique N2 - This article presents a unique method of installing a special type of embedded ultrasonic transducers inside a 36-m-long section of an old bridge in Germany. A small-scale load test was carried out by a 16 ton truck to study the temperature and load influence on the bridge, as well as the performance of the embedded transducers. Ultrasonic coda wave interferometry technique, which has high sensitivity in detecting subtle changes in a heterogeneous medium, was used for the data evaluation and interpretation. The separation of two main influence factors (load effect and temperature variation) is studied, and future applications of wave velocity variation rate Φ for structural health condition estimation are discussed. As a preliminary research stage, the installation method and the performance of the ultrasonic transducer are recognized. Load- and temperature-induced weak wave velocity variations are successfully detected with a high resolution of 10−4%. The feasibility of the whole system for long-term structural health monitoring is considered, and further research is planned. KW - Ultrasound KW - Bridge KW - Monitoring KW - coda wave interferometry KW - embedded PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527978 DO - https://doi.org/10.1177/14759217211014430 SN - 1475-9217 VL - 21 IS - 3 SP - 913 EP - 927 PB - SAGE AN - OPUS4-52797 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Evsevleev, Sergei A1 - Mishurova, Tatiana A1 - Khrapov, D. A1 - Paveleva, A. A1 - Meinel, Dietmar A1 - Surmenev, R. A1 - Surmeneva, M. A1 - Koptyug, A. A1 - Bruno, Giovanni T1 - X-ray Computed Tomography Procedures to Quantitatively Characterize the Morphological Features of Triply Periodic Minimal Surface Structures N2 - Additively manufactured (AM) metallic sheet-based Triply Periodic Minimal Surface Structures (TPMSS) meet several requirements in both bio-medical and engineering fields: Tunable mechanical properties, low sensitivity to manufacturing defects, mechanical stability, and high energy absorption. However, they also present some challenges related to quality control, which can prevent their successful application. In fact, the optimization of the AM process is impossible without considering structural characteristics as manufacturing accuracy, internal defects, as well as surface topography and roughness. In this study, the quantitative non-destructive analysis of TPMSS manufactured from Ti-6Al-4V alloy by electron beam melting was performed by means of X-ray computed tomography (XCT). Several advanced image analysis workflows are presented to evaluate the effect of build orientation on wall thicknesses distribution, wall degradation, and surface roughness reduction due to the chemical etching of TPMSS. It is shown that the manufacturing accuracy differs for the structural elements printed parallel and orthogonal to the manufactured layers. Different strategies for chemical etching show different powder removal capabilities and both lead to the loss of material and hence the gradient of the wall thickness. This affects the mechanical performance under compression by reduction of the yield stress. The positive effect of the chemical etching is the reduction of the surface roughness, which can potentially improve the fatigue properties of the components. Finally, XCT was used to correlate the amount of retained powder with the pore size of the functionally graded TPMSS, which can further improve the manufacturing process. KW - Metamaterials KW - Functionally graded porous structure KW - Triply periodic minimal surface structures KW - Roughness analysis KW - Powder removal KW - Deep learning segmentation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528142 DO - https://doi.org/10.3390/ma14113002 VL - 14 IS - 11 SP - 3002 PB - MDPI AN - OPUS4-52814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lugovtsova, Yevgeniya A1 - Bulling, Jannis A1 - Mesnil, O. A1 - Prager, Jens A1 - Gohlke, Dirk A1 - Boller, C. T1 - Damage quantification in an aluminium-CFRP composite structure using guided wave wavenumber mapping: Comparison of instantaneous and local wavenumber analyses N2 - Composite-overwrapped pressure vessels (COPV) are increasingly used in the transportation industry due to their high strength to mass ratio. Throughout the years, various designs were developed and found their applications. Currently, there are five designs, which can be subdivided into two main categories - with a load-sharing metal liner and with a non-load-sharing plastic liner. The main damage mechanism defining the lifetime of the first type is fatigue of the metal liner, whereas for the second type it is fatigue of the composite overwrap. Nevertheless, one damage type which may drastically reduce the lifetime of COPV is impact-induced damage. Therefore, this barely visible damage needs to be assessed in a non-destructive way to decide whether the pressure vessel can be further used or has to be put out of service. One of the possible methods is based on ultrasonic waves. In this contribution, both conventional ultrasonic testing (UT) by high-frequency bulk waves and wavenumber mapping by low frequency guided waves are used to evaluate impact damage. Wavenumber mapping techniques are first benchmarked on a simulated aluminium panel then applied to experimental measurements acquired on a delaminated aluminium-CFRP composite plate which corresponds to a structure of COPV with a load-sharing metal liner. The analysis of experimental data obtained from measurements of guided waves propagating in an aluminium-CFRP composite plate with impact-induced damage is performed. All approaches show similar performance in terms of quantification of damage size and depths while being applied to numerical data. The approaches used on the experimental data deliver an accurate estimate of the in-plane size of the large delamination at the aluminium-CFRP interface but only a rough estimate of its depth. Moreover, none of the wavenumber mapping techniques used in the study can quantify every delamination between CFRP plies caused by the impact, which is the case for conventional UT. This may be solved by using higher frequencies (shorter wavelengths) or more advanced signal processing techniques. All in all, it can be concluded that imaging of complex impact damage in fibre-reinforced composites based on wavenumber mapping is not straightforward and stays a challenging task. KW - Ultrasonic guided waves KW - Instantaneous wavenumber analysis KW - Local wavenumber analysis KW - Signal processing PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528203 DO - https://doi.org/10.1016/j.ndteint.2021.102472 SN - 0963-8695 VL - 122 SP - 2472 PB - Elsevier Ltd. CY - Amsterdam, Netherlands AN - OPUS4-52820 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tschöke, K. A1 - Müller, I. A1 - Memmolo, V. A1 - Moix-Bonet, M. A1 - Moll, J. A1 - Lugovtsova, Yevgeniya A1 - Golub, M. A1 - Sridaran Venkat, R. A1 - Schubert, L. T1 - Feasibility of Model-Assisted Probability of Detection Principles for Structural Health Monitoring Systems based on Guided Waves for Fibre-Reinforced Composites N2 - In many industrial sectors, Structural Health Monitoring (SHM) is considered as an addition to Non-Destructive Testing (NDT) that can reduce maintenance effort during lifetime of a technical facility, structural component or vehicle. A large number of SHM methods is based on ultrasonic waves, whose properties change depending on structural health. However, the wide application of SHM systems is limited due to the lack of suitable methods to assess their reliability. The evaluation of the system performance usually refers to the determination of the Probability of Detection (POD) of a test procedure. Up to now, only few limited methods exist to evaluate the POD of SHM systems, which prevent them from being standardised and widely accepted in industry. The biggest hurdle concerning the POD calculation is the large amount of samples needed. A POD analysis requires data from numerous identical structures with integrated SHM systems. Each structure is then damaged at different locations and with various degrees of severity. All of this is connected to high costs. Therefore, one possible way to tackle this problem is to perform computer-aided investigations. In this work, the POD assessment procedure established in NDT according to the Berens model is adapted to guided wave-based SHM systems. The approach implemented here is based on solely computer-aided investigations. After efficient modelling of wave propagation phenomena across an automotive component made of a carbon fibre-reinforced composite, the POD curves are extracted. Finally, the novel concept of a POD map is introduced to look into the effect of damage position on system reliability. KW - Reliability KW - Acoustics KW - Monitoring KW - Automotive engineering KW - Elastodynamic Finite Inegration Technique PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528218 DO - https://doi.org/10.1109/TUFFC.2021.3084898 VL - 68 IS - 10 SP - 3156 EP - 3173 AN - OPUS4-52821 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph T1 - Quantification of the Knudsen Effect on the Effective Gas diffusion Coefficient in Partially Saturated Pore Distributions N2 - The effective gas diffusion coefficient describes the process of gas diffusion in porous materials. Several materials have a significant number of micropores in the lower nanometre range leading to a reduction of gas diffusion (Knudsen effect). In the case of partial pore saturation during adsorption, the available pore space is further reduced, as is the gas diffusion. In this study, the influence of partially saturated pores on the Knudsen effect and on the gas diffusion is quantified. Three different pore geometries are investigated (slit, cylindrical and spherical pores) and three different types of pore size distribution, including a broad equal distribution, three narrow normal distributions and two measured distributions of concrete. Besides the intensive computation of the exact pore saturation, a simplified model with low computational requirements is suggested. This study shows that the influence of the water layer thickness on the effective diffusion becomes significant for pore radii below 50 nm and the assumed pore geometry is important. At the end, the overall effect is quantified for an amorphous material with most pore radii below 30 nm. At a moisture level of 50% relative humidity, the effective diffusion is reduced by 35% due to partial saturation. KW - Effective gas diffusion coefficient KW - Gas transport in porous media KW - Knudsen diffusion KW - Moisture transport KW - Nanopores PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528509 DO - https://doi.org/10.1002/adem.202100106 VL - 23 IS - 10 SP - 2100106 PB - Wiley AN - OPUS4-52850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Churiaque, C. A1 - Sanchez-Amaya, J.M. A1 - Üstündag, Ömer A1 - Porrua-Lara, M. A1 - Gumenyuk, Andrey A1 - Rethmeier, Michael T1 - Improvements of hybrid laser arc welding for shipbuilding T-joints with 2F position of 8 mm thick steel N2 - the joints throughout the structure. The flat units are constituted by butt welded flat plates, on which longitudinal T-welded reinforcements are placed to rigidize the structure. Among the different welding technologies, Hybrid Laser Arc Welding (HLAW) is becoming a mature process, profitable and highly productive. In addition, more innovative welding equipment are being developed nowadays, offering greater work flexibility, and raising expectations of achieving better quality, and economic viability. Another key point of HLAW to keep in mind is that structural distortions are reduced, resulting in decreasing the cost and time of straightening work. In the present contribution, the influence of HLAW parameters on the quality of fillet joints of naval steel has been analysed. Experimental HLAW tests were performed with a high power disk laser to join EH36 naval steel plates, with a T configuration. The influence of different processing parameters has been analysed, as the laser power, welding speed, wire feed rate and the configuration of the HLAW processes (including head angle and laser/arc leading process). In addition, FEM simulations were carried out in order to estimate residual stresses and distortion of welded part. The distortion values provided by FEM presented excellent agreement with the measured experimental results. To evaluate the welds, non destructive tests including X-ray tests, metallographic analysis of cross sections, and microhardness mapping tests were performed. Full penetration 8 mm T welds were obtained for the first time at an industrially applicable 2F position with a reasonable HLAW head angle, in one single step without sealing root, and using zero gap square groove Edge preparation. The present contribution presents welding rates up to 2.2 m/min for 2F T-joints of this steel thickness, a much higher processing velocity than previously reported for industrial applications. KW - Hybrid laser arc welding PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528410 DO - https://doi.org/10.1016/j.optlastec.2021.107284 VL - 143 SP - 1 EP - 20 PB - Elsevier Ltd. AN - OPUS4-52841 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bennet, Francesca A1 - Burr, L. A1 - Schmid, D. A1 - Hodoroaba, Vasile-Dan T1 - Towards a method for quantitative evaluation of nanoparticle from suspensions via microarray printing and SEM analysis N2 - As part of the development of a library of accurate and efficient methods for measurement of nanoparticle properties, we develop and optimize a method for the efficient analysis of nanoparticle size distribution from suspensions via microprinting and digital analysis of electron microscopy (SEM and TEM) images, with the ultimate aim of automated quantitative concentration analysis (calculated from drop volume). A series of different nanoparticle suspensions (gold, latex, and SiO2 in varying sizes and concentrations) were printed onto TEM grids in a 4 x 4 array in the concentration range 7x10^8 to 1x10^11 nanoparticles/mL and imaged with SEM. Concentrations and printing conditions (temperature, relative humidity) were varied in order to minimize the coffee-ring effect. KW - Nanoparticles KW - Particle size distribution KW - Electron microscopy KW - Microarray printing KW - Sample preparation KW - Nanoparticle concentration PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528455 DO - https://doi.org/10.1088/1742-6596/1953/1/012002 VL - 1953 SP - 012002 PB - IOP Publishing AN - OPUS4-52845 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mundra, Shishir A1 - Provis, J. L. T1 - Mechanisms of passivation and chloride-induced corrosion of mild steel in sulfide-containing alkaline solutions N2 - The pore fluid within many concretes is highly alkaline and rich in reduced sulfur species, but the influence of such alkaline-sulfide solutions on the surface film formed on steel reinforcement is poorly understood. This study investigates the critical role of HS− in defining mild steel passivation chemistry. The surface film formed on the steel in alkaline-sulfide solutions contains Fe(OH)2 and Fe–S complexes, and the critical chloride concentration to induce corrosion increases at high sulfide concentration. However, this behavior is dependent on the duration of exposure of the steel to the electrolyte, and the nature of the sulfidic surface layer. KW - Alkali-activated materials KW - Steel corrosion KW - Sulfide KW - Chloride PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528861 DO - https://doi.org/10.1007/s10853-021-06237-x VL - 56 IS - 26 SP - 14783 EP - 14802 PB - Springer Nature AN - OPUS4-52886 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - James, G. L. A1 - Latif, M. T. A1 - Isa, M. N. M. A1 - Bakar, M. F. A. A1 - Yusuf, N. Y. M. A1 - Broughton, William A1 - Murad, A. M. A1 - Abu Bakar, F. D. T1 - Metagenomic datasets of air samples collected during episodes of severe smoke-haze in Malaysia N2 - Transboundary emissions of smoke-haze from land and forest fires have recurred annually during the dry period (June to October, over the past few decades) in South East Asia. Hazardous air quality has been recorded in Malaysia during these episodes. Agricultural practices such as slash-and-burn of biomass and peat fires particularly in Sumatera and Kalimantan, Indonesia, have been implicated as the major causes of the haze. Past findings have shown that a diversity of microbes can thrive in air including in smoke-haze polluted air. In this study, metagenomic data were generated to reveal the diversity of microorganisms in air during days with and without haze. Air samples were collected during non-haze (2013A01) and two haze (2013A04 and 2013A05) periods in the month of June 2013. DNA was extracted from the samples, subjected to Multiple Displacement Amplification and whole genome sequencing (Next Generation Sequencing) using the HiSeq 2000 Platform. Extensive bio-informatic analyses of the raw sequence data then followed. Raw reads from these six air samples were deposited in the NCBI SRA databases under Bioproject PRJNA662021 with accession numbers SRX9087478, SRX9087479 and SRX9087480. KW - Forest fires KW - Haze Samples KW - NGS KW - Multiple Displacement Amplification PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528973 DO - https://doi.org/10.1016/j.dib.2021.107124 SN - 2352-3409 VL - 36 SP - 107124 PB - Elsevier Inc. CY - Amsterdam, Netherlands AN - OPUS4-52897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kraus, David A1 - Trappe, Volker T1 - Transverse damage in glass fiber reinforced polymer under thermo-mechanical loading N2 - In this study, the thermomechanical damage behavior of a glass fiber reinforced polymer material is investigated. The coefficients of thermal expansion of the composite as well as the matrix are measured in a wide temperature range. Quasi-static experiments with neat resin, unidirectional and multidirectional laminates are performed as well as fatigue experiments in a temperature range from 213 K to 343 K. This study focusses on the matrix damage due to fiber-parallel loading. A correlation between matrix effort, the dilatational strain energy of the matrix and the damage state of the specimen is demonstrated. It is shown that a fatigue life assessment can be performed with the aid of a temperature-independent master fatigue curve. KW - Composite KW - Glass fiber reinforced polymer KW - Thermo-mechanics KW - Fatigue KW - Damage KW - Temperature PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527462 DO - https://doi.org/10.1016/j.jcomc.2021.100147 SN - 2666-6820 VL - 5 SP - 100147 PB - Elsevier B.V. AN - OPUS4-52746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wallau, Wilma A1 - Recknagel, Christoph A1 - Smales, Glen Jacob T1 - Structural silicone sealants after exposure to laboratory test for durability assessment N2 - During the service life of structural sealant glazing (SSG) facades, the loadbearing capacity of the silicone bonds needs to be guaranteed. Laboratory Tests can assess the durability of SSG-systems based on mechanical characteristics of the bond after simultaneous exposure to both climatic and mechanical loads. This article studies how the material characteristics of two common structural sealants are affected by laboratory and field exposure. Dynamic mechanical Analysis (DMA) confirms a reduction in the dynamic modulus of exposed Silicone samples. Results from thermogravimetric analysis, Fourier-transform infrared spectroscopy, differential scanning calorimetry, and small-angle X-ray scattering/wide-angle X-ray scattering show differences between the two sealants and indicate no/minor changes in the composition and morphology of the laboratory and field exposed sealants. Mechanical characterization methods, such as DMA, and tensile and shear testing of the structural bond, are shown to be sensitive toward the combined climatic and mechanical loadings, and are hence suitable for studying degradation mechanisms of structural sealants. KW - Aging KW - Analytical methods KW - Fatigue KW - Silicone elastomer KW - Structural sealant glazing PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527217 DO - https://doi.org/10.1002/app.50881 VL - 138 IS - 35 SP - 50881 PB - Wiley AN - OPUS4-52721 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schaupp, Thomas A1 - Schröder, Nina A1 - Schröpfer, Dirk A1 - Kannengießer, Thomas T1 - Hydrogen-Assisted Cracking in GMA Welding of High-Strength Structural Steel—A New Look into This Issue at Narrow Groove N2 - Modern arc processes, such as the modified spray arc (Mod. SA), have been developed for gas metal arc welding of high-strength structural steels with which even narrow weld seams can be welded. High-strength joints are subjected to increasingly stringent requirements in terms of welding processing and the resulting component performance. In the present work, this challenge is to be met by clarifying the influences on hydrogen-assisted cracking (HAC) in a high-strength structural steel S960QL. Adapted samples analogous to the self-restraint TEKKEN test are used and analyzed with respect to crack formation, microstructure, diffusible hydrogen concentration and residual stresses. The variation of the seam opening angle of the test seams is between 30° and 60°. To prevent HAC, the effectiveness of a dehydrogenation heat treatment (DHT) from the welding heat is investigated. As a result, the weld metals produced at reduced weld opening angle show slightly higher hydrogen concentrations on average. In addition, increased micro- as well as macro-crack formation can be observed on these weld metal samples. On all samples without DHT, cracks in the root notch occur due to HAC, which can be prevented by DHT immediately after welding. KW - High-strength structural steel KW - Gas metal arc welding KW - Diffusible hydrogen KW - Hydrogen-assisted cracking KW - TEKKEN KW - Residual stresses KW - Weld metal cracking PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527260 DO - https://doi.org/10.3390/met11060904 VL - 11 IS - 6 SP - 904 PB - MDPI CY - Basel AN - OPUS4-52726 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlick-Hasper, Eva A1 - Bruchno, Martin A1 - Thomas, Goedecke T1 - Release of Powdery or Granular Substances from Intact Dangerous Goods Bags During Road Transport - Analysis of the Causes and Development of a Test Concept N2 - The leaks of dangerous goods from actually intact bags detected in the years 2018 to 2020 tend to be at an almost constant high level. These releases of powdery or granular dangerous goods represent violations of the sift-proofness required in the dangerous goods regulations. This article first analyzes the causes. The components of the bags that are affected by leaks are micro-perforations, joins and closures, in particular internal sleeve valves. A distinction must be made between bags closed in conformity with or contrary to the manufacturer's instructions. The particle release is determined by a number of influencing factors of the filling substance, the packaging and other boundary conditions. Therefore, a comprehensive test concept is developed in this work, which takes all these factors into account. The application of this test concept facilitates the planning of the test setup and the experiments. On this basis, the complex mechanisms involved in the release of solid substances can be systematically investigated in the test laboratory. To prevent releases of powdery or granular substances from intact bags, it is necessary that the user has access to the closing instructions and the relevant properties of the test substance used for the design type approval. Further experimental investigations are needed to assess whether filling substances change their properties during transport and whether this enables them to escape. KW - Bags KW - Dangerous goods packagings KW - Leak KW - Particles KW - Sift-proofness PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527287 DO - https://doi.org/10.1002/pts.2575 SN - 0894-3214 VL - 34 IS - 7 SP - 435 EP - 446 PB - Wiley AN - OPUS4-52728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steiner, S. A1 - Heldt, J. A1 - Sobol, Oded A1 - Unger, Wolfgang A1 - Frömeling, T. T1 - Influence of oxygen vacancies on core-shell formation in solid solutions of (Na,Bi)TiO3 and SrTiO3 N2 - Solid solutions of (Na,Bi)TiO3 (NBT) and SrTiO3 (ST) are materials of interest for high-strain or high-energy density capacitor applications. Often, they exhibit chemical heterogeneity and develop core-shell structures during regular solid-state synthesis with an NBT-rich core. In this case, the NBT forms first so that the strontium needs to diffuse into the material to reach chemical homogeneity. Depending on the presence of core-shell structures, the electrical properties can vary drastically. In this work, we rationalize the effect of variations in oxygen vacancy concentration by Fe-acceptor and Nb-donor doping. It can be shown that a diffusion couple of strontium and oxygen is responsible for chemical homogenization and that the oxygen vacancy content can control the formation of a core-shell structure. KW - Lead-free ceramics KW - Bismuth titanates KW - Core-shell structures KW - Diffusion/diffusivity KW - Ferroelectricity/ferroelectric materials PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525988 DO - https://doi.org/10.1111/jace.17845 SP - 1 EP - 10 PB - Wiley Periodicals LLC, John Wiley & Sons, Inc. AN - OPUS4-52598 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Valet, Svenja A1 - Burkert, Andreas A1 - Ebell, Gino A1 - Babutzka, Martin T1 - Determination of the corrosion product layer resistance on zinc and electrolytically galvanized steel samples by using gel electrolytes N2 - Although zinc and zinc coatings have been widely used for corrosion protection for decades new zinc coatings are constantly being developed. Characterizing the corrosion protectiveness of these new coatings, however, should not be underestimated. While exposure tests are time intensive, cyclic tests can only be used for a very limited field of application. Thus, electrochemical measurements provide both an efficient and an effective alternative. Conventional aqueous bulk electrolytes influence the surface layers of a tested zinc coating and are therefore not reliable. Gel electrolytes, however, have evolved over the last few years, are minimally invasive and provide reliable results. This work describes experiments with gel electrolytes made of agar. Unlike previous work, it proposes a composition of gel electrolyte for minimally invasive description of the protective power of naturally formed oxide layers on zinc and zinc coatings. Therefore, as a first part, the gel electrolyte made of agar is verified as a method for zinc and zinc-coated samples. Afterwards, this paper introduces the corrosion product layer resistance RL as a promising parameter to evaluate the protective power of zinc coatings. Results are verified with EIS and FTIR measurements. An example on a representative zinc coating demonstrates the practical application. KW - Gel electrolytes KW - Agar KW - Zinc coatings KW - Atmospheric exposure KW - Corrosion PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526053 DO - https://doi.org/10.1016/j.electacta.2021.138191 SN - 0013-4686 VL - 385 SP - 138191 PB - Elsevier Ltd. AN - OPUS4-52605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Horf, M. A1 - Gebbers, R. A1 - Vogel, S. A1 - Ostermann, Markus A1 - Piepel, M.-F. A1 - Olfs, H.-W. T1 - Determination of Nutrients in Liquid Manures and Biogas Digestates by Portable Energy-Dispersive X-ray Fluorescence Spectrometry N2 - Knowing the exact nutrient composition of organic fertilizers is a prerequisite for their appropriate application to improve yield and to avoid environmental pollution by over-fertilization. Traditional standard chemical analysis is cost and time-consuming and thus it is unsuitable for a rapid analysis before manure application. As a possible alternative, a handheld X-ray fluorescence (XRF) spectrometer was tested to enable a fast, simultaneous, and on-site analysis of several elements. A set of 62 liquid pig and cattle manures as well as biogas digestates were collected, intensively homogenized and analysed for the macro plant nutrients phosphorus, potassium, magnesium, calcium, and sulphur as well as the micro nutrients manganese, iron, copper, and zinc using the standard lab procedure. The effect of four different sample preparation steps (original, dried, filtered, and dried filter residues) on XRF measurement accuracy was examined. Therefore, XRF results were correlated with values of the reference analysis. The best R2 s for each element ranged from 0.64 to 0.92. Comparing the four preparation steps, XRF results for dried samples showed good correlations (0.64 and 0.86) for all elements. XRF measurements using dried filter residues showed also good correlations with R2 s between 0.65 and 0.91 except for P, Mg, and Ca. In contrast, correlation Analysis for liquid samples (original and filtered) resulted in lower R2 s from 0.02 to 0.68, except for K (0.83 and 0.87, respectively). Based on these results, it can be concluded that handheld XRF is a promising measuring system for element analysis in manures and digestates. KW - XRF KW - Animal slurry KW - Fertilizer KW - Soil KW - Precision farming PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527622 DO - https://doi.org/10.3390/s21113892 VL - 21 IS - 11 SP - 3892 PB - MDPI CY - Basel, Switzerland AN - OPUS4-52762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Keshmiri, Hamid A1 - Armin, F. A1 - Elsayad, K. A1 - Schreiber, Frank A1 - Moreno, M. T1 - Leaky and waveguide modes in biperiodic holograms N2 - This study details a theoretical analysis of leaky and waveguide modes in biperiodic all-dielectric holograms. By tuning diffraction orders and subsequently confining local density of optical states at two distinct resonance wavelengths, we present a new class of highly sensitive refractive index biosensing platforms that are capable of resolving 35.5 to 41.3 nm/RIU of spectral shift for two separate biological analytes. KW - Antimicrobial resistance KW - Bacteria KW - Photonics KW - Diffractive gratings PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527632 DO - https://doi.org/10.1038/s41598-021-89971-1 SN - 2045-2322 (online) VL - 11 IS - 1 SP - 10991 PB - Springer Nature AN - OPUS4-52763 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 -