TY - JOUR A1 - Palkowski, Carsten A1 - Schwarzenberg, S. A1 - Simo, Anne T1 - Seasonal cooling performance of air conditioners: The importance of independent test procedures used for MEPS and labels N2 - Minimum energy performance standards and labels are commonly used tools to reduce the household energy use thus mitigating greenhouse gas emissions. However, the technical foundation for minimum energy performance standards and labels are test procedures for rating and testing of appliances. To de- termine the seasonal cooling performance of air conditioners, the current test standards require fixing of the compressor speed of the units to achieve steady-state conditions; this way of operation, how- ever, differs from real-life use. To make the seasonal cooling performance testing better reflect the real use conditions, this study proposes a compensation method which can be conducted independently from manufacturer data and still allows modulation of the tested units. Our results show that the tested units behave differently under part-load conditions, which results in a lower energy efficiency rating for some of the tested devices. KW - Air conditioner KW - Independent test method KW - Real use behavior KW - Seasonal energy efficiency ratio KW - Minimum energy performance standards KW - Energy label PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-485813 DO - https://doi.org/10.1016/j.ijrefrig.2019.05.021 SN - 0140-7007 VL - 104 SP - 417 EP - 425 PB - Elsevier AN - OPUS4-48581 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Knieschewski, Arno A1 - Stamminger, R. A1 - Simo, Anne T1 - Cost analysis of screening methods to find non-compliant models using the example of tumble dryers N2 - The European energy label was established to reduce energy consumption in Europe. All classes and values on the energy label are stated by the supplier. The task of market surveillance is to ensure correct labels and to validate their values through compliance tests. However, this can only be done for a small fraction of all models on the market, since physical tests are expensive. Screening methods can be used to narrow down the number of critical products before compliance tests are done to decrease the costs of finding non-compliant models. This study shows a mathematical approach to analyze the cost benefits of screening methods to find non-compliant models. Furthermore, the analysis presented has been applied to 18 screening methods for tumble dryers. The performance test for tumble dryers consists of seven test runs. All screening methods evaluated are composed of a reduced number of test runs. The most efficient screening method reduces the surveillance costs by 40 %. KW - Screening method KW - Market surveillance KW - Tumble dryer KW - Energy label PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-486762 DO - https://doi.org/10.1007/s12053-019-09805-y SN - 1570-646X SN - 1570-6478 VL - 12 IS - 7 SP - 1707 EP - 1715 PB - Springer CY - Dordrecht AN - OPUS4-48676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Liehr, Sascha A1 - Münzenberger, Sven A1 - Krebber, Katerina T1 - Wavelength-scanning distributed acoustic sensing for structural monitoring and seismic applications N2 - We introduce wavelength-scanning coherent optical time domain reflectometry (WS-COTDR) for dynamic vibration sensing along optical fibers. The method is based on spectral shift computation from Rayleigh backscatter spectra. Artificial neural networks (ANNs) are used for fast and high-resolution strain computation from raw measurement data. The applicability of the method is demonstrated for vibration monitoring of a reinforced concrete bridge. We demonstrate another application example for quasi-static and dynamic measurement of ground deformation and surface wave propagation along a dark fiber in a telecommunication cable. T2 - 7th International Symposium on Sensor Science CY - Napoli, Italy DA - 09.05.2019 KW - Optical fiber sensor KW - Distributed acoustic sensor (DAS) KW - Optical time domain reflectometry KW - Rayleigh scattering KW - Artificial neural networks KW - Structural health monitoring KW - Seismic measurement PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-487733 DO - https://doi.org/10.3390/proceedings2019015030 SN - 2504-3900 VL - 15 SP - Paper 30, 1 EP - 5 PB - MDPI CY - Basel AN - OPUS4-48773 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Ronald T1 - Effect of repair models on risk based optimal inspection strategies for support structures of offshore wind turbines N2 - Owners or operators of offshore wind farms perform inspections to collect information on the condition of the wind turbine support structures and perform repairs if required. These activities are costly and should be optimized. Risk-based methods can be applied to identify inspection and repair strategies that ensure an optimal balance between the expected total service life cost of inspection and repair, and the achieved risk reduction. Such an optimization requires explicit modeling of repairs. In this paper, the impact of different repair models on the results of a risk-based optimization of inspection and repair strategies is quantified in a numerical example considering a jacket-type steel frame subject to high-cycle fatigue. The example showed that, in this specific application, there is no need for detailed modeling of the behavior of repaired welded connections. T2 - 5th International Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures (SMAR 2019) CY - Potsdam, Germany DA - 27.08.2019 KW - Risk KW - Reliability KW - Inspection planning KW - Offshore wind turbines PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-488297 UR - https://www.smar2019.org/Portals/smar2019/bb/Th.2.A.4.pdf SP - Paper Th.2.A.4, 1 EP - 8 AN - OPUS4-48829 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hüsken, Götz A1 - Shamsuddoha, Md A1 - Thiele, Marc A1 - Baeßler, Matthias A1 - Kühne, Hans-Carsten T1 - Comparison of cracks formed in scaled grouted connection of offshore energy structures under static and cyclic loads N2 - Global energy consumption will increase in the future necessitating both fossil fuels and renewable energy choices - especially wind energy. Such high energy demand requires installation of offshore energy structures, rigs, platforms and towers, which are susceptible to adverse environmental conditions along with maintenances. Due to their large size and remote locations, cylindrical grouted joints are often adopted between substructure and foundation in these offshore platforms and wind structures such as monopiles. However, these connections are composite structures with exterior sleeve, interior pile and infill mortar. Degradation and settlements were reported inside similar connections, which were installed in last three decades. Besides, grouting in the offshore sites were proven difficult to obtain ideal load bearing capacity. In-situ loading conditions were also found to be affecting the failure mechanism inside such connections. This study aims at characterizing the nature of cracks generated in these grouted connections under both static and cyclic loading. Scaled grouted joints were manufactured using a novel reusable mold, and connections were loaded to failure to visualize the main failure patterns. An assessment between failure under these two types of load is drawn along with comparison to previously available literature. T2 - 5th International Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures CY - Potsdam, Germany DA - 27.08.2019 KW - Grouted connection KW - Crack formation KW - Crack pattern KW - Static load KW - Cyclic load PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-487961 SP - Th.2.A.1-1 EP - Th.2.A.1-9 AN - OPUS4-48796 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kullolli, Borana A1 - Cuéllar, Pablo A1 - Baeßler, Matthias A1 - Stutz, H. H. T1 - Modelling and calibration for cyclic soil-structure interface behaviour N2 - The structural performance of many geotechnical systems (e.g. axially-loaded pile foundations), depends on the shearing resistance at the soil interface, which may govern the load bearing capacity of the foundation. Experimental investigations have shown that this interaction is mainly localised within a narrow shear band next to the structure. Under cyclic loading, a contraction of the soil at the interface may arise (net volume loss), possibly leading to a stress relaxation and thus to a reduction of the load bearing capacity (the so-called friction fatigue). Based on the constitutive similarities between soil continua and interfaces, we propose here the adaption of a Generalized Plasticity model for sandy soils for the numerical analysis of interface problems. In this contribution, the results of an experimental campaign for the parameter calibration of the constitutive model are presented. The tests have been conducted with a ring shear device involving different normal stresses, roughness of the steel plates as well as cyclic loading. The new modelling approach shows promising results and has the additional practical advantage that the interface zone and the soil continuum can both be described with the same constitutive model in general boundary value problems. T2 - Konferenz 7th International Symposium on Deformation Characteristics of Geomaterials CY - Glasgow, Scotland DA - 26.06.2019 KW - Soil-structure interaction KW - Offshore foundations PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-489096 DO - https://doi.org/10.1051/e3sconf/20199213007 VL - 92 SP - 13007 EP - 13013 PB - EDP Sciences CY - Glasgow, Scotland AN - OPUS4-48909 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Babutzka, Martin T1 - Investigation of the salinization in marine and offshore environment - test methods and challenges N2 - Salinization and contamination of metal surfaces by chloride-containing aerosols is of great importance with regard to corrosion phenomena in the maritime sector and in offshore applications. Especially Offshore Wind Turbines are exposed to extreme corrosive conditions due to high chloride concentrations in the atmosphere and the resulting high chloride deposition rates. It is of great importance to evaluate to what extent salinization of the surface influences the corrosion protection of coatings and pitting occurrence on stainless steels under atmospheric conditions to evaluate the durability of metallic building structures in offshore and marine environments. The evaluation of the scientific literature and regulatory guidelines has shown that there are still many open questions regarding the contamination of metal surfaces by chlorides. This contribution will discuss how salinization of metal surfaces is evaluated and monitored according to current standards and guidelines. Future challenges concerning test methods and the application of evaluated salinization values and deposition rates will be discussed. T2 - 5th International Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures CY - Potsdam, Germany DA - 27.08.20019 KW - Maritime Atmosphäre KW - Versalzung KW - Maritime atmosphere KW - Salinization PY - 2019 SP - Th.2.A.5, 1 EP - 8 PB - SMAR 2019 AN - OPUS4-48905 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Haustein, T. A1 - Busweiler, Sabine A1 - Haustein, V. A1 - von Laar, C. A1 - Plarre, Rüdiger T1 - Laboratory breeding of Korynetes caeruleus (Coleoptera: Cleridae) for the biological of Anobium punctatum) (Coleoptera, Ptinidae) N2 - Larvae and adults of Korynetes caeruleus (de Geer 1775) (Coleoptera: Cleridae) were collected from old churches and reared in the laboratory on Anobium punctatum (de Geer 1774) (Coleoptera: Ptinidae). Breeding success of K. caeruleus was low, but basic parameters of this species’ developmental cycle were identifi ed. At 21°C and 75% relative humidity and a fourmonth cold period at 4°C, the development of K. caeruleus from egg to adult appearance lasted 2 years. The pupal stage may be reached and completed after one and a half years. Feeding on larvae of A. punctatum by larvae of K. caeruleus was observed and consisted of a combination of sucking haemolymph and consuming body parts. The sickle-like mandibles of larvae of K. caeruleus penetrate the cuticle of prey larvae; this is followed by pumping and sucking body movements. Adult beetles of A. punctatum were not attacked by K. caeruleus larvae. Feeding behaviour of adult K. caeruleus was not investigated. KW - Cultural heritage KW - Coleoptera KW - Korynetes caeruleus KW - Cleridae KW - Ptinidae KW - Anobium punctatum KW - Biological pest control KW - Life history data KW - Laboratory breeding KW - Wood protection PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-494999 DO - https://doi.org/10.14411/eje.2019.038 SN - 1802-8829 VL - 116 SP - 362 EP - 371 PB - České Budějovice AN - OPUS4-49499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kindrachuk, Vitaliy A1 - Fedelich, Bernard A1 - Rehmer, Birgit A1 - Peter, Frauke T1 - Computational methods for lifetime prediction of metallic components under high-temperature fatigue N2 - The issue of service life prediction of hot metallic components subjected to cyclic loadings is addressed. Two classes of lifetime models are considered, namely, the incremental lifetime rules and the parametric models governed by the fracture mechanics concept. Examples of application to an austenitic cast iron are presented. In addition, computational techniques to accelerate the time integration of the incremental models throughout the fatigue loading history are discussed. They efficiently solve problems where a stabilized response of a component is not observed, for example due to the plastic strain which is no longer completely reversed and accumulates throughout the fatigue history. The performance of such an accelerated Integration technique is demonstrated for a finite element simulation of a viscoplastic solid under repeating loading–unloading cycles. KW - Fatigue KW - Incremental lifetime models KW - Finite element analysis PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-481215 UR - https://www.mdpi.com/2075-4701/9/4/390 DO - https://doi.org/10.3390/met9040390 SN - 2075-4701 VL - 9 IS - 4 SP - 390, 1 EP - 24 PB - mdpi CY - Basel, Switzerland AN - OPUS4-48121 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Haferkamp, Sebastian A1 - Paul, Andrea A1 - Michalchuk, Adam A1 - Emmerling, Franziska T1 - Unexpected polymorphism during a catalyzed mechanochemical Knoevenagel condensation N2 - The transformation of a base-catalyzed, mechano-assisted Knoevenagel condensation of mono-fluorinated benzaldehyde derivatives (p-, m-, o-benzaldehyde) with malonodinitrile was investigated in situ and in real time. Upon milling, the para-substituted product was found to crystallize initially into two different polymorphic forms, depending on the quantity of catalyst used. For low catalyst concentrations, a mechanically metastable phase (monoclinic) was initially formed, converting to the mechanically stable phase (triclinic) upon further grinding. Instead, higher catalyst concentrations crystallize directly as the triclinic product. Inclusion of catalyst in the final product, as evidenced by mass spectrometric analysis, suggests this complex polymorphic pathway may be due to seeding effects. Multivariate analysis for the in situ Raman spectra supports this complex formation pathway, and offers a new approach to monitoring multi-phase reactions during ball milling. KW - Ball milling KW - C-C coupling KW - In situ KW - Mechanochemistry KW - Multivariate data analysis PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-481872 DO - https://doi.org/10.3762/bjoc.15.110 SN - 1860-5397 VL - 15 SP - 1141 EP - 1148 PB - Beilstein Insitut CY - Frankfurt am Main AN - OPUS4-48187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Belenguer, A. A1 - Michalchuk, Adam A1 - Lampronti, G A1 - Sanders, J T1 - Understanding the unexpected effect of frequency on the kinetics of a covalent reaction under ball-milling conditions N2 - We here explore how ball-mill-grinding frequency affects the kinetics of a disulfide exchange reaction. Our kinetic data show that the reaction progress is similar at all the frequencies studied (15–30 Hz), including a significant induction time before the nucleation and growth process starts. This indicates that to start the reaction an initial energy accumulation is necessary. Other than mixing, the energy supplied by the mechanical treatment has two effects: (i) reducing the crystal size and (ii) creating defects in the structure. The crystal-breaking process is likely to be dominant at first becoming less important later in the process when the energy supplied is stored at the molecular level as local crystal defects. This accumulation is taken here to be the rate-determining step. We suggest that the local defects accumulate preferentially at or near the crystal surface. Since the total area increases exponentially when the crystal size is reduced by the crystal-breaking process, this can further explain the exponential dependence of the onset time on the milling frequency. KW - Mechanochemistry KW - Kinetics KW - Diffraction PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483361 DO - https://doi.org/10.3762/bjoc.15.120 SN - 2195-951X VL - 15 SP - 1226 EP - 1235 PB - Beilstein-Institut zur Förderung der Chemischen Wissenschaften CY - Frankfurt, M. AN - OPUS4-48336 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Ghigo, Tea A1 - Rabin, Ira ED - Buzi, P. T1 - Detecting Early Medieval Coptic literature in Dayr Al-Anba Maqar, Between textual conservation and literary rearrangement: The case of Vat. Copt. 57 N2 - The study of the VAt.Copt. 57 at the Vatican Library. Codicological, palaeographical, textual and archaeometrical considerations. KW - Coptic KW - Archaeometry KW - Ink KW - Manuscripts PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-494004 SN - 978-88-210-1025-5 SP - 77 EP - 83 PB - Biblioteca Apostolica Vaticana AN - OPUS4-49400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wegner, Karl David A1 - Dussert, F. A1 - Truffier-Boutry, D. A1 - Benayad, A. A1 - Beal, D. A1 - Mattera, L. A1 - Ling, W. L. A1 - Carrière, M. A1 - Reiss, P. T1 - Influence of the Core/Shell Structure of Indium Phosphide Based Quantum Dots on Their Photostability and Cytotoxicity N2 - With the goal to improve their photostability, InP-based QDs are passivated with three types of inorganic shells, namely (i) a gradient ZnSexS1−x shell, (ii) an additional ZnS shell on top of the gradient shell with two different thicknesses (core/shell/shell, CSS), (iii) an alumina coating on top of ZnS. All three systems have photoluminescence Quantum yields (PLQY) > 50%and similar PL decay times (64–67 ns). To assess their photostability they are incorporated into a transparent poly (methyl methacrylate) (PMMA) matrix and exposed to continuous irradiation with simulated sunlight in a climate chamber. The alumina coated core/shell system exhibits the highest stability in terms of PLQY Retention as well as the lowest shift of the PL maximum and lowest increase of the PL linewidth, followed by the CSS QDs and finally the gradient shell system. By means of XPS studies we identify the degradation of the ZnS outer layer and concomitant xidation of the emissive InZnP core as the main origins of degradation in the gradient structure. These modifications do not occur in the case of the alumina-capped sample, which exhibits excellent chemical stability. The gradient shell and CSS systems could be transferred to the aqueous phase using surface ligand exchange with penicillamine. Cytotoxicity studies on human primary keratinocytes revealed that exposure for 24 h to 6.25–100 nM of QDs did not affect cell viability. However, a trend toward reduced cell proliferation is observed for higher concentrations of gradient shell and CSS QDs with a thin ZnS shell, while CSS QDs with a thicker ZnS shell do not exhibit any impact. KW - Indium phosphide KW - Quantum dots KW - Cytotoxicity KW - Photostability PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-494249 DO - https://doi.org/10.3389/fchem.2019.00466 VL - 7 SP - Article Number: 466 PB - Frontiers Media SA AN - OPUS4-49424 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Otto, Peter A1 - de Lorenzis, L. A1 - Unger, Jörg F. T1 - Explicit dynamics in impact simulation using a NURBS contact interface N2 - In this paper, the impact problem and the subsequent wave Propagation are considered. For the contact discretization an intermediate non-uniform rational B-spline (NURBS) layer is added between the contacting finite element bodies, which allows a smooth contact formulation and efficient element-based integration. The impact event is ill-posed and requires a regularization to avoid propagating stress oscillations. A nonlinear mesh-dependent penalty regularization is used, where the stiffness of the penalty regularization increases upon mesh refinement. Explicit time integration methods are well suited for wave propagation problems, but are efficient only for diagonal mass matrices. Using a spectral element discretization in combination with a NURBS contact layer the bulk part of the mass matrix is diagonal. KW - Explicit dynamics KW - Impact simulation KW - Isogeometric analysis KW - mortar method KW - spectral elements PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506041 DO - https://doi.org/10.1002/nme.6264 VL - 121 IS - 6 SP - 1248 EP - 1267 PB - Wiley Online Libary AN - OPUS4-50604 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zinke, R. A1 - Virothi, N. A1 - Köhler, F. A1 - Klippel, A. A1 - Schalau, Sebastian A1 - Krause, U. T1 - Experimental measurement of initial evaporation mass flows from gasoline spills and comparison with empirical models N2 - In this paper, we investigate the evaporation mass flow originating from spills of gas-oline. Large spills of gasoline may form during partial or complete roof sinkings or inthe case of perforations at various deck fittings at external floating roof tanks usedfor the storage. Additionally, spills may form in the retention area in the case of leak-ages at pipes or at the hull. The aim is to predict the order of magnitude of real-scaleevaporation mass flow. The determined evaporation mass flows will be used in arelated project as input values for subsequent dispersion modeling in the vicinity ofthe tanks. This is relevant for questions of fire and explosion protection as well as forenvironmental protection aspects in tank farms or refineries, which use externalfloating roof tanks. The measurements presented in this paper were compared withpredictions by empirical models and investigations of evaporations from small floorspills, round-bottom flask, or from Petri dishes published in the literature. The maingoal of this paper is to test the applicability of empirical models to provide reasonableevaporation mass flows as input for CFD dispersion simulations. KW - Spill evaporation PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504322 DO - https://doi.org/10.1002/prs.12128 VL - 39 IS - 3 SP - e12128 PB - Wiley Online Libary AN - OPUS4-50432 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schaumann, P. A1 - Schürmann, K. A1 - Pittner, Andreas A1 - Rethmeier, Michael T1 - Automatically Welded Tubular X Joints for Jacket Substructures – Prediction of the Technical Fatigue Crack Location N2 - To increase the competitiveness of jacket substructures compared to monopiles a changeover from an individual towards a serial jacket production based on automated manufactured tubular joints combined with standardized pipes has to be achieved. Therefore, this paper addresses fatigue tests of automatically welded tubular X-joints focusing on the location of the technical fatigue crack. The detected location of the technical crack is compared to numerical investigations predicting the most fatigue prone notch considering the structural stress approach as well as the notch stress approach. Besides, the welding process of the automated manufactured tubular X-joints is presented. T2 - Nordic Steel 2019 CY - Copenhagen, Denmark DA - 18.09.2019 KW - Automated arc welding KW - Fatigue tests KW - Tubular X-joints KW - Technical crack detection KW - Local fatigue approaches PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-518490 DO - https://doi.org/10.1002/cepa.1140 VL - 3 IS - 3-4 SP - 823 EP - 828 PB - Wiley-VCH Verlag GmbH on behalf of Ernst & Sohn Verlag für Architektur und technische Wissenschaften GmbH & Co. KG CY - Berlin AN - OPUS4-51849 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kapa, Thomas A1 - Schreier, Andy A1 - Krebber, Katerina T1 - A 100-km BOFDA Assisted by First-Order Bi-Directional Raman Amplification N2 - We present, to our knowledge for the first time, a 100-km Brillouin Optical Frequency-Domain Analysis (BOFDA) employing a 200-km fiber loop. Compared to our previous publication, enhanced sensor length, sensor accuracy and spatial resolution are presented. The performance improvements are achieved by applying distributed Raman amplification (DRA) and a digital high-pass filter. We report on temperature measurements over sensing distances of 75 km and 100 km both with a 12.5-m spatial resolution. Temperature changes of 5 °C have been measured along 75 km sensing fiber. A temperature change of 30 °C has been detected at 99.5 km. KW - Distributed sensing KW - Fiber optics sensors KW - Stimulated Brillouin scattering PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476577 DO - https://doi.org/10.3390/s19071527 SN - 1424-8220 VL - 19 IS - 7 SP - 1527, 1 EP - 9 PB - MDPI CY - Basel, Switzerland AN - OPUS4-47657 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiele, Marc A1 - Hille, Falk A1 - Makris, Ruben ED - Helmerich, Rosemarie ED - Ilki, A. ED - Motavalli, M. T1 - Comparison of fatigue crack detection methods for high-cyclic loaded steel structures N2 - At present, to produce renewable energy offshore wind farms play an important role. The available space combined with the more valuable wind conditions make offshore locations very attractive for wind powered energy production. In Europe a significant number of offshore wind farms already exist, especially in the North and Baltic Sea. In future this trend will continue, and further offshore wind farms will be built. The majority of offshore wind turbines are mounted on steel foundation structures. Due to the high-cyclic loading by wind and waves fatigue stress plays a substantial role regarding structural safety. Besides the consideration of fatigue within the design process, to monitor existing steel structures for potential fatigue cracks during their life time is a major topic and a challenge. For the structures of the offshore wind turbines are large and partially under water effective reliable methods for the detection of fatigue cracks are required. This contribution presents investigations on different crack detection methods applied at high-cycle fatigue tests on small-scale welded steel samples as well as on large-scale welded steel components. The tests were conducted at the BAM laboratories. For crack detection mainly three different methods were used and compared. The first method regards to the measurement of strain by conventionally strain gauges. Secondly, the crack luminescence was used as a new and effective optical method for surface monitoring. And finally, crack detection by pressure differentials of the inner and outer section of tubular steel elements was investigated. A comparison study will emphasize the advantages and disadvantages of the different methods and show which of the described methods is potentially more suitable for an application on real offshore wind structures. T2 - 5th International Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures CY - Potsdam, Germany DA - 27.08.2019 KW - Fatigue KW - Steel structures KW - Crack detection PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-489433 SP - Th.2.A.1-1 EP - Th.2.A.1-8 AN - OPUS4-48943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst A1 - Maak, Stefan A1 - Mielentz, Frank A1 - Effner, Ute A1 - Strangfeld, Christoph A1 - Timofeev, Juri T1 - Review of recent developments in ultrasonic echo testing of concrete N2 - Ultrasonic methods are used in concrete investigations since decades. While being limited to transmission testing in the laboratory for a while, in-situ echo measurements for structural investigations and condition assessment have made their way into practical application in the past 20 years. However, several challenges remain. On one side, there are technical issues as limitations in depth of penetration, resolution and imaging capabilities. On the other side there are still gaps in validation, standardization and certification, which are limiting the applicability in condition/load capacity assessment. This review reports a couple of developments which will help to overcome these issues. This includes technical developments as new devices which are easier to handle on site or giving a much deeper penetration depth (e.g. the LAUS device at BAM) as well as improvements in imaging by hardware update (e. g. air coupled ultrasound or coded signals) or new software (e. g. RTM imaging). To foster the application in real world projects we are as well working on standardization by developing new reference specimen with international partners which will ensure world-wide comparability of ultrasonic and other methods and quality assurance codes. Further, non-destructive methods are being used to update probabilistic models used for the reassessment of existing structures to support the structural engineer’s decisions. T2 - SMAR 2019 CY - Potsdam, Germany DA - 27.08.2019 KW - Engineered Barrier System (EBS) KW - Ultraschall KW - NDT KW - Re-assessment of exiting bridges PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-489686 SP - 1 EP - 6 AN - OPUS4-48968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Teng, Jun A1 - Tang, De-Hui A1 - Zhang, Xiao A1 - Hu, Wei-Hua A1 - Said, Samir A1 - Rohrmann, Rolf G. T1 - Automated modal analysis for tracking structural change during construction and operation phases N2 - The automated modal analysis (AMA) technique has attracted significant interest over the last few years, because it can track variations in modal parameters and has the potential to detect structural changes. In this paper, an improved density-based spatial clustering of applications with noise (DBSCAN) is introduced to clean the abnormal poles in a stabilization diagram. Moreover, the optimal system model order is also discussed to obtain more stable poles. A numerical Simulation and a full-scale experiment of an arch bridge are carried out to validate the effectiveness of the proposed algorithm. Subsequently, the continuous dynamic monitoring system of the bridge and the proposed algorithm are implemented to track the structural changes during the construction phase. Finally, the artificial neural network (ANN) is used to remove the temperature effect on modal frequencies so that a health index can be constructed under operational conditions. KW - Automated Modal Analysis for Tracking Structural Change during Construction and Operation Phases PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475116 UR - https://www.mdpi.com/1424-8220/19/4/927/pdf DO - https://doi.org/10.3390/s19040927 SN - 1424-8220 VL - 19 IS - 4 SP - 927, 1 EP - 23 PB - MDPI AG CY - Basel, Switzerland AN - OPUS4-47511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ren, J. A1 - Weigert, Florian A1 - Weber, F. A1 - Wang, Y. A1 - Choudhury, S. A1 - Xiao, J. A1 - Lauermann, I. A1 - Resch-Genger, Ute A1 - Bande, A. A1 - Petit, T. ED - Petit, Tristan T1 - Influence of surface chemistry on optical, chemical and electronic properties of blue luminescent carbon dots N2 - Carbon dots have attracted much attention due to their unique optical, chemical and electronic properties enabling a wide range of applications. The properties of carbon dots can be effectively adjusted through modifying their chemical composition. However, a major challenge remains in understanding the core and surface contributions to optical and electronic transitions. Here, three blue luminescent carbon dots with carboxyl, amino and hydroxyl groups were comprehensively characterized by UV-vis absorption and emission spectroscopy, synchrotron-based X-ray spectroscopy, and infrared spectroscopy. The influence of the surface functionality on their fluorescence was probed by pH-dependent photoluminescence measurements. Moreover, the hydrogen bonding interactions between water and the surface groups of carbon dots were characterized by infrared spectroscopy. Our results show that both core and surface electronic states of blue luminescent carbon dots contribute to electronic acceptor levels while the chemical nature of the surface groups determines the hydrogen bonding behavior of the carbon dots. This comprehensive spectroscopic study demonstrates that the surface chemistry has a profound influence on the electronic configuration and surface–water interaction of carbon dots, thus affecting their photoluminescence properties. KW - Quantum dots KW - Spectroscopy KW - UV Vis KW - Fluorescence KW - Surface chemistry PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-472325 DO - https://doi.org/10.1039/c8nr08595a SN - 2040-3372 VL - 11 IS - 4 SP - 2056 EP - 2064 PB - RSC AN - OPUS4-47232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krautz, M. A1 - Beyer, M. A1 - Jäschke, C. A1 - Schinke, L. A1 - Waske, Anja A1 - Seifert, J. T1 - A Magnetocaloric Booster Unit for Energy-Efficient Air-Conditioning N2 - A concept for the application of a magnetocaloric device in energy-efficient air conditioners is introduced. In order to evaluate this concept, a test stand has been developed equipped with a magnetic field source providing about a 1.5-T flux density change into which different Regenerator geometries can be implemented and evaluated. A processing route for the production of profiled magnetocaloric LaFeSiMn-based composite plates by tape casting is presented. The processed plates show a maximum isothermal entropy change of about 3.8 J kg−1 K−1 at a magnetic field change of 1.5 T at 285 K. The hydraulic and thermal performance of regenerator geometries that can be realized by profiled plates is assessed by calculations. KW - Magnetocaloric effect KW - Regenerator KW - Air-conditioning KW - Solid state cooling KW - Tape casting PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-480926 DO - https://doi.org/10.3390/cryst9020076 VL - 9 IS - 2 SP - 76 EP - 91 PB - MDPI AN - OPUS4-48092 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ghafafian, Carineh A1 - Popiela, Bartosz A1 - Nielow, Dustin A1 - Trappe, Volker T1 - Restoration of structural integrity – a comparison of various repair concepts for wind turbine rotor blade shells N2 - Localized patches are a cost- and time-effective method for repairing fiber-reinforced polymer (FRP) sandwich wind turbine rotor blade shells. To increase the understanding of their effect on the fatigue of the blades, this study examines the effect of various layup methods of localized repair patches on the structural integrity of composite sandwich structures. Manufactured with the vacuum-assisted resin infusion (VARI) process, the shell test specimens are produced as a curved structure with glass fiber reinforced polymer (GFRP) sandwiching a polyvinyl chloride (PVC) foam core. Patch repairs are then introduced with varying layup techniques, and material properties are examined with cyclic fatigue tests. The transition region between patch and parent material is studied in greater detail with finite element method (FEM) simulations, with a focus on the effect of fiber orientation mismatch. Damage onset, crack development, and eventual failure are monitored with in-situ non-destructive testing methods to develop a robust understanding of the effects of repair concepts on material stiffness and strength. T2 - SMAR 2019 - 5th International Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures CY - Potsdam, Germany DA - 27.08.2019 KW - Lightweight materials KW - Glass fiber reinforced polymers KW - Sandwich KW - Wind turbine blades PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-482170 SP - 1 EP - 8 PB - German Society for Non-Destructive Testing (DGZfP e.V.) AN - OPUS4-48217 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Priebe, Nsesheye Susan A1 - Gluth, Gregor A1 - Sturm, Patrick A1 - Vogler, Nico A1 - Kühne, Hans-Carsten T1 - Comparison of calcined illitic clays (brick clays) and low-grade kaolinitic clays as supplementary cementitious materials N2 - The use of calcined clays as supplementary cementitious materials (SCMs) has been identified as a viable option to decrease the CO2 emissions related to cement production. However, while extensive data is available about kaolinitic clays in this context, other clays such as illitic clays appear to be under-studied. Therefore, in the present study, two illitic clays were compared to two low-grade kaolinitic clays in terms of transformations in the calcination temperature range 650–900 °C, and performance of the calcined clays in blended cement pastes as measured by strength evolution, heat release, hydrated phase formation and portlandite consumption. The illitic clays required a higher calcination temperature for complete dehydroxylation of their illite than what is necessary for dehydroxylation of kaolinite. These higher calcination temperatures also led to particle sintering, significantly decreasing the specific surface area of the illitic clays, particularly for the clay with the higher Fe2O3 content. Nevertheless, while the kaolinitic clays generally exhibited the best performance as SCM, the illitic clay with lower Fe2O3 content performed similar to the kaolinitic clays when calcined at optimum temperature and applied at a moderate substitution rate. These findings demonstrate that several different clays have the potential to be used as SCM and indicate possible routes to identify suitable deposits for this purpose. KW - Blended cement KW - Calcined clay KW - Brick clay KW - Illite KW - Kaolinite PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-488195 DO - https://doi.org/10.1617/s11527-019-1393-2 SN - 1359-5997 SN - 1871-6873 N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. VL - 52 IS - 5 SP - Article Number 94 PB - Springer Nature AN - OPUS4-48819 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schwarz, W. A1 - Wilsch, Gerd A1 - Pichelhöfer, A. A1 - Ebell, Gino A1 - Völker, Tobias T1 - Galvanic chloride extraction by an embedded zinc anode: Ion distribution mapped by laser induced breakdown spectroscopy (LIBS) N2 - An important aspect with regard to the service life of zinc based galvanic anodes and the durability of the corrosion protection of steel in concrete is the “galvanic chloride extraction”. Chloride ions move in the electric field generated by the current, flowing between the galvanic anode and the cathodic steel. Migration leads to an accumulation of anions, e.g. chloride ions, at the anode and depletion of chlorides near the steel rebar surface. The ion migration was studied on steel reinforced concrete specimens admixed with 3 wt.% chloride/wt. cement and galvanically protected by a surface applied embedded zinc anode (EZA). The zinc anode was embedded and glued to the concrete surface by a geo-polymer based chloride free binder. The EZA was operated over a period of 1 year and the ion distribution between anode (EZA) and cathode (steel reinforcement) was studied by laser induced breakdown spectroscopy (LIBS) after 5 months, 7 months and 12 months. The results show that chloride ions efficiently migrate in the direction of the zinc-anode and accumulate there. Chloride distribution in the EZA correlates with the distribution of zinc ions generated by the anodic dissolution of the zinc anode in the binder matrix. The microstructure of the binder matrix and its interface to the zinc-anode are studied by REM/EDX – preliminary results will be reported. T2 - Concrete Solutions 2019 CY - Cluj Napoca, Romania DA - 30.09.2019 KW - Galvanic corrosion KW - Corrosion KW - Chloride extraction PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-488189 DO - https://doi.org/10.1051/matecconf/201928903010 VL - 289 SP - 03010, 1 EP - 5 PB - MATEC Web of Conferences AN - OPUS4-48818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Otto, Peter A1 - Lorenzis, L. A1 - Unger, Jörg F. T1 - Explicit dynamics in impact simulation using a NURBS contact interface N2 - In this paper, the impact problem and the subsequent wave propagation are considered. For the contact discretization an intermediate NURBS layer is added between the contacting finite element bodies, which allows a smooth contact formulation and efficient element‐based integration. The impact event is ill‐posed and requires a regularization to avoid propagating stress oscillations. A nonlinear mesh dependent penalty regularization is used, where the stiffness of the penalty regularization increases upon mesh refinement. Explicit time integration methods are well suited for wave propagation problems, but are efficient only for diagonal mass matrices. Using a spectral element discretization and the coupled FE‐NURBS approach the bulk part of the mass matrix is diagonal. KW - Impact simulation KW - Explicit dynamics KW - Isogeometric analysis KW - Spectral elements KW - Mortar method PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-494947 DO - https://doi.org/10.1002/nme.6264 SP - 1 EP - 21 PB - Wiley Online Libary AN - OPUS4-49494 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markwart, Jens C. A1 - Battig, Alexander A1 - Zimmermann, Lisa A1 - Wagner, Martin A1 - Fischer, Jochen A1 - Schartel, Bernhard A1 - Wurm, Frederik R. T1 - Systematically controlled decomposition mechanism in phosphorus flame retardants by precise molecular architecture: P−O vs P−N N2 - Flame retardants (FR) are inevitable additives to many plastics. Halogenated organics are effective FRs but are controversially discussed due to the release of toxic gases during a fire or their persistence if landfilled. Phosphorus-containing compounds are effective alternatives to halogenated FRs and have potential lower toxicity and degradability. In addition, nitrogencontaining additives were reported to induce synergistic effects with phosphorus-based FRs. However, no systematic study of the gradual variation on a single phosphorus FR containing both P−O and P−N moieties and their comparison to the respective blends of phosphates and phosphoramides was reported. This study developed general design principles for P−O- and P−N-based FRs and will help to design effective FRs for various polymers. We synthesized a library of phosphorus FRs that only differ in their P-binding pattern from each other and studied their decomposition mechanism in epoxy resins. Systematic control over the decomposition pathways of phosphate (PO(OR)3), phosphoramidate (PO(OR)2(NHR)), phosphorodiamidate (PO(OR)(NHR)2), phosphoramide (PO(NHR)3), and their blends was identified, for example, by reducing cis-elimination and the formation of P−N-rich char with increasing nitrogen content in the P-binding sphere. Our FR epoxy resins can compete with commercial FRs in most cases, but we proved that the blending of esters and amides outperformed the single molecule amidates/diamidates due to distinctively different decomposition mechanisms acting synergistically when blended. KW - Phosphorus KW - Flame retardants KW - Epoxies KW - Mechanistic study KW - Toxicity PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-481549 DO - https://doi.org/10.1021/acsapm.9b00129 SN - 2637-6105 VL - 1 IS - 5 SP - 1118 EP - 1128 PB - ACS AN - OPUS4-48154 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wosniok, Aleksander A1 - Skoczowsky, Danilo A1 - Schukar, Marcus A1 - Pötzsch, Sina A1 - Pötschke, Samuel A1 - Krüger, Simone T1 - Fiber optic sensors for high-temperature measurements on composite tanks in fire N2 - For the purpose of increasing payload and reduce freight cost, lightweight composite tank containers used for Transportation have been progressively developed during the last years. Compared to conventionally produced cylindrical steel tanks, the fiber-reinforced solutions allow greater flexibility in the tank design. Despite a number of further material-related benefits of fiber-reinforced composites as non-conductive and non-magnetic behavior as well as corrosion resistance and high strength, the optimization of their thermal degradation properties during combustion is still a challenge. To improve the fire performance of lightweight composite containers, special intumescent fire protection coatings can be applied onto the outside tank surface. This paper presents fire tests on glass-fiber-reinforced plastic transport tanks with complex geometries sheltered with different surface-applied fire protection systems. To evaluate the fire resistance of the tank structures, a fiber optic monitoring system was developed. This system is based on distributed temperature measurements using high-Resolution optical backscatter reflectometry and pointwise reference measurements using fiber Bragg gratings. Thereby, all the fiber optic sensors were directly integrated in the composite layer structure of the tanks. The focus of the presented work is on the demonstration of capability of fiber optic monitoring system in such high-temperature application. Moreover, the fiber optic measurements provide new insights into the efficiency of intumescent coating applied for fire protection of fiber-reinforced plastic transport tanks. KW - Fire resistance KW - Composite material KW - Glass-fiber-reinforced plastic transport tank KW - Distributed fiber optic sensing KW - Optical backscatter reflectometry KW - Fiber optic sensor PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-481972 DO - https://doi.org/10.1007/s13349-019-00338-7 SN - 2190-5452 SN - 2190-5479 SP - 1 EP - 8 PB - Springer Nature AN - OPUS4-48197 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zirnstein, Benjamin A1 - Schulze, Dietmar A1 - Schartel, Bernhard T1 - Mechanical and fire properties of multicomponent flame retardant EPDM rubbers using aluminum trihydroxide, ammonium polyphosphate, and polyaniline N2 - In this study, multicomponent flame retardant systems, consisting of Ammonium polyphosphate (APP), aluminum trihydroxide (ATH), and polyaniline (PANI), were used in ethylene propylene diene monomer (EPDM) rubber. The multicomponent system was designed to improve flame retardancy and the mechanical properties of the rubber compounds, while simultaneously reducing the amount of filler. PANI was applied at low loadings (7 phr) and combined with the phosphorous APP (21 phr) and the mineral flame retardant ATH (50 phr). A comprehensive study of six EPDM rubbers was carried out by systematically varying the fillers to explain the impact of multicomponent flame retardant systems on mechanical properties. The six EPDM materials were investigated via the UL 94, limiting oxygen index (LOI), FMVSS 302, glow wire tests, and the cone calorimeter, showing that multicomponent flame retardant systems led to improved fire performance. In cone calorimeter tests the EPDM/APP/ATH/PANI composite reduced the maximum average rate of heat emission (MARHE) to 142 kW·m-2, a value 50% lower than that for the unfilled EPDM rubber. Furthermore, the amount of phosphorus in the residues was quantified and the mode of action of the phosphorous flame retardant APP was explained. The data from the cone calorimeter were used to determine the protective layer effect of the multicomponent flame retardant systems in the EPDM compounds. KW - EPDM KW - Rubber KW - Flame retardant KW - Polyaniline KW - Aluminum trihydroxide (ATH) PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-482769 DO - https://doi.org/10.3390/ma12121932 SN - 1996-1944 VL - 12 IS - 12 SP - 1932, 1 EP - 22 PB - MDPI AN - OPUS4-48276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hussels, Maria-Teresa A1 - Chruscicki, Sebastian A1 - Arndt, Detlef A1 - Scheider, Swen A1 - Prager, Jens A1 - Homann, Tobias A1 - Habib, Abdel Karim T1 - Localization of transient events threatening pipeline integrity by fiber-optic distributed acoustic sensing N2 - Pipe integrity is a central concern regarding technical safety, availability, and environmental compliance of industrial plants and pipelines. A condition monitoring system that detects and localizes threats in pipes prior to occurrence of actual structural failure, e.g., leakages, especially needs to target transient events such as impacts on the pipe wall or pressure waves travelling through the medium. In the present work, it is shown that fiber-optic distributed acoustic sensing (DAS) in conjunction with a suitable application geometry of the optical fiber sensor allows to track propagating acoustic waves in the pipeline wall on a fast time-scale. Therefore, short impacts on the pipe may be localized with high fidelity. Moreover, different acoustic modes are identified, and their respective group velocities are in good agreement with theoretical predications. In another set of experiments modeling realistic damage scenarios, we demonstrate that pressure waves following explosions of different gas mixtures in pipes can be observed. Velocities are verified by local piezoelectric pressure transducers. Due to the fully distributed nature of the fiber-optic sensing system, it is possible to record accelerated motions in detail. Therefore, in addition to detection and localization of threatening events for infrastructure monitoring, DAS may provide a powerful tool to study the development of gas explosions in pipes, e.g., investigation of deflagration-to-detonation-transitions (DDT). KW - Distributed acoustic sensing (DAS) KW - Distributed vibrations sensing (DVS) KW - Fiber-optic sensing KW - Condition monitoring KW - Pipeline integrity KW - Gas explosion PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-488555 DO - https://doi.org/10.3390/s19153322 SN - 1424-8220 VL - 19 IS - 15 SP - 3322, 1 EP - 20 PB - MDPI CY - Basel, CH AN - OPUS4-48855 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Provis, J. L. A1 - Arbi, K. A1 - Bernal, S. A. A1 - Bondar, D. A1 - Buchwald, A. A1 - Castel, A. A1 - Chithiraputhiran, S. A1 - Cyr, M. A1 - Dehghan, A. A1 - Dombrowski-Daube, K. A1 - Dubey, A. A1 - Ducman, V. A1 - Gluth, Gregor A1 - Nanukuttan, S. A1 - Peterson, K. A1 - Puertas, F. A1 - van Riessen, A. A1 - Torres-Carrasco, M. A1 - Ye, G. A1 - Zuo, Y. T1 - RILEM TC 247-DTA round robin test: mix design and reproducibility of compressive strength of alkali-activated concretes N2 - The aim of RILEM TC 247-DTA ‘Durability Testing of Alkali-Activated Materials’ is to identify and validate methodologies for testing the durability of alkali-activated concretes. To underpin the durability testing work of this committee, five alkali-activated concrete mixes were developed based on blast furnace slag, fly ash, and flash-calcined metakaolin. The concretes were designed with different intended performance levels, aiming to assess the capability of test methods to discriminate between concretes on this basis. A total of fifteen laboratories worldwide participated in this round robin test programme, where all concretes were produced with the same mix designs, from single-source aluminosilicate precursors and locally available aggregates. This paper reports the mix designs tested, and the compressive strength results obtained, including critical insight into reasons for the observed variability in strength within and between laboratories. KW - Alkali-activated materials KW - Alkali-activated slag KW - Compressive strength KW - Concrete KW - Mix-design PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-489131 DO - https://doi.org/10.1617/s11527-019-1396-z SN - 1359-5997 SN - 1871-6873 VL - 52 IS - 5 SP - Article Number 99 PB - Springer Nature AN - OPUS4-48913 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoevelmann, J. A1 - Stawski, T. M. A1 - Besselink, R. A1 - Freeman, H. M. A1 - Dietmann, K. M. A1 - Mayanna, S. A1 - Pauw, Brian Richard A1 - Benning, L. G. T1 - A template-free and low temperature method for the synthesis of mesoporous magnesium phosphate with uniform pore structure and high surface area N2 - Mesoporous phosphates are a group of nanostructured materials with promising applications, particularly in biomedicine and catalysis. However, their controlled synthesis via conventional template-based routes presents a number of challenges and limitations. Here, we show how to synthesize a mesoporous Magnesium phosphate with a high surface area and a well-defined pore structure through thermal decomposition of a crystalline struvite (MgNH4PO4·6H2O) precursor. In a first step, struvite crystals with various morphologies and sizes, ranging from a few micrometers to several millimeters, had been synthesized from supersaturated aqueous solutions (saturation index (SI) between 0.5 and 4) at ambient pressure and temperature conditions. Afterwards, the crystals were thermally treated at 70–250 °C leading to the release of structurally bound water (H2O) and ammonia (NH3). By combining thermogravimetric analyses (TGA), scanning and transmission electron microscopy (SEM, TEM), N2 sorption analyses and small- and wide-angle X-ray scattering (SAXS/WAXS) we show that this decomposition process results in a pseudomorphic transformation of the original struvite into an amorphous Mg-phosphate. Of particular importance is the fact that the final material is characterized by a very uniform mesoporous structure with 2–5 nm wide pore channels, a large specific surface area of up to 300 m2 g−1 and a total pore volume of up to 0.28 cm3 g−1. Our struvite decomposition method is well controllable and reproducible and can be easily extended to the synthesis of other mesoporous phosphates. In addition, the so produced mesoporous material is a prime candidate for use in biomedical applications considering that Magnesium phosphate is a widely used, non-toxic substance that has already shown excellent biocompatibility and biodegradability. KW - Struvite KW - SAXS KW - Scattering KW - Nanoporous KW - Geology PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-477130 DO - https://doi.org/10.1039/c8nr09205b VL - 11 IS - 14 SP - 6939 EP - 6951 PB - Royal Society of Chemistry AN - OPUS4-47713 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Descalzo, Ana B. A1 - Ashokkumar, Pichandi A1 - Shen, Z. A1 - Rurack, Knut T1 - On the Aggregation Behaviour and Spectroscopic Properties of Alkylated and Annelated BoronDipyrromethene (BODIPY) Dyes in Aqueous Solution N2 - The tendency of boron-dipyrromethene (BODIPY) dyes to associate in water is well known, and usually a cause for inferior fluorescence properties. Synthetic efforts to chemically improve BODIPYs’ water solubility and minimize this problem have been numerous in the past. However, a deeper understanding of the phenomena responsible for fluorescence quenching is still required. Commonly, the spectroscopic behaviour in aqueous media has been attributed to aggregate or excimer formation, with such works often centring on a single BODIPY family. Herein, we provide an integrating discussion including very diverse types of BODIPY dyes. Our studies revealed that even subtle structural changes can distinctly affect the association behaviour of the fluorophores in water, involving different photophysical processes. The palette of behaviour found ranges from unperturbed emission, to the formation of H or J aggregates and excimers, to the involvement of tightly bound, preformed excimers. These results are a first step to a more generalized understanding of spectroscopic properties vs. structure, facilitating future molecular design of BODIPYs, especially as probes for biological applications. KW - Aggregates KW - BODIPY KW - Excimers KW - Fluorescence KW - Photophysics PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-497771 DO - https://doi.org/10.1002/cptc.201900235 SN - 2367-0932 VL - 4 IS - 2 SP - 120 EP - 131 PB - WILEY-VCH CY - Weinheim AN - OPUS4-49777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liu, H. A1 - Song, W. A1 - Gröninger, Delia A1 - Zhang, L. A1 - Lu, Y. A1 - Chan, K. S. A1 - Zhou, Z. A1 - Rurack, Knut A1 - Shen, Z. T1 - Real-time monitoring of newly acidified organelles during autophagy enabled by reaction-based BODIPY dyes N2 - Real-time monitoring of newly acidified organelles during autophagy in living cells is highly desirable for a better understanding of intracellular degradative processes. Herein, we describe a reaction-based boron dipyrromethene (BODIPY) dye containing strongly electron-withdrawing diethyl 2-cyanoacrylate groups at the α-positions. The probe exhibits intense red fluorescence in acidic organelles or the acidified cytosol while negligible fluorescence in other regions of the cell. The underlying mechanism is a nucleophilic reaction at the central meso-carbon of the indacene core, resulting in the loss of π-conjugation entailed by dramatic spectroscopic changes of more than 200 nm between its colorless, non-fluorescent leuco-BODIPY form and its red and brightly emitting form. The reversible transformation between red fluorescent BODIPY and leuco-BODIPY along with negligible cytotoxicity qualifies such dyes for rapid and direct intracellular lysosome imaging and cytosolic acidosis detection simultaneously without any washing step, enabling the real-time monitoring of newly acidified organelles during autophagy. KW - Autophagy KW - BODIPY KW - Fluorescence KW - Lysosome KW - Real-time imaging PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498358 UR - https://www.nature.com/articles/s42003-019-0682-1 DO - https://doi.org/10.1038/s42003-019-0682-1 SN - 23993642 VL - 2 SP - 442 PB - Nature Research CY - London AN - OPUS4-49835 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Büchele, Dominique A1 - Chao, Madlen A1 - Ostermann, Markus A1 - Leenen, M. A1 - Bald, Ilko T1 - Multivariate chemometrics as a key tool for prediction of K and Fe in a diverse German agricultural soil-set using EDXRF N2 - Within the framework of precision agriculture, the determination of various soil properties is moving into focus, especially the demand for sensors suitable for in-situ measurements. Energy-dispersive X-ray fluorescence (EDXRF) can be a powerful tool for this purpose. In this study a huge diverse soil set (n = 598) from 12 different study sites in Germany was analysed with EDXRF. First, a principal component analysis (PCA) was performed to identify possible similarities among the sample set. Clustering was observed within the four texture classes clay, loam, silt and sand, as clay samples contain high and sandy soils low iron mass fractions. Furthermore, the potential of uni- and multivariate data evaluation with partial least squares regression (PLSR) was assessed for accurate Determination of nutrients in German agricultural samples using two calibration sample sets. Potassium and iron were chosen for testing the performance of both models. Prediction of these nutrients in 598 German soil samples with EDXRF was more accurate using PLSR which is confirmed by a better overall averaged deviation and PLSR should therefore be preferred. KW - XRF KW - Chemometrics KW - Soil KW - Agriculture KW - Multivariate PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498671 DO - https://doi.org/10.1038/s41598-019-53426-5 VL - 9 SP - 17588 PB - Nature AN - OPUS4-49867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yildirim, Arda A1 - Sentker, K. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Huber, P. A1 - Schönhals, Andreas T1 - Collective orientational order and phase behavior of a discotic liquid crystal under nanoscale confinement N2 - The phase behavior and molecular ordering of hexakishexyloxy triphenylene (HAT6) DLC under cylindrical nanoconfinement is studied utilizing differential scanning calorimetry (DSC) and dielectric spectroscopy (DS), where cylindrical nanoconfinement is established through embedding HAT6 into the nanopores of anodic aluminum oxide membranes (AAO), and a silica membrane with pore diameters ranging from 161 nm down to 12 nm. Both unmodified and modified pore walls were considered, and in the latter case the pore walls of AAO membranes were chemical treated with n octadecylphosphonic acid (ODPA) resulting in the formation of a 2.2 nm thick layer of grafted alkyl chains. Phase transition enthalpies decrease with decreasing pore size, indicating that a large proportion of the HAT6 molecules within the pores has a disordered structure, which increases with decreasing pore size for both pore walls. In the case of the ODPA modification the amount of ordered HAT6 is increased compared to the unmodified case. The pore size dependencies of the phase transition temperatures were approximated using the Gibbs Thomson equation, where the estimated surface tension is dependent on the molecular ordering of HAT6 molecules within the pores and upon their surface. DS was employed to investigate the molecular ordering of HAT6 within the nanopores. These investigations revealed that with a pore size of around 38 nm, for the samples with the unmodified pore walls, the molecular ordering changes from planar axial to homeotropic radial. However, the planar axial configuration, which is suitable for electronic applications, can be successfully preserved through ODPA modification for most of the pore sizes. KW - Discotic Liquid Crystals KW - Nanoconfinement PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475222 DO - https://doi.org/10.1039/c8na00308d SN - 2516-0230 VL - 1 IS - 3 SP - 1104 EP - 1116 PB - RSC AN - OPUS4-47522 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gramse, G. A1 - Schönhals, Andreas A1 - Kienberger, F. T1 - Nanoscale dipole dynamics of protein membranes studied by broadband dielectric microscopy N2 - We investigate the nearfield dipole mobility of protein membranes in a wide frequency range from 3 kHz to 10 GHz. The results of our nanoscale dielectric images and spectra of bacteriorhodopsin (bR) reveal Debye relaxations with time constants of τ ∼ 2 ns and τ ∼ 100 ns being characteristic of the Dipole moments of the bR retinal and α-helices, respectively. However, the dipole mobility and therefore the protein biophysical function depend critically on the amount of surface water surrounding the protein, and the characteristic mobility in the secondary structure is only observed for humidity levels <30%. Our results have been achieved by adding the frequency as a second fundamental dimension to quantitative dielectric microscopy. The key elements for the success of this advanced technique are the employed heterodyne detection scheme, the broadband electrical signal source, a high frequency optimized cabling, development of calibration procedures and precise finite element modelling. Our study demonstrates the exciting possibilities of broadband dielectric microscopy for the investigation of dynamic processes in cell bioelectricity at the individual molecular level. Furthermore, the technique may shed light on local dynamic processes in related materials science applications like semiconductor Research or nano-electronics. KW - Broadband dielectric microscopy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475230 DO - https://doi.org/10.1039/c8nr05880f SN - 2040-3372 VL - 11 IS - 10 SP - 4303 EP - 4309 PB - RSC AN - OPUS4-47523 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Röhsler, Andreas A1 - Sobol, Oded A1 - Unger, Wolfgang A1 - Böllinghaus, Thomas T1 - Comprehensive study of deuterium-induced effects in in austenitic stainless steel AISI 304L N2 - The damaging impact of hydrogen on the austenitic stainless steel AISI 304 L was analysed. To this aim, samples were charged electrochemically with the hydrogen isotope deuterium (2H, D) and examined with time-of-flight secondary ion mass spectrometry (ToF-SIMS) and electron backscatter diffraction (EBSD). The fusion of the obtained chemical and structural information revealed local enrichment of deuterium in austenite, transformation into martensite, crack formation and severe roughening of the specimen surface. The results indicated that martensite was not only formed during charging but also during Desorption and ToF-SIMS examinations. Furthermore, cross-sections of deuterium-charged samples revealed that in preferred deformation bands a g/ε/a 0 evolution is taking place. By means of microscopic analyses and carrier gas hot extraction (CGHE), it was found that the use of NaAsO2 as recombination poison decreased the uptake of hydrogen significantly and resulted in severe precipitation on the specimen surfaces. This is in contrast to the popular presumption that NaAsO2 enhances the uptake of hydrogen (and deuterium) during electrochemical charging by hampering its recombination from Atoms to molecules. KW - AISI 304L KW - Hydrogen KW - ToF-SIMS KW - Deuterium KW - Martensite PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-477540 DO - https://doi.org/10.1016/j.ijhydene.2019.03.058 SN - 0360-3199 SN - 1879-3487 VL - 44 IS - 23 SP - 12228 EP - 12238 PB - Elsevier Ltd. AN - OPUS4-47754 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schwibbert, Karin A1 - Menzel, F. A1 - Epperlein, N. A1 - Bonse, Jörn A1 - Krüger, Jörg T1 - Bacterial adhesion on femtosecond laser-modified polyethylene N2 - In this study, femtosecond laser-induced sub-micrometer structures are generated to modify polyethylene (PE) surface topographies. These surfaces were subjected to bacterial colonization studies with Escherichia coli and Staphylococcus aureus as test strains. The results reveal that the nanostructures do not influence S. aureus coverage, while the adhesion of E. coli is reduced. KW - Bacterial adhesion KW - Laser-modified surface KW - Polyethylene KW - Laser-induced nanostructures KW - Biofilm PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-492280 DO - https://doi.org/10.3390/ma12193107 VL - 12 IS - 19 SP - 3107 PB - MDPI CY - Basel, Schweiz AN - OPUS4-49228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gharaati, S. A1 - Wang, Cui A1 - Förster, C. A1 - Weigert, Florian A1 - Resch-Genger, Ute A1 - Heinze, K. T1 - Triplet–Triplet Annihilation Upconversion in a MOF with AcceptorFilled Channels N2 - In summary, we report a highly modular solid TTA-UC system comprising of a crystalline, thermally stable PCN222(Pd) MOF with CA-coated MOF channels and with a DPA annihilator embedded in a solution-like environment in the MOF channels. This solid material displays blue upconverted delayed emission with a luminescence lifetime of 373 us, a threshold value of 329 mW*cm-2 and a triplet–triplet energy transfer efficiency of 82%. This optical application adds another facet to the versatile chemistry of PCN-222 MOFs. The design concept is also applicable to other TTA-UC pairs and enables tuning of the UCL color, for example, by replacing DPA with other dyes as exemplarily shown for 2,5,8,11-tetra-tert-butyl-perylene, that yields UCL at 450 nm. Current work aims to reduce the oxygen sensitivity and to increase the retention of the trapped annihilators in organic environments, for example, by tuning the chain length of the carboxylic acid and by coating the MOF surface. In addition, the TTA-UC efficiency will be further enhanced by reducing the reabsorption of the UC emission caused by Pd(TCPP) and by optimizing the sensitizer/annihilator interface. KW - Porphyrin KW - Method KW - MOF KW - Fluorescence KW - Dye KW - Sensor KW - Oxygen sensitive KW - Single molecule KW - DPA KW - Lifetime KW - Upconverstion KW - Quantum yield KW - Triplet-triplet annihilation KW - Sensitization KW - Energy transfer KW - NMR PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-500580 DO - https://doi.org/10.1002/chem.201904945 VL - 26 IS - 5 SP - 1003 EP - 1007 PB - Wiley-VCH Verlag CY - Weinheim AN - OPUS4-50058 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kembuan, C. A1 - Saleh, Maysoon I. A1 - Rühle, Bastian A1 - Resch-Genger, Ute A1 - Graf, C. T1 - Coating of upconversion nanoparticles with silica nanoshells of 5–250 nm thickness N2 - A concept for the growth of silica shells with a thickness of 5–250 nm onto oleate-coated NaYF4:Yb3+/Er3+ upconversion nanoparticles (UCNP) is presented. The concept enables the precise adjustment of shell thicknesses for the preparation of thick-shelled nanoparticles for applications in plasmonics and sensing. First, an initial 5–11 nm thick shell is grown onto the UCNPs in a reverse microemulsion. This is followed by a stepwise growth of these particles without a purification step, where in each step equal volumes of tetraethyl orthosilicate and ammonia water are added, while the volumes of cyclohexane and the surfactant Igepal® CO-520 are increased so that the ammonia water and surfactant concentrations remain constant. Hence, the number of micelles stays constant, and their size is increased to accommodate the growing core–shell particles. Consequently, the formation of core-free silica particles is suppressed. When the negative zeta potential of the particles, which continuously decreased during the stepwise growth, falls below −40 mV, the particles can be dispersed in an ammoniacal ethanol solution and grown further by the continuous addition of tetraethyl orthosilicate to a diameter larger than 500 nm. Due to the high colloidal stability, a coalescence of the particles can be suppressed, and single-core particles are obtained. This strategy can be easily transferred to other nanomaterials for the design of plasmonic nanoconstructs and sensor systems. KW - Reverse microemulsion KW - Silica coating KW - Stepwise growth KW - Thick shells KW - Upconversion nanoparticles PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-502769 DO - https://doi.org/10.3762/bjnano.10.231 SN - 2190-4286 VL - 10 SP - 2410 EP - 2421 PB - Beilstein-Institut zur Förderung der Chemischen Wissenschaften CY - Frankfurt, M. AN - OPUS4-50276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, A. A1 - Gröber, A. A1 - Simkin, Roman A1 - Kranzmann, Axel T1 - Influence of Surface Quality on the Corrosion and Corrosion Fatigue Behavior of High Alloyed Steels Exposed to Different Saline Aquifer Water Environment N2 - Coupons of X5CrNiCuNb16-4 with different surface roughness that may be utilized as injection pipe with 16% Chromium and 0.05% Carbon (1.4542, AISI 630) were exposed for 3000 h to CO2-saturated saline aquifer water simulating the conditions in the Northern German Basin at ambient pressure and 60 °C. Additionally, corrosion fatigue experiments (ambient pressure, technically clean CO2, saline aquifer water of Stuttgart Aquifer) were performed using specimen of X46Cr13 (1.4043, AISI 420C) with regard to the influence of the roughness of technical surfaces on the number of cycles to failure at different stress amplitudes. Specimen of Duplex stainless steel X2CrNiMoN22-3-2 (1.4462) for corrosion fatigue experiments were provided with technical surfaces after machining as well as polished surfaces. Results were obtained at load amplitudes ranging from 175 MPa to 325 MPa in the geothermal brine of the Northern German Basin at 98 °C. The main precipitation phases on the surface as well as within pits reveal carbonates or hydroxides such as siderite (FeCO3) and ferrous hydroxide goethite (FeOOH) independent of the original surface roughness. Corrosion rates for polished and technical surfaces were below 0.005 mm/year compared to corrosion rates of 0.035 mm/year after shot peening. Specimen with technical surfaces tested at high stress amplitudes (>275 MPa) lasted longer (cycles to failure: P50% at Sa 300 MPa=5x105) than specimen with polished surfaces (cycles to failure: P50% at Sa 300 MPa=1.5x105). This behavior is emphasized by the slope coefficient (technical surfaces k = 19.006, polished surfaces k=8.78) meaning earlier failure for polished at high stress amplitude Sa. Although rather low scatter ranges (technical surface: TN=1:1.35, polished surface: TN=1.1.95) indicate no change in failure mechanism it may be assumed that at low stress pitting is the initiating crack growth process whereas at high stress amplitudes the formation of micro cracks is reason for crack propagation and failure. KW - High Alloyed Steel KW - Pitting KW - Surface KW - Roughness KW - Corrosion Fatigue PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503772 DO - https://doi.org/10.20319/mijst.2019.51.115137 SN - 2454-5880 VL - 5 IS - 1 SP - 115 EP - 137 PB - Global Research and Development Services Publishing CY - Rajasthan, India AN - OPUS4-50377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, A. A1 - Kranzmann, Axel T1 - Corrosion and Fatigue of Heat Treated Martensitic Stainless Steel 1.4542 used for Geothermal Applications N2 - During capture and storage technology (CCS) as well as in geothermal energy production Steels need to withstand the corrosive environment such as: heat, pressure, salinity of the aquifer and CO2-partial pressure. 1.4542 shows unusual corrosion phenomena, but is still sufficiently resistant in corrosive environments. To better understand its behaviour differently heat treated coupons of 1.4542 and for comparison X20Cr13 and X46Cr13 were kept in the artificial brine of the Northern German Basin at T=60 °C. Ambient pressure as well as p=100 bar for 700 h - 8000 h in water saturated supercritical CO2 and CO2-saturated synthetic aquifer Environment was applied. Fatigue tests were performed via push-pull tests with a series of 30 specimens from 150 MPa to 500 MPa (sinusoidal dynamic test loads, R=-1; resonant frequency ~ 30 Hz). FeCO3 and FeOOH are corrosion products also after dynamic corrosion tests. Martensitic microstructure offers good corrosion resistance in geothermal environment. The S-N-curve showing no typical fatigue strength and very steep slopes of possible fatigue strength for finite life. Possible influencing artefacts, such as Al-inclusions could not be correlated to early rupture despite specimens containing inclusions at the fracture surface and cross section reached lower number of cycles. Applied potential proofed to enhance fatigue life tremendously. KW - High Alloyed Steel KW - Pitting KW - Corrosion Fatigue KW - Corrosion KW - Endurance Limit PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503765 DO - https://doi.org/10.20319/mijst.2019.51.138158 SN - 2454-5880 VL - 5 IS - 1 SP - 138 EP - 158 PB - Global Research and Development Services Publishing CY - Rajasthan, India AN - OPUS4-50376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Javaheri, E. A1 - Lubritz, J. A1 - Graf, B. A1 - Rethmeier, Michael T1 - Mechanical Properties Characterization of Welded Automotive Steels N2 - Among the various welding technologies, resistance spot welding (RSW) and laser beam welding (LBW) play a significant role as joining methods for the automobile industry. The application of RSW and LBW for the automotive body alters the microstructure in the welded areas. It is necessary to identify the mechanical properties of the welded material to be able to make a reliable statement about the material behavior and the strength of welded components. This study develops a method by which to determine the mechanical properties for the weldment of RSW and LBW for two dual phase (DP) steels, DP600 and DP1000, which are commonly used for the automotive bodies. The mechanical properties of the resistance spot weldment were obtained by performing tensile tests on the notched tensile specimen to cause an elongation of the notched and welded area in order to investigate its properties. In order to determine the mechanical properties of the laser beam weldment, indentation tests were performed on the welded material to calculate its force-penetration depth-curve. Inverse numerical simulation was used to simulate the indentation tests to determine and verify the parameters of a nonlinear isotropic material model for the weldment of LBW. Furthermore, using this method, the parameters for the material model of RSW were verified. The material parameters and microstructure of the weldment of RSW and LBW are compared and discussed. The results show that the novel method introduced in this work is a valid approach to determine the mechanical properties of welded high-strength steel structures. In addition, it can be seen that LBW and RSW lead to a reduction in ductility and an increase in the amount of yield and tensile strength of both DP600 and DP1000. KW - Mechanical property KW - Laser beam welding KW - Dual phase steel KW - Resistance spot welding PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-502269 DO - https://doi.org/10.3390/met10010001 VL - 10 IS - 1 SP - 1 EP - 20 PB - MDPI AN - OPUS4-50226 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beygi Nasrabadi, Hossein A1 - Bauer, Felix A1 - Uhlemann, Patrick A1 - Thärig, Steffen A1 - Rehmer, Birgit A1 - Skrotzki, Birgit T1 - Mechanical testing dataset of cast copper alloys for the purpose of digitalization N2 - This data article presents a set of primary, analyzed, and digitalized mechanical testing datasets for nine copper alloys. The mechanical testing methods including the Brinell and Vickers hardness, tensile, stress relaxation, and low-cycle fatigue (LCF) testing were performed according to the DIN/ISO standards. The obtained primary testing data (84 files) mainly contain the raw measured data along with the testing metadata of the processes, materials, and testing machines. Five secondary datasets were also provided for each testing method by collecting the main meta- and measurement data from the primary data and the outputs of data analyses. These datasets give materials scientists beneficial data for comparative material selection analyses by clarifying the wide range of mechanical properties of copper alloys, including Brinell and Vickers hardness, yield and tensile strengths, elongation, reduction of area, relaxed and residual stresses, and LCF fatigue life. Furthermore, both the primary and secondary datasets were digitalized by the approach introduced in the research article entitled “Toward a digital materials mechanical testing lab” [1]. The resulting open-linked data are the machine-processable semantic descriptions of data and their generation processes and can be easily queried by semantic searches to enable advanced data-driven materials research. KW - FAIR principles KW - Hardness KW - Low-Cycle Fatigue (LCF) KW - Tensile testing KW - Stress relaxation PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-605005 DO - https://doi.org/10.1016/j.dib.2024.110687 SN - 2352-3409 SP - 1 EP - 15 PB - Elsevier BV AN - OPUS4-60500 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Han, Ying A1 - Kruse, Julius A1 - Rosalie, Julian A1 - Radners, J. A1 - von Hartrott, P. A1 - Skrotzki, Birgit T1 - Influence of mean stress and overaging on fatigue life of aluminum alloy EN AW-2618A N2 - Fatigue tests were performed on the forged aluminum alloy EN AW-2618A in the T61 state. Different stress ratios (R = -1, R = 0.1) were selected to study the influence of mean stress on fatigue life. Two overaged states (10 h/230 ◦C, 1000 h/230 ◦C) were also tested to investigate the influence of overaging on fatigue life. Transmission electron microscopy (TEM) was used to characterize the precipitates (S-phase), which are mainly responsible for the strength of the alloy. A fractographic analysis was also performed to determine the failure mode. Overaging reduces the fatigue life compared to the T61 state. The longer the aging time, the lower the fatigue resistance. The reason is the decrease in (yield) strength, which correlates with the radius of the S-phase: the precipitate radius increases by a factor of approximately two for the overaged states compared to the initial state. The analysis of the fracture surfaces showed crack initiation occurs predominantly on the outer surface and is associated with the primary phases. KW - Aluminum alloys KW - Aging KW - Fatigue KW - Microstructure KW - Electron microscopy KW - S-Phase PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583708 DO - https://doi.org/10.1016/j.msea.2023.145660 SN - 0921-5093 VL - 886 SP - 1 EP - 10 PB - Elsevier B.V. AN - OPUS4-58370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rehmer, Birgit A1 - Bayram, Faruk A1 - Ávila Calderón, Luis A1 - Mohr, Gunther A1 - Skrotzki, Birgit T1 - Elastic modulus data for additively and conventionally manufactured variants of Ti-6Al-4V, IN718 and AISI 316 L N2 - This article reports temperature-dependent elastic properties (Young’s modulus, shear modulus) of three alloys measured by the dynamic resonance method. The alloys Ti-6Al-4V, Inconel IN718, and AISI 316 L were each investigated in a variant produced by an additive manufacturing processing route and by a conventional manufacturing processing route. The datasets include information on processing routes and parameters, heat treatments, grain size, specimen dimensions, and weight, as well as Young’s and shear modulus along with their measurement uncertainty. The process routes and methods are described in detail. The datasets were generated in an accredited testing lab, audited as BAM reference data, and are hosted in the open data repository Zenodo. Possible data usages include the verification of the correctness of the test setup via Young’s modulus comparison in low-cycle fatigue (LCF) or thermo-mechanical fatigue (TMF) testing campaigns, the design auf VHCF specimens and the use as input data for simulation purposes. KW - Elastic modulus KW - Young's modulus KW - Shear modulus KW - Additive manufacturing KW - AISI 316L KW - IN 718 KW - Ti-6Al-4V KW - Reference data KW - Temperature dependence PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579716 DO - https://doi.org/10.1038/s41597-023-02387-6 VL - 10 IS - 1 SP - 1 EP - 9 PB - Springer Nature AN - OPUS4-57971 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chemello, Giovanni A1 - Knigge, Xenia A1 - Ciornii, Dmitri A1 - Reed, B.P. A1 - Pollard, A.J. A1 - Clifford, C.A. A1 - Howe, T. A1 - Vyas, N. A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - Influence of the Morphology on the Functionalization of Graphene Nanoplatelets Analyzed by Comparative Photoelectron Spectroscopy with Soft and Hard X-Rays N2 - Since its isolation, graphene has received growing attention from academia and industry due to its unique properties. However, the “what is my material” barrier hinders further commercialization. X-ray photoelectron spectroscopy (XPS) is considered as a method of choice for the determination of the elemental and chemical composition. In this work the influence of the morphology of graphene particles on the XPS results is studied and investigated as a function of X-ray energy, using conventional XPS with Al K𝜶 radiation and hard X-ray photoemission spectroscopy (HAXPES) using Cr K𝜶 radiation. Thereby, the information depth is varied between 10 and 30 nm. For this purpose, two commercial powders containing graphene nanoplatelets with lateral dimensions of either ≈100 nm or in the micrometer range are compared. These larger ones exist as stack of graphene layers which is inspected with scanning electron microscopy. Both kinds of particles are then functionalized with either oxygen or fluorine. The size of the graphene particles is found to influence the degree of functionalization. Only the combination of XPS and HAXPES allows to detect the functionalization at the outermost surface of the particles or even of the stacks and to provide new insights into the functionalization process. KW - Functionalized graphene KW - Hard-energy X-ray photoelectron spectroscopy KW - X-ray photoelectron spectroscopy PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-578860 DO - https://doi.org/10.1002/admi.202300116 SN - 2196-7350 SP - 1 EP - 8 PB - Wiley VCH AN - OPUS4-57886 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Terborg, R. A1 - Kim, K. J. A1 - Hodoroaba, Vasile-Dan T1 - Elemental composition and thickness determination of thin films by electron probe microanalysis N2 - Electron probe microanalysis (EPMA) applies to solid samples of homogenous (bulk) chemical composition and can usually not be applied to structures which are inhomogeneous in the micrometer range such as thin film systems down to a few nm. However, in combination with the established thin film software Stratagem, the thickness as well as the elemental composition of thin films on a substrate can be determined. This has been recently successfully demonstrated for Fe-Ni on Si and Si-Ge on Al2O3 thin film systems. For both systems five samples of different elemental composition and a reference were produced and characterised by inductively coupled plasma mass spectrometry (ICP-MS), Rutherford backscattering (RBS), and transmission electron microscopy (TEM) as reference values. Last year, a new and open-source thin film evaluation programme called BadgerFilm has been released. It can also be used to determine thin film composition and thickness from intensity ratios of the unknown sample and standards (k-ratios). In this contribution, we reevaluated the data acquired for the Fe-Ni and Si-Ge systems using the BadgerFilm software package and compared the obtained elemental compositions and thickness values with the results of the Stratagem software and the reference methods. The conclusion is that the BadgerFilm software shows good agreement with the elemental composition and thickness calculated by Stratagem (mostly <2% for both composition and thickness) and with the reference values for two representative thin film systems (<1%–2% for composition and <10%–20% for thickness). KW - Elemental composition KW - EPMA KW - Film thickness KW - Thin films PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576368 DO - https://doi.org/10.1002/sia.7183 SN - 0142-2421 VL - 55 SP - 496 EP - 500 PB - Wiley AN - OPUS4-57636 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sonntag, Nadja A1 - Jürgens, Maria A1 - Uhlemann, Patrick A1 - Skrotzki, Birgit A1 - Olbricht, Jürgen T1 - Experimental data from service-like creep-fatigue experiments on grade P92 steel N2 - This article refers to the research article entitled “Creep-Fatigue of P92 in Service-Like Tests with Combined Stress- and Strain-Controlled Dwell Times” [1]. It presents experimental mechanical data from complex service-like creep-fatigue experiments performed isothermally at 620 °C and a low strain amplitude of 0.2 % on tempered martensite-ferritic grade P92 steel. The data sets in text file format provide cyclic deformation (min. and max. stresses) and the total (hysteresis) data of all recorded fatigue cycles for three different creep-fatigue experiments: 1) a standard relaxation fatigue (RF) test with symmetrical dwell times of three minutes introduced at minimum and maximum strain, 2) a fully strain-controlled service-like relaxation (SLR) test combining these three-minute peak strain dwells with a 30-minute dwell in between at zero strain, and 3) a partly stress-controlled service-like creep (SLC) test combining the three-minute peak strain dwells with 30-minute dwells at constant stress. Such service-like (SL) tests with additional long-term stress- and strain-controlled dwell times are non-standard, rare, and expensive, making these data very valuable. They may be used to approximate cyclic softening in the technically relevant range, for the design of complex SL experiments, or for detailed analyses of stress-strain hystereses (e.g., for stress or strain partitioning methods, for the determination of hysteresis energies (work), inelastic strain components, etc.). In addition, the latter analyses may supply important input for advanced parametric lifetime modeling of components under creep-fatigue loading or model calibration parameters. KW - Tempered martensite-ferritic steel KW - Creep KW - Stress relaxation KW - Creep-fatigue KW - Dwell times PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-578407 DO - https://doi.org/10.1016/j.dib.2023.109333 SN - 2352-3409 VL - 49 SP - 1 EP - 9 PB - Elsevier Inc. AN - OPUS4-57840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Bartczack, Dorota A1 - Taché, Olivier A1 - Hodoroaba, Vasile-Dan T1 - Report on the homogeneity assessment of bimodal gold materials (nPSize1 and nPSize2) and particle number concentration by frequency method N2 - The main objective was to assess homogeneity of two bimodal gold materials, namely nPsize1 and nPSize2, containing approximately 1:1 and 10:1 particle number-based ratio of ~30nm and ~60nm particles. Particle number-based concentration within the two size fractions was determined with spICP-MS using the particle frequency method of calibration. KW - Nanoparticles KW - Homogeneity KW - Particle number concentration KW - Gold KW - nPSize PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595451 DO - https://doi.org/10.5281/zenodo.10654245 SP - 1 EP - 5 PB - Zenodo CY - Geneva AN - OPUS4-59545 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jentzsch, Stefan A1 - Stock, Daniel A1 - Häcker, Ralf A1 - Skrotzki, Birgit A1 - Darvishi Kamachali, Reza A1 - Klingbeil, Dietmar A1 - Kindrachuk, Vitaliy T1 - Shear Band Formation with Split Hopkinson Bar Experiments N2 - The essence of dynamic failure is closely linked to dramatic shear deformations which often lead to the formation of adiabatic shear bands (ASB). Under high loading velocities and the subsequent rapid temperature increase, the localization of shear strain is crucial in view of safety issues of systems in mechanical and aircraft engineering, especially with respect to fast rotating components and diverse crash scenarios. In this research, we perform high speed impact tests at the split Hopkinson pressure bar (SHPB) setup and use particular hat-shaped specimen geometries that resemble the stresses and failure conditions at the component level. In the first step, we specify a notched specimen geometry using finite element (FE) simulations to ensure pure shear. Further, quasi-static compressive tests and a series of impact tests at high strain rates of 10^3-10^4 s^-1 are conducted on specimens manufactured from a fine-grain structural steel with the properties of S355. Optical microscopy and electron backscatter diffraction (EBSD) of the sheared zones unveil significant localization to maximal shear strains of about 0.9 accompanied by grain refinement by factors 5 to 14. The displacements across the surface of the specimens are captured with subset-based local digital image correlation (DIC) during the impact time, and serve as an objective to validate a viscoplastic constitutive relationship. More precisely, the deformation distribution is accurately reproduced by the widely recognized Johnson-Cook (JC) model, which features an enhanced description of damage evolution. Thus, combining experimental and characterization techniques, continuum mechanics and reasonable optimization strategies for the identification of model parameters provides an efficient approach for comprehensive insights into the strain localization behaviour and its impact on the mechanical performance of S355 under extreme strain rates and deformations. KW - Adiabatic shear bands KW - Finite element analysis KW - Viscoplastic material modelling KW - Split Hopkinson pressure bar KW - Hat-shaped specimen KW - Johnson–Cook parameter identification PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613339 DO - https://doi.org/10.1016/j.ijmecsci.2024.109749 VL - 284 SP - 1 EP - 14 PB - Elsevier BV AN - OPUS4-61333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eisenbart, Miriam A1 - Hanke, Thomas A1 - Bauer, Felix A1 - Beygi Nasrabadi, Hossein A1 - Junghanns, Kurt A1 - Dziwis, Gordian A1 - Tikana, Ladji A1 - Parvez, Ashak Mahmud A1 - van den Boogaart, Karl Gerald A1 - Sajjad, Mohsin A1 - Friedmann, Valerie A1 - Preußner, Johannes A1 - Ramakrishnan, Anantha Narayanan A1 - Klengel, Sandy A1 - Meyer, Lars‐Peter A1 - Martin, Michael A1 - Klotz, Ulrich Ernst A1 - Skrotzki, Birgit A1 - Weber, Matthias T1 - KupferDigital: Ontology‐Based Digital Representation for the Copper Life Cycle N2 - The copper life cycle comprises numerous stages from the alloy production to the manufacturing and usage of engineered parts until recycling. At each step, valuable data are generated and stored; some are transferred to the subsequent stations. A thorough understanding of the materials’ behavior during manufacturing processes or throughout their product lifetime is highly dependent on a reliable data transfer. If, for example, a failure occurs during the service life, information about the manufacturing route can be of decisive importance for detecting the root cause of the failure. Additionally, the life cycle assessment hinges on the availability of data. Recording and storing interoperable structured data is, therefore, a thriving research field with huge implications for the economic strength of the manufacturing industry. In the KupferDigital project, it is demonstrated how an ontology‐based data space can be utilized not only as an innovative method for storing and providing interoperable life cycle data but also as a means to enable automated data analysis and evaluation, leading to new insights and the creation of new knowledge using semantic data and technologies. This work illustrates how data recorded at different research facilities can be integrated into one single data space, allowing queries across heterogeneous sources. KW - Copper Alloy KW - Ontology KW - Digitalization KW - Data Space KW - Semantic Representation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630213 SN - 1527-2648 DO - https://doi.org/10.1002/adem.202401735 VL - 27 IS - 8 SP - 1 EP - 29 PB - Wiley AN - OPUS4-63021 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ciornii, Dmitri A1 - Hodoroaba, Vasile-Dan A1 - Wachtendorf, Volker A1 - Fengler, Petra A1 - Altmann, Korinna T1 - Interlaboratory Comparison Reveals State of the Art in Microplastic Detection and Quantification Methods N2 - In this study, we investigate the current accuracy of widely used microplastic (MP) detection methods through an interlaboratory comparison (ILC) involving ISO-approved techniques. The ILC was organized under the prestandardization platform of VAMAS (Versailles Project on Advanced Materials and Standards) and gathered a large number (84) of analytical laboratories across the globe. The aim of this ILC was (i) to test and to compare two thermo-analytical and three spectroscopical methods with respect to their suitability to identify and quantify microplastics in a water-soluble matrix and (ii) to test the suitability of the microplastic test materials to be used in ILCs. Two reference materials (RMs), polyethylene terephthalate (PET) and polyethylene (PE) as powders with rough size ranges between 10 and 200 μm, were used to press tablets for the ILC. The following parameters had to be assessed: polymer identity, mass fraction, particle number concentration, and particle size distribution. The reproducibility, SR, in thermo-analytical experiments ranged from 62%−117% (for PE) and 45.9%−62% (for PET). In spectroscopical experiments, the SR varied between 121% and 129% (for PE) and 64% and 70% (for PET). Tablet dissolution turned out to be a very challenging step and should be optimized. Based on the knowledge gained, development of guidance for improved tablet filtration is in progress. Further, in this study, we discuss the main sources of uncertainties that need to be considered and minimized for preparation of standardized protocols for future measurements with higher accuracy. KW - Microplastics KW - Interlaboratory comparison KW - PlasticsFatE KW - PET KW - PE KW - Reference materials KW - VAMAS KW - Thermo-analytical methods KW - Spectroscopical methods PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630462 DO - https://doi.org/10.1021/acs.analchem.4c05403 SN - 1520-6882 VL - 97 SP - 8719 EP - 8728 PB - ACS Publications AN - OPUS4-63046 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Reliable physico–chemical characterisation of graphene-related and other 2D materials: present and future N2 - In the path of commercialisation of graphene-related and other 2D materials the consolidation has begun. In this phase, it is important to build trust between the individual partners in the product value chain. This requires trustworthy statements based on reliable and reproducible material characterisation. The first steps have been taken to measure graphene and other related 2D materials (GR2Ms) under well-defined conditions. Measurands and protocols for key methods were made available for this purpose. But there are still some challenges to overcome such as (i) reference materials, (ii) reference data, (iii) reproducibility throughout the workflow, (iv) credible structure-activity relationships, bringing the standards to (v) the factory floor and to (vi) real-word products. In addition, 2D materials beyond graphene should also be considered exploiting the knowledge gained from the characterisation of GR2M. KW - 2D Materials KW - Commercialisation KW - Standardisation KW - Trust PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638122 DO - https://doi.org/10.1088/2053-1583/aded9d SN - 2053-1583 VL - 12 IS - 4 SP - 1 EP - 8 PB - IOP Publishing AN - OPUS4-63812 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wolf, M. E. A1 - Vickery, W. M. A1 - Swift-Ramirez, W. A1 - Arnold, A. M. A1 - Orlando, J. D. A1 - Schmidt, S. J. A1 - Liu, Y. A1 - Er, Jasmin A1 - Schusterbauer, Robert A1 - Ahmed, R. A1 - Nickl, Philip A1 - Radnik, Jörg A1 - Donskyi, Ievgen A1 - Sydlik, S. A. T1 - The Mitsunobu reaction for the gentle covalent attachment of biomolecules to graphene oxide N2 - Graphene oxide (GO) has emerged as a promising biomaterial as it is easily and cheaply synthesized, strong, cytocompatible, osteoinductive, and has a well-characterized aqueous degradation pathway. It is also a great substrate for functionalization with biomolecules such as proteins, peptides, and small molecules that can enhance or add bioactivity. Covalent chemical linkages as opposed to typical noncovalent association methods are preferable so that the biomolecules do not quickly diffuse away or face replacement by other proteins, which is critical in long time scale applications like bone regeneration. However, covalent chemistry tends to carry a drawback of harsh reaction conditions that can damage the structure, conformation, and therefore function of a delicate biomolecule like a protein. Here, the Mitsunobu reaction is introduced as a novel method of covalently attaching proteins to graphene oxide. It features gentle reaction conditions and has the added benefit of utilizing the plentiful basal plane alcohol functionalities on graphene oxide, allowing for high yield protein functionalization. The amino acid Glycine (G), the protein bovine serum albumin (BSA), and the small molecule SVAK-12 are utilized to create the three Mitsunobu Graphene (MG) materials G-MG, BSA-MG, and SVAK-MG that demonstrate the wide applicability of this functionalization method. KW - Graphene oxide KW - Mitsunobu reaction KW - Covalent attachment KW - Bovine serum albumin KW - Macrophage polarization KW - Osteogenesis PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630483 DO - https://doi.org/10.1016/j.carbon.2025.120221 VL - 238 SP - 1 EP - 15 PB - Elsevier Ltd. AN - OPUS4-63048 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fadda, Marta A1 - Sacco, Alessio A1 - Altmann, Korinna A1 - Ciornii, Dmitri A1 - Milczewski, Frank A1 - Bañares, Miguel A. A1 - Portela, Raquel A1 - Giovannozzi, Andrea Mario A1 - Rossi, Andrea Mario T1 - Tracking nanoplastics in drinking water: a new frontier with the combination of dielectrophoresis and Raman spectroscopy N2 - Detection of micro- (MPs) and nanoplastics (NPs) in food and environmental matrices has been gaining relevance due to their potential toxicological effects on human health. While MPs have been detected in a wide range of complex matrices, suitable methods for the characterization and chemical identification of NPs are still lacking, primarily due to significant methodological challenges associated with their nano-specific physiochemical properties, including size distribution (1 nm – 1 µm), dynamic surface chemical changes, and carbon-based composition, which complicate their detection compared to engineered nanomaterials. To overcome the traditional limitations of spectroscopic techniques in terms of spatial resolution and sensitivity at the sub-micrometer level, a novel label-free methodology is presented for specifically identifying the chemical composition of NPs directly in suspension by combining Raman spectroscopy with dielectrophoresis (DEP). Using a custom-built device, small volumes of NPs are injected into a dielectrophoretic cell and locally trapped by DEP forces to fill the Raman confocal volume, facilitating their detection and identification, and providing high signal-to-noise ratio Raman spectra for more reliable analysis. This approach was successfully applied to both Milli-Q water and a commercial brand of drinking water, enabling the rapid identification of various types of NPs with different sizes and polymer compositions at concentrations as low as 20 µg/mL. These included certified reference polystyrene beads ranging from 800 to 60 nm in diameter, as well as polydisperse NPs, more representative of real samples in terms of size distribution and polymer type, such as polyethylene (450 nm), polypropylene (180 nm), and polyethylene terephthalate (100 nm). Moreover, the chemical fingerprint of each NPs was thoroughly investigated and compared with the corresponding bulk polymers, highlighting possible changes in the Raman bands due to surface oxidation or nanometer-scale effect. Therefore, this innovative method can be considered a valuable approach for addressing gaps in the detection and identification of NPs, as well as for monitoring their dynamic phisiochemical changes in real matrices. KW - Nanoplastics KW - Water contaminants KW - Raman microspectroscopy KW - Dielectrophoresis PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-633658 DO - https://doi.org/10.1186/s43591-025-00131-y SN - 2662-4966 VL - 5 IS - 1 SP - 1 EP - 11 PB - Springer Science and Business Media LLC AN - OPUS4-63365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chemello, Giovanni A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - XPS–SEM/EDS Tandem Analysis for the Elemental Composition of Functionalized Graphene Nanoplatelets N2 - Over the past decade, energy-dispersive X-ray spectrometry (EDS) with scanning electron microscopy (SEM) has advanced to enable the accurate analysis of light elements such as C, N, or O. For this reason, EDS is becoming increasingly interesting as an analytical method for the elemental analysis of functionalized graphene and could be an attractive alternative to Xray photoelectron spectroscopy (XPS), which is considered the most important method for elemental analysis. In this study, comparative XPS and EDS investigations under different excitation conditions are carried out on commercially available powders containing graphene particles with different morphologies. The slightly different XPS/HAXPES and EDS results can be explained by the different information depths of the methods and the functionalization of the particle surfaces. For the material with smaller graphene particles and higher O/C ratios, all methods reported a lower O/C ratio in pellets compared with the unpressed powder samples. This clearly shows that sample preparation has a significant influence on the quantification results, especially for such a type of morphology. Overall, the study demonstrates that EDS is a reliable and fast alternative to XPS for the elemental quantification of functionalized graphene particles, provided that differences in the information depth are taken into account. Particle morphology can be examined in parallel with quantitative element analysis, since EDS spectrometers are typically coupled with SEM, which are available in a huge number of analytical laboratories. KW - Graphene oxide KW - SEM/EDS KW - XPS/HAXPES KW - Elemental composition KW - Functionalization PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647294 DO - https://doi.org/10.1021/acsomega.5c07830 SN - 2470-1343 SP - 1 EP - 7 PB - American Chemical Society (ACS) AN - OPUS4-64729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radnik, Jörg A1 - Dang, T. T. H. A1 - Gatla, S. A1 - Raghuwanshi, V. S. A1 - Tatchev, D. A1 - Hoell, A. T1 - Identifying the location of Cu ions in nanostructured SAPO-5 molecular sieves and its impact on the redox properties N2 - Combining X-ray Absorption Fine Spectroscopy (XAFS) with Anomalous Small-Angle X-ray Scattering (ASAXS) determines the location of Cu2+ ions in silicoaluminophosphate (SAPO-5) frameworks prepared by hydrothermal crystallization or impregnation. As expected, for the hydrothermally prepared sample, incorporation in the SAPO-5 framework was observed. For the first time preferential location of Cu2+ ions at the inner and outer surfaces of the framework is determined. Temperature-Programmed Reduction (TPR) and X-ray Photoelectron Spectroscopy (XPS) investigations demonstrated that such Cu2+ is stable in an argon (Ar) atmosphere up to 550 °C and can only be reduced under a hydrogen atmosphere. In contrast, Cu2+ deposited by impregnation on the pure SAPO-5 framework can be easily reduced to Cu+ in an Ar atmosphere. At lower Cu amounts, mononuclear tetrahedrally coordinated Cu species were formed which are relatively stable in the monovalent form. In contrast, at higher Cu amounts, CuO particles were found which change easily between the mono- and bivalent species. KW - Nanostructured material KW - Molecular sieves KW - X-ray absorption Fine Spectroscopy KW - Anomalous Small Angle X-ray Scattering KW - X-ray Photoelectron Spectroscopy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474793 DO - https://doi.org/10.1039/c8ra10417d SN - 2046-2069 VL - 9 IS - 12 SP - 6429 EP - 6437 PB - RSC AN - OPUS4-47479 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lisec, Jan A1 - Jaeger, Carsten A1 - Rashid, R. A1 - Munir, R. A1 - Zaidi, N. T1 - Cancer cell lipid class homeostasis is altered under nutrient-deprivation but stable under hypoxia N2 - Background: Cancer cells modify the balance between fatty acid (FA) synthesis and uptake under metabolic stress, induced by oxygen/nutrient deprivation. These modifications were shown to alter the levels of individual triglyceride (TG) or phospholipid sub-species. To attain a holistic overview of the lipidomic profiles of cancer cells under stress we performed a broad lipidomic assay, comprising 244 lipids from six major classes. This assay allowed us to perform robust analyses and assess the changes in averages of broader lipid-classes, stratified on the basis of saturation index of their fatty-acyl side chains. Methods: Global lipidomic profiling using Liquid Chromatography-Mass Spectrometry was performed to assess lipidomic profiles of biologically diverse cancer cell lines cultivated under metabolically stressed conditions. Results: Neutral lipid compositions were markedly modified under serum-deprived conditions and, strikingly, the cellular level of triglyceride subspecies decreased with increasing number of double bonds in their fatty acyl chains. In contrast and unexpectedly, no robust changes were observed in lipidomic profiles of hypoxic (2% O2) Cancer cells despite concurrent changes in proliferation rates and metabolic gene expression. Conclusions: Serum-deprivation significantly affects lipidomic profiles of cancer cells. Although, the levels of individual lipid moieties alter under hypoxia (2% O2), the robust averages of broader lipid classes remain unchanged. KW - Tumor metabolism KW - Fatty acid metabolism KW - Lipidomic profile KW - Metabolic stress PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-481061 DO - https://doi.org/10.1186/s12885-019-5733-y SN - 1471-2407 VL - 19 SP - 501, 1 EP - 11 PB - Springer Nature AN - OPUS4-48106 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reimann, C. A1 - Kaufmann, Jan Ole A1 - Adams, L. C. A1 - Onthank, D. C. A1 - Thöne-Reineke, C. A1 - Robinson, S. P. A1 - Hamm, B. A1 - Botnar, R. M. A1 - Makowski, M. R. T1 - Dual-probe molecular MRI for the in vivo characterization of atherosclerosis in a mouse model: Simultaneous assessment of plaque inflammation and extracellular-matrix remodeling N2 - Molecular MRI is a promising in-vivo modality to detect and quantify morphological and molecular vessel-wall changes in atherosclerosis. The combination of different molecular biomarkers may improve the risk stratification of patients. This study aimed to investigate the feasibility of simultaneous visualization and quantification of plaque-burden and inflammatory activity by dual-probe molecular MRI in a mouse-model of progressive atherosclerosis and in response-to-therapy. Homozygous apolipoprotein E knockout mice (ApoE−/−) were fed a high-fat-diet (HFD) for up to four-months prior to MRI of the brachiocephalic-artery. To assess response-to-therapy, a statin was administered for the same duration. MR imaging was performed before and after administration of an elastin-specific gadolinium-based and a macrophage-specific iron-oxide-based probe. Following in-vivo MRI, samples were analyzed using histology, immunohistochemistry, inductively-coupled-mass-spectrometry and laser-inductively-coupled-mass-spectrometry. In atherosclerotic-plaques, intraplaque expression of elastic-fibers and inflammatory activity were not directly linked. While the elastin-specific probe demonstrated the highest accumulation in advanced atherosclerotic-plaques after four-months of HFD, the iron-oxide-based probe showed highest accumulation in early atherosclerotic-plaques after two-months of HFD. In-vivo measurements for the elastin and iron-oxide-probe were in good agreement with ex-vivo histopathology (Elastica-van-Giesson stain: y = 298.2 + 5.8, R2 = 0.83, p < 0.05; Perls‘ Prussian-blue-stain: y = 834.1 + 0.67, R2 = 0.88, p < 0.05). Contrast-to-noise-ratio (CNR) measurements of the elastin probe were in good agreement with ICP-MS (y = 0.11x-11.3, R² = 0.73, p < 0.05). Late stage atherosclerotic-plaques displayed the strongest increase in both CNR and gadolinium concentration (p < 0.05). The gadolinium probe did not affect the visualization of the iron-oxide-probe and vice versa. This study demonstrates the feasibility of simultaneous assessment of plaque-burden and inflammatory activity by dual-probe molecular MRI of progressive atherosclerosis. The in-vivo detection and quantification of different MR biomarkers in a single scan could be useful to improve characterization of atherosclerotic-lesions. KW - In-vivo KW - Molecular MRI PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-492514 DO - https://doi.org/10.1038/s41598-019-50100-8 VL - 9 IS - 1 SP - Article number: 13827 PB - Nature AN - OPUS4-49251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reed, B.P. A1 - Radnik, Jörg A1 - Shard, A.G. T1 - Ionic liquid [PMIM]+[NTf2]− (Solarpur®) characterized by XPS N2 - X-ray photoelectron spectroscopy (XPS) was performed on the meniscus of a droplet of ionic liquid 1-propyl-3-methyl-imidazolium bis(trifluoromethylsulfonyl) imide [PMIM]+[NTf2]− (Solarpur®) in ultrahigh vacuum. High-resolution spectra of F 1s, O 1s, N 1s, C 1s, and S 2p are presented along with a survey spectrum and the valence band structure. The spectra presented here were generated using monochromatic Al Kα radiation (1486.6 eV). KW - Ionic liquid KW - 1-propyl-3-methyl-imidazolium bis(trifluoromethylsulfonyl)imide KW - X-ray Photoelectron Spectroscopy PY - 2022 DO - https://doi.org/10.1116/6.0001518 VL - 29 IS - 1 SP - 014001-1 PB - AVS AN - OPUS4-54335 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duewer, D. L. A1 - Murray, J. A. A1 - Wood, L. J. A1 - Wise, S. A. A1 - Hein, Sebastian A1 - Koch, Matthias A1 - Philipp, Rosemarie A1 - Werneburg, Martina A1 - Hackenberg, R. A1 - Polzer, J. A1 - Avila, M. A. A1 - Serrano, V. A1 - Kakoulides, E. A1 - Alexopoulos, C. A1 - Giannikopoulou, P. A1 - Gui, E. M. A1 - Lu, T. A1 - Teo, T. L. A1 - Hua, T. A1 - Dazhou, C. A1 - Chunxin, L. A1 - Changjun, Y. A1 - Hongmei, L. A1 - Nammoonnoy, J. A1 - Sander, L. C. A1 - Lippa, K. A1 - Quinn, L. A1 - Swiegelaar, C. A1 - Fernandes-Whaley, M. A1 - Gören, A. C. A1 - Gökcen, T. T1 - CCQM-K95.1 Low-polarity analytes in a botanical matrix: Polycyclic aromatic hydrocarbons (PAHs) in tea N2 - Extraction, chromatographic separation, and quantification of low-concentration organic compounds in complex matrices are core challenges for reference material producers and providers of calibration services. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2014 the Organic Analysis Working Group (OAWG) initiated CCQM-K95.1 "Low-Polarity Analytes in a Botanical Matrix: Polycyclic Aromatic Hydrocarbons (PAHs) in Tea". This was a follow-on comparison from CCQM-K95 which was completed in 2014. The polycyclic aromatic hydrocarbons (PAHs) benz[a]anthracene (BaA) and benzo[a]pyrene (BaP) are considered priority pollutants by U.S. Environmental Protection Agency and are regulated contaminants in food, pose chromatographic separation challenges, and for which exist well-characterized measurement procedures and standard materials. BaA and BaP in a smoked tea were therefore selected as representative target measurands for CCQM-K95.1. Ten NMIs participated in CCQM-K95.1. The consensus summary mass fractions for the two PAHs are in the range of (50 to 70) ng/g with relative standard deviations of (6 to 10) %. Successful participation in CCQM K95.1 demonstrates the following measurement capabilities in determining mass fraction of organic compounds, with molar mass of 100 g/mol to 500 g/mol and having polarity pKow −2, in a botanical matrix ranging in mass fraction from 10 ng/g to 1000 ng/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, (3) extraction of analytes of interest from the matrix, (4) cleanup and separation of analytes of interest from interfering matrix or extract components, and (5) separation and quantification using gas chromatography or liquid chromatography. KW - Benz[a]anthracene (BaA) KW - Benzo[a]pyrene (BaP) KW - Gas chromatography (GC) KW - Isotope dilution (ID) KW - Liquid chromatography (LC) KW - Mass spectrometry (MS) KW - Polycyclic aromatic hydrocarbon (PAH) KW - Yerba mate tea PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471430 DO - https://doi.org/10.1088/0026-1394/56/1A/08002 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1 A SP - 08002, 1 EP - 89 PB - IOP Science AN - OPUS4-47143 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nitz, Phillip D. H. A1 - Rosaz, Paul A1 - Kreysina, Daniela A1 - Kasprzak, Dawid A1 - Qi, Naiyu A1 - Baller, Johannes A1 - Graeber, Gustav T1 - Water-in-Salt Electrolytes Embedded in Polyacrylamide Hydrogels: A First Step toward Deformable Sodium-Ion Batteries N2 - The development of flexible, safe, and sustainable Energy storage systems is critical for next-generation technologies, including wearable electronics, biomedical devices, and soft robotics. In this work, we provide a systematic investigation of sodium perchlorate-based water-in-salt (WIS) electrolytes embedded in polyacrylamide (PAM) hydrogels as a potential platform for deformable sodium-ion batteries or aqueous supercapacitors. Using Raman spectroscopy, we track the transition from free to intermediate water states with increasing salt concentration, identifying the onset of the WIS regime around 10 mol kg−1. Electrochemical measurements reveal that both the aqueous and hydrogel-based electrolytes exhibit a broadened electrochemical stability window (ESW) at higher salt concentrations, reaching up to 2.75 V. Impedance spectroscopy shows that while aqueous electrolytes achieve higher peak conductivity (156 mS cm−1), hydrogel-based electrolytes offer greater stability across a range of concentrations. This observation was supported by cyclic voltammetry, as it showed enhanced electrochemical stability of the PAM hydrogel compared to the aqueous electrolyte. This comprehensive and systematic study demonstrates that highly concentrated WIS electrolytes can be successfullyembedded into PAM hydrogels, while preserving good electrochemical stability and ionic conductivity. This could make them a promising foundation for all-hydrogel, sodium-based energy storage devices that are safe, sustainable, and mechanically compliant. KW - Battery PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653156 DO - https://doi.org/10.1021/acsapm.5c03031 SN - 2637-6105 SP - 1 EP - 8 PB - American Chemical Society (ACS) AN - OPUS4-65315 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Wohlleben, W. A1 - Mielke, Johannes A1 - Hodoroaba, Vasile-Dan A1 - Zimathies, Annett A1 - Bianchin, A. A1 - Lecloux, A. A1 - Roebben, G. A1 - Rauscher, H. A1 - Gibson, N. T1 - Development of an integrated approach based on validated and standardized methods to support the implementation of the EC recommendation for a definition of nanomaterial N2 - The VSSA approach has the important advantage over classifying, imaging and counting techniques that it does not involve dispersion protocols. Further, the BET technique as the basis for VSSA determination it is in widespread use, generates low costs and is specified for many commercial materials. Finally, the same equipment allows for a deeper analysis by full isotherm evaluation. The present deliverable assesses all NanoDefine powders, supplemented by further real-world materials (in total 26 powders), and quantitatively compares the relationship between the median size (by Electron Microscopy – considered as benchmark for the EC nanomaterial definition) vs. the size derived from VSSA. The VSSA method mitigates the challenges of EM to assess the thickness of platelets, but worked as well on fibbers and particles of irregular shapes. A screening strategy is proposed. If applied to the further data from real-world materials as validation set, this screening does achieve a correct classification, leaving only borderline materials for tier 2 assessment. KW - Nanomaterial KW - Classification KW - Regulation KW - VSSA KW - Size measurement KW - Particle size PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-398938 DO - https://doi.org/10.1007/s11051-017-3741-x SP - 1 EP - 26 PB - The NanoDefine Consortium CY - Wageningen, The Netherlands AN - OPUS4-39893 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Hodoroaba, Vasile-Dan A1 - Mielke, Johannes T1 - Techniques evaluation report for selection of characterisation methods N2 - This report is the result of a comprehensive study on the available CMs which come potentially in question for the reliable analysis of the number based size distribution of a nanomaterial according to the EC recommendation for a definition of nanomaterial. Based on the performance criteria already established in NanoDefine the potential CMs are evaluated according to studies available in the literature as well as following the expertise of the NanoDefine consortium partners. The specific advantages and disadvantages of each method with respect to its applicability to the scope of NanoDefine are particularly highlighted. An CM evaluation table is produced so that the mostly suited CMs with respect to the EC definition can be grouped and recommended to the corresponding NanoDefine work packages for further specific development (improvement and adaption), or for direct validation and standardisation, respectively. The actual evaluation report including the recommended CMs will be revised and, if necessary, eventually updated at the mid time of the project. The update will be jointly discussed in the NanoDefine consortium on the basis of the results of testing the methods on the NanoDefine real world materials. KW - Nanomaterial KW - Characterization method KW - EC definition PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-389473 UR - http://www.nanodefine.eu/publications/reports/NanoDefine_TechnicalReport_D3.1.pdf SP - D3.1, 1 EP - 57 CY - Wageningen, The Netherlands AN - OPUS4-38947 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neamtu, Mariana A1 - Nadejde, C. A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf A1 - Verestiuc, L. A1 - Panne, Ulrich T1 - Functionalized magnetic nanoparticles: Synthesis, characterization, catalytic application and assessment of toxicity N2 - Cost-effective water cleaning approaches using improved Treatment technologies, for instance based on catalytic processes with high activity catalysts, are urgently needed. The aim of our study was to synthesize efficient Fenton-like photo-catalysts for rapid degradation of persistent organic micropollutants in aqueous medium. Iron-based nanomaterials were chemically synthesized through simple procedures by immobilization of either iron(II) oxalate (FeO) or iron(III) citrate (FeC) on magnetite (M) nanoparticles stabilized with polyethylene glycol (PEG). Various investigation techniques were performed in order to characterize the freshly prepared catalysts. By applying advanced oxidation processes, the effect of catalyst dosage, hydrogen peroxide concentration and UV-A light exposure were examined for Bisphenol A (BPA) conversion, at laboratory scale, in mild conditions. The obtained results revealed that BPA degradation was rapidly enhanced in the presence of low-concentration H2O2, as well as under UV-A light, and is highly dependent on the surface characteristics of the catalyst. Complete photo-degradation of BPA was achieved over the M/PEG/FeO catalyst in less than 15 minutes. Based on the catalytic performance, a hierarchy of the tested catalysts was established: M/PEG/FeO > M/PEG/FeC > M/PEG. The results of cytotoxicity assay using MCF-7 cells indicated that the aqueous samples after treatment are less cytotoxic. KW - Bisphenol A KW - Magnetic nanocatalyst KW - Endocrine disruptor KW - Nanoparticle KW - Photodegradation KW - Fenton PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-448297 DO - https://doi.org/10.1038/s41598-018-24721-4 SN - 2045-2322 VL - 8 SP - Article 6278, 1 EP - 11 PB - Springer Nature CY - London AN - OPUS4-44829 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dhamo, Lorena A1 - Wegner, Karl David A1 - Würth, Christian A1 - Häusler, I. A1 - Hodoroaba, Vasile-Dan A1 - Resch-Genger, Ute T1 - Assessing the influence of microwave-assisted synthesis parameters and stabilizing ligands on the optical properties of AIS/ZnS quantum dots N2 - Luminescent semiconductor quantum dots (QDs) are frequently used in the life and material sciences as reporter for bioimaging studies and as active components in devices such as displays, light-emitting diodes, solar cells, and sensors. Increasing concerns regarding the use of toxic elements like cadmium and lead, and hazardous organic solvents during QD synthesis have meanwhile triggered the search for heavy-metal free QDs using green chemistry syntheses methods. Interesting candidates are ternary AgInS2 (AIS) QDs that exhibit broad photoluminescence (PL) bands, large effective Stokes shifts, high PL quantum yields (PL QYs), and long PL lifetimes, which are particularly beneficial for applications such as bioimaging, white light-emitting diodes, and solar concentrators. In addition, these nanomaterials can be prepared in high quality with a microwave-assisted (MW) synthesis in aqueous solution. The homogeneous heat diffusion and instant temperature rise of the MW synthesis enables a better control of QD nucleation and growth and thus increases the batch-to-batch reproducibility. In this study, we systematically explored the MW synthesis of AIS/ZnS QDs by varying parameters such as the order of reagent addition, precursor concentration, and type of stabilizing thiol ligand, and assessed their influence on the optical properties of the resulting AIS/ZnS QDs. Under optimized synthesis conditions, water-soluble AIS/ZnS QDs with a PL QY of 65% and excellent colloidal and long-term stability could be reproducible prepared. KW - Quantum dots KW - Microwave-assisted synthesis KW - AgInS KW - Aqueous synthesis PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567091 DO - https://doi.org/10.1038/s41598-022-25498-3 SN - 2045-2322 VL - 12 IS - 1 SP - 1 EP - 11 PB - Nature Publishing Group CY - London AN - OPUS4-56709 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radnik, Jörg A1 - Kersting, R. A1 - Hagenhoff, B. A1 - Bennet, Francesca A1 - Ciornii, Dmitri A1 - Nymark, P. A1 - Grafström, R. A1 - Hodoroaba, Vasile-Dan T1 - Reliable Surface Analysis Data of Nanomaterials in Support of Risk Assessment Based on Minimum Information Requirements N2 - The minimum information requirements needed to guarantee high-quality surface Analysis data of nanomaterials are described with the aim to provide reliable and traceable Information about size, shape, elemental composition and surface chemistry for risk assessment approaches. The widespread surface analysis methods electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and secondary ion mass spectrometry (SIMS) were considered. The complete analysis sequence from sample preparation, over measurements, to data analysis and data format for reporting and archiving is outlined. All selected methods are used in surface analysis since many years so that many aspects of the analysis (including (meta)data formats) are already standardized. As a practical analysis use case, two coated TiO2 reference nanoparticulate samples, which are available on the Joint Research Centre (JRC) repository, were selected. The added value of the complementary analysis is highlighted based on the minimum information requirements, which are well-defined for the analysis methods selected. The present paper is supposed to serve primarily as a source of understanding of the high standardization level already available for the high-quality data in surface analysis of nanomaterials as reliable input for the nanosafety community. KW - Electron microscopy KW - X-ray photoelectron spectroscopy KW - Secondary ion mass spectrometry KW - Energy dispersive X-ray spectroscopy KW - Standardization PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522683 DO - https://doi.org/10.3390/nano11030639 VL - 11 IS - 3 SP - 639 PB - MDPI AN - OPUS4-52268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brüngel, R. A1 - Rückert, J. A1 - Wohlleben, W. A1 - Babick, F. A1 - Ghanem, A. A1 - Gaillard, C. A1 - Mech, A. A1 - Rauscher, H. A1 - Hodoroaba, Vasile-Dan A1 - Weigel, S. A1 - Friedrich, C. M. T1 - NanoDefiner e-Tool: An Implemented Decision Support Framework for Nanomaterial Identification N2 - The European Commission’s recommendation on the definition of nanomaterial (2011/696/EU) established an applicable standard for material categorization. However, manufacturers face regulatory challenges during registration of their products. Reliable categorization is difficult and requires considerable expertise in existing measurement techniques (MTs). Additionally, organizational complexity is increased as different authorities’ registration processes require distinct reporting. The NanoDefine project tackled these obstacles by providing the NanoDefiner e-tool: A decision support expert system for nanomaterial identification in a regulatory context. It providesMT recommendations for categorization of specific materials using a tiered approach (screening/confirmatory), and was constructed with experts from academia and industry to be extensible, interoperable, and adaptable for forthcoming revisions of the nanomaterial definition. An implemented MT-driven material categorization scheme allows detailed description. Its guided workflow is suitable for a variety of user groups. Direct feedback and explanation enable transparent decisions. Expert knowledge is Held in a knowledge base for representation of MT performance criteria and physicochemical particle type properties. Continuous revision ensured data quality and validity. Recommendations were validated by independent case studies on industry-relevant particulate materials. Besides supporting material identification and registration, the free and open-source e-tool may serve as template for other expert systems within the nanoscience domain. KW - EC nanomaterial definition KW - Decision support KW - Expert system KW - Nanomaterial KW - Nanoparticles PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-492449 DO - https://doi.org/10.3390/ma12193247 VL - 12 IS - 19 SP - 3247 PB - MDPI CY - Basel, CH AN - OPUS4-49244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Waqfi, R. A. A1 - Khan, C. J. A1 - Irving, O. J. A1 - Matthews, Lauren A1 - Albrecht, T. T1 - Crowding Effects during DNA Translocation in Nanopipettes N2 - Quartz nanopipettes are an important emerging class of electric single-molecule sensors for DNA, proteins, their complexes, as well as other biomolecular targets. However, in comparison to other resistive pulse sensors, nanopipettes constitute a highly asymmetric environment and the transport of ions and biopolymers can become strongly directiondependent. For double-stranded DNA, this can include the characteristic translocation time and tertiary structure, but as we show here, nanoconfinement can also unlock capabilities for biophysical and bioanalytical studies at the single-molecule level. To this end, we show how the accumulation of DNA inside the nanochannel leads to crowding effects, and in some cases reversible blocking of DNA entry, and provide a detailed analysis based on a range of different DNA samples and experimental conditions. Moreover, using biotin-functionalized DNA and streptavidinmodified gold nanoparticles as target, we demonstrate in a proof-of-concept study how the crowding effect, and the resulting increased residence time in nanochannel, can be exploited by first injecting the DNA into the nanochannel, followed by incubation with the nanoparticle target and analysis of the complex by reverse translocation. We thereby integrate elements of sample processing and detection into the nanopipette, as an important conceptual advance, and make a case for the wider applicability of this device concept. KW - DNA translocation KW - Transport KW - Resistive-pulse sensing KW - Nanopores KW - Nanopipettes KW - Crowding KW - Confinement PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630448 DO - https://doi.org/10.1021/acsnano.5c01529 SN - 1936-086X VL - 19 IS - 17 SP - 1 EP - 9 PB - ACS Publications AN - OPUS4-63044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ferrari, Bruno A1 - Fantin, Andrea A1 - Said, D. A1 - Fitch, A. N. A1 - Suárez Ocano, Patricia A1 - Mishurova, Tatiana A1 - Roveda, Ilaria A1 - Kromm, Arne A1 - Darvishi Kamachali, Reza A1 - Bruno, Giovanni A1 - Evans, Alexander A1 - Requena, G. A1 - Agudo Jácome, Leonardo A1 - Serrano Munoz, Itziar T1 - The impact of scanning strategy on cell structures in PBF-LB/M/IN718: an in situ synchrotron x-ray diffraction study N2 - In additive manufacturing, any change of the process parameters, such as scanning strategy, directly affects the cooling rates, heat accumulation, and overall thermal history of the build. Consequently, parts built with different process parameters tend to have different levels of crystallographic texture, residual stress, and dislocation density. These features can influence the properties of the material and their development during post-processing operations. In this study, IN718 prisms were built by laser powder bed fusion (PBF-LB/M) using two different scanning strategies (continuous 67° rotations around the build direction, ROT, and alternating 0°/67° scans, ALT) to provide two different as-built conditions. In situ time-resolved synchrotron diffraction was performed during a solution heat treatment at 1027 °C for 1 h. Ex situ scanning electron microscopy was used to support and complement the in situ observations. An approach to quantify the effect of elemental microsegregation at the cell walls is developed based on the deconvolution of asymmetric γ-nickel matrix peaks. Following this approach, the scanning strategies are shown to affect the as-built fraction of cell walls in the material, resulting in a difference of approximately 5 %, in weight fraction, between ROT and ALT (19 % vs. 24 %, respectively). This microsegregation was observed to be rapidly homogenized during the heating ramp, and no significant changes to the peak shape in the γ peaks occurred during the isothermal part of the heat treatment, regardless of the scanning strategy. KW - Additive manufacturing KW - Inconel 718 KW - Synchrotron x-ray diffraction KW - Heat treatment KW - Laser powder bed fusion KW - Cellular microstructure PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-650958 DO - https://doi.org/10.1016/j.jmrt.2025.11.214 SN - 2238-7854 VL - 41 SP - 593 EP - 608 PB - Elsevier B.V. AN - OPUS4-65095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mehta, B. A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Markötter, Henning A1 - Bruno, Giovanni A1 - Hryha, E. A1 - Nyborg, L. A1 - Virtanen, E. T1 - Microstructure, mechanical properties and fracture mechanisms in a 7017 aluminium alloy tailored for powder bed fusion – laser beam N2 - This study addressed a 7017 Al-alloy tailored for powder bed fusion – laser beam (PBF-LB) process. The alloy was prepared by mixing 3 wt% Zr and 0.5 wt% TiC powder to standard pre-alloyed 7017 grade aluminium powder. This made printing of the alloys possible avoiding solidification cracking in the bulk and achieving high relative density (99.8 %). Such advanced alloys have significantly higher Young’s modulus (>80 GPa) than conventional Al-alloys (70–75 GPa), thus making them attractive for applications requiring high stiffness. The resulting microstructure in as-printed condition was rich in particles originating from admixed powders and primary precipitates/inclusions originating from the PBF-LB process. After performing a T6-like heat treatment designed for the PBF-LB process, the microstructure changed: Zr-nanoparticles and Fe- or Mg/Zn- containing precipitates formed thus providing 75 % increase in yield strength (from 254 MPa to 444 MPa) at the cost of decreasing ductility (∼20 % to ∼9 %). In-situ tensile testing combined with SXCT, and ex-situ tensile testing combined with fracture analysis confirmed that the fracture initiation in both conditions is highly dependent on defects originated during printing. However, cracks are deflected from decohesion around Zr-containing inclusions/precipitates embedded in the Al-matrix. This deflection is seen to improve the ductility of the material. KW - Additive manufacturing KW - Powder bed fusion Laser beam KW - X-ray computed tomography KW - Strengthening mechanisms KW - Crack propagation KW - Zirconium PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568243 DO - https://doi.org/10.1016/j.matdes.2023.111602 SN - 0264-1275 VL - 226 SP - 1 EP - 14 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-56824 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zerbst, Uwe A1 - Madia, Mauro A1 - Bruno, Giovanni A1 - Hilgenberg, Kai T1 - Towards a Methodology for Component Design of Metallic AM Parts Subjected to Cyclic Loading N2 - The safe fatigue design of metallic components fabricated by additive manufacturing (AM) is still a largely unsolved problem. This is primarily due to (a) a significant inhomogeneity of the material properties across the component; (b) defects such as porosity and lack of fusion as well as pronounced surface roughness of the asuilt components; and (c) residual stresses, which are very often present in the as‐built parts and need to be removed by post‐fabrication treatments. Such morphological and microstructural features are very different than in conventionally manufactured parts and play a much bigger role in determining the fatigue life. The above problems require specific solutions with respect to the identification of the critical (failure) sites in AM fabricated components. Moreover, the generation of representative test specimens characterized by similar temperature cycles needs to be guaranteed if one wants to reproducibly identify the critical sites and establish fatigue assessment methods taking into account the effect of defects on crack initiation and early propagation. The latter requires fracture mechanics‐based approaches which, unlike common methodologies, cover the specific characteristics of so‐called short fatigue cracks. This paper provides a discussion of all these aspects with special focus on components manufactured by laser powder bed fusion (L‐PBF). It shows how to adapt existing solutions, identifies fields where there are still gaps, and discusses proposals for potential improvement of the damage tolerance design of L‐PBF components KW - L‐PBF KW - Fatigue KW - Fracture KW - Defects PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525822 DO - https://doi.org/10.3390/met11050709 VL - 11 IS - 5 SP - 709 PB - MDPI CY - Basel AN - OPUS4-52582 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Léonard, Fabien A1 - Zhang, Zhen A1 - Krebs, Holger A1 - Bruno, Giovanni T1 - Structural and Morphological Quantitative 3D Characterisation of Ammonium Nitrate Prills by X-ray Computed Tomography N2 - The mixture of ammonium nitrate (AN) prills and fuel oil (FO), usually referred to as ANFO, is extensively used in the mining industry as a bulk explosive. One of the major performance predictors of ANFO mixtures is the fuel oil retention, which is itself governed by the complex pore structure of the AN prills. In this study, we present how X-ray computed tomography (XCT), and the associated advanced data processing workflow, can be used to fully characterise the structure and morphology of AN prills. We show that structural parameters such as volume fraction of the different phases and morphological parameters such as specific surface area and shape factor can be reliably extracted from the XCT data, and that there is a good agreement with the measured oil retention values. Importantly, oil retention measurements (qualifying the efficiency of ANFO as explosives) correlate well with the specific surface area determined by XCT. XCT can therefore be employed non-destructively; it can accurately evaluate and characterise porosity in ammonium nitrate prills, and even predict their efficiency. KW - ANFO KW - Explosives KW - Surface area KW - Porosity KW - XCT KW - Data processing PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505395 DO - https://doi.org/10.3390/ma13051230 VL - 13 IS - 5 (Special Issue "Micro Non-Destructive Testing and Evaluation") SP - 1230 PB - MDPI AN - OPUS4-50539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ulbricht, Alexander A1 - Mohr, Gunther A1 - Altenburg, Simon A1 - Oster, Simon A1 - Maierhofer, Christiane A1 - Bruno, Giovanni ED - Czujko, T. ED - Benedetti, M. T1 - Can Potential Defects in LPBF Be Healed from the Laser Exposure of Subsequent Layers? A Quantitative Study N2 - Additive manufacturing (AM) of metals and in particular laser powder bed fusion (LPBF) enables a degree of freedom in design unparalleled by conventional subtractive methods. To ensure that the designed precision is matched by the produced LPBF parts, a full understanding of the interaction between the laser and the feedstock powder is needed. It has been shown that the laser also melts subjacent layers of material underneath. This effect plays a key role when designing small cavities or overhanging structures, because, in these cases, the material underneath is feed-stock powder. In this study, we quantify the extension of the melt pool during laser illumination of powder layers and the defect spatial distribution in a cylindrical specimen. During the LPBF process, several layers were intentionally not exposed to the laser beam at various locations, while the build process was monitored by thermography and optical tomography. The cylinder was finally scanned by X-ray computed tomography (XCT). To correlate the positions of the unmolten layers in the part, a staircase was manufactured around the cylinder for easier registration. The results show that healing among layers occurs if a scan strategy is applied, where the orientation of the hatches is changed for each subsequent layer. They also show that small pores and surface roughness of solidified material below a thick layer of unmolten material (>200 µm) serve as seeding points for larger voids. The orientation of the first two layers fully exposed after a thick layer of unmolten powder shapes the orientation of these voids, created by a lack of fusion. KW - Computed tomography KW - Laser Powder Bed Fusion KW - In situ monitoring KW - infrared Thermography KW - Optical Tomography KW - Additive manufacturing KW - AISI 316L PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528778 DO - https://doi.org/10.3390/met11071012 VL - 11 IS - 7 SP - 1012 PB - MDPI CY - Basel AN - OPUS4-52877 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ziesche, R.F. A1 - Hack, J. A1 - Rasha, L. A1 - Maier, M. A1 - Tan, C. A1 - Heenan, T.M.M. A1 - Markötter, Henning A1 - Kardjilov, N. A1 - Manke, I. A1 - Kockelmann, W. A1 - Brett, D.J.L. A1 - Shearing, P.R. T1 - High-speed 4D neutron computed tomography for quantifying water dynamics in polymer electrolyte fuel cells N2 - In recent years, low-temperature polymer electrolyte fuel cells have become an increasingly important pillar in a zero-carbon strategy for curbing climate change, with their potential to power multiscale stationary and mobile applications. The performance improvement is a particular focus of research and engineering roadmaps, with water management being one of the major areas of interest for development. Appropriate characterisation tools for mapping the evolution, motion and removal of water are of high importance to tackle shortcomings. This article demonstrates the development of a 4D high-speed neutron imaging technique, which enables a quantitative analysis of the local water evolution. 4D visualisation allows the time-resolved studies of droplet formation in the flow fields and water quantification in various cell parts. Performance parameters for water management are identified that offer a method of cell classification, which will, in turn, support computer modelling and the engineering of next-generation flow field designs. KW - Neutron imaging KW - Tomography KW - Polymer electrolyte membrane fuel cell PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545978 DO - https://doi.org/10.1038/s41467-022-29313-5 VL - 13 IS - 1 SP - 1616 PB - Nature Publishing Group UK CY - London AN - OPUS4-54597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Serrano-Munoz, Itziar A1 - Fernández, R. A1 - Saliwan Neumann, Romeo A1 - González-Doncel, G. A1 - Bruno, Giovanni T1 - Dislocation substructures in pure aluminium after creep deformation as studied by electron backscatter diffraction N2 - In the present work, electron backscatter diffraction was used to determine the microscopic dislocation structures generated during creep (with tests interrupted at the steady state) in pure 99.8% aluminium. This material was investigated at two different stress levels, corresponding to the power-law and power-law breakdown regimes. The results show that the formation of subgrain cellular structures occurs independently of the crystallographic orientation. However, the density of these cellular structures strongly depends on the grain crystallographic orientation with respect to the tensile axis direction, with <111> grains exhibiting the highest densities at both stress levels. It is proposed that this behaviour is due to the influence of intergranular stresses, which is different in <111> and <001> grains. KW - Creep KW - Pure aluminium KW - Electron backscatter diffraction KW - Cellular structures KW - Power law and power-law breakdown PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552003 DO - https://doi.org/10.1107/S1600576722005209 SN - 0021-8898 SN - 1600-5767 VL - 55 SP - 860 EP - 869 PB - Wiley-Blackwell CY - Copenhagen AN - OPUS4-55200 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tsamos, Athanasios A1 - Evsevleev, Sergei A1 - Bruno, Giovanni T1 - Noise and blur removal from corrupted X-ray computed tomography scans: A multilevel and multiscale deep convolutional framework approach with synthetic training data (BAM SynthCOND) N2 - Regardless of the experimental care practiced in acquiring X-ray computed tomography (XCT) data, artifacts might still exist, such as noise and blur. This is typical for fast XCT data acquisitions (e.g., in-situ investigations), or low-dose XCT. Such artifacts can complicate subsequent analysis of the data. Digital filters can moderately cure extensive artifacts. The selection of filter type, intensity, and order of application is not always straight forward. To tackle these problems, a complete sequential multilevel, multi-scale framework: BAM SynthCOND, employing newly designed deep convolutional neural networks (DCNNs), was formulated. Although data conditioning with neural networks is not uncommon, the main complication is that completely artifact-free XCT data for training do not exist. Thus, training data were acquired from an in-house developed library (BAM SynthMAT) capable of generating synthetic XCT material microstructures. Some novel DCNN architectures were introduced (2D/3D ACEnet_Denoise, 2D/3D ACEnet_Deblur) along with the concept of Assertive Contrast Enhancement (ACE) training, which boosts the performance of neural networks trained with continuous loss functions. The proposed methodology accomplished very good generalization from low resemblance synthetic training data. Indeed, denoising, sharpening (deblurring), and even ring artifact removal performance were achieved on experimental post-CT scans of challenging multiphase Al-Si Metal Matrix Composite (MMC) microstructures. The conditioning efficiencies were: 92% for combined denoising/sharpening, 99% for standalone denoising, and 95% for standalone sharpening. The results proved to be independent of the artifact intensity. We believe that the novel concepts and methodology developed in this work can be directly applied on the CT projections prior to reconstruction, or easily be extended to other imaging techniques such as: Microscopy, Neutron Tomography, Ultrasonics, etc. KW - XCT Data Conditioning KW - Denoising Deblurring Sharpening KW - Deep Convolutional Neural Network (DCNN) KW - Synthetic Training Data KW - ACEnet KW - Metal Matrix Composite (MMC) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579129 DO - https://doi.org/10.1016/j.tmater.2023.100011 VL - 2 SP - 1 EP - 16 PB - Elsevier B.V. AN - OPUS4-57912 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Evans, Alexander A1 - Schröder, Jakob A1 - Pirling, T. A1 - Ulbricht, Alexander A1 - Suárez Ocaño, Patricia A1 - Bruno, Giovanni T1 - Resolving the Subsurface Residual Stress Maximum in Laser Powder Bed-Fused 316L Stainless Steel by Diffraction-Based Analysis N2 - Laser powder bed fusion (PBF-LB/M) is a metal additive manufacturing process. Due to the complex nature of the layer-wise, repeated heating and cooling cycles, it tends to generate high-magnitude residual stresses. If not correctly understood and mitigated through in- or post-process approaches, these residual stresses can be detrimental as they are often tensile at the surface. However, determining the magnitude and location of peak tensile residual stresses is not trivial as they are often located subsurface. This work focuses on determining the magnitude and location of these deleterious tensile residual stresses in a PBF-LB/316L specimen. Two diffraction-based Methods are used to reveal the relationship between the residual stresses and the underlying microstructure. On the one hand, high spatial resolution Neutron diffraction is used to determine triaxial stresses from the bulk to a depth of 0.15 mm. On the other hand, laboratory X-ray diffraction coupled with electrolytical layer removal allows the biaxial residual stress depth profile to be probed from the surface to a depth of about 0.6 mm. The results show a good agreement between the two methods. The peak residual stress is shown to be 500 MPa, which appears as a plateau between 0.08 and 0.35 mm in depth. KW - Residual stress KW - Diffraction KW - Laser Powder Bed Fusion KW - 316L KW - Additive manufacturing KW - Microstructure KW - AGIL PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652138 DO - https://doi.org/10.1007/s11837-025-07719-y SN - 1543-1851 VL - 77 IS - 12 SP - 9726 EP - 9737 PB - Springer Nature AN - OPUS4-65213 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Evsevleev, Sergei A1 - Paciornik, S. A1 - Bruno, Giovanni T1 - Advanced Deep Learning-Based 3D Microstructural Characterization of Multiphase Metal Matrix Composites N2 - The quantitative analysis of microstructural features is a key to understanding the micromechanical behavior of metal matrix composites (MMCs), which is a premise for their use in practice. Herein, a 3D microstructural characterization of a five-phase MMC is performed by synchrotron X-ray computed tomography (SXCT). A workflow for advanced deep learning-based segmentation of all individual phases in SXCT data is shown using a fully convolutional neural network with U-net architecture. High segmentation accuracy is achieved with a small amount of training data. This enables extracting unprecedently precise microstructural parameters (e.g., volume fractions and particle shapes) to be input, e.g., in micromechanical models. KW - Computed tomography KW - Convolutional neural networks KW - Deep learning KW - Metal matrix composites KW - Segmentations PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504261 DO - https://doi.org/10.1002/adem.201901197 SN - 1438-1656 VL - 22 IS - 4 SP - 1901197 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-50426 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröder, Jakob A1 - Evans, Alexander A1 - Polatidis, E. A1 - Čapek, J. A1 - Mohr, Gunther A1 - Serrano-Munoz, Itziar A1 - Bruno, Giovanni T1 - Understanding the impact of texture on the micromechanical anisotropy of laser powder bed fused Inconel 718 N2 - The manufacturability of metallic alloys using laser-based additive manufacturing methods such as laser powder bed fusion has substantially improved within the last decade. However, local melting and solidification cause hierarchically structured and crystallographically textured microstructures possessing large residual stress. Such microstructures are not only the origin of mechanical anisotropy but also pose metrological challenges for the diffraction-based residual stress determination. Here we demonstrate the influence of the build orientation and the texture on the microstructure and consequently the mechanical anisotropy of as-built Inconel 718. For this purpose, we manufactured specimens with [001]/[011]-, [001]- and [011]/[111]-type textures along their loading direction. In addition to changes in the Young’s moduli, the differences in the crystallographic textures result in variations of the yield and ultimate tensile strengths. With this in mind, we studied the anisotropy on the micromechanical scale by subjecting the specimens to tensile loads along the different texture directions during in situ neutron diffraction experiments. In this context, the response of multiple lattice planes up to a tensile strain of 10% displayed differences in the load partitioning and the residual strain accumulation for the specimen with [011]/[111]-type texture. However, the relative behavior of the specimens possessing an [001]/[011]- and [001]-type texture remained qualitatively similar. The consequences on the metrology of residual stress determination methods are discussed. KW - Laser powder bed fusion KW - Additive manufacturing KW - Electron backscatter diffraction KW - Tensile testing KW - Diffraction PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555840 DO - https://doi.org/10.1007/s10853-022-07499-9 SN - 1573-4803 VL - 2022 IS - 57 SP - 15036 EP - 15058 PB - Springer Science + Business Media B.V. CY - Dordrecht AN - OPUS4-55584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oster, Simon A1 - Fritsch, Tobias A1 - Ulbricht, Alexander A1 - Mohr, Gunther A1 - Bruno, Giovanni A1 - Maierhofer, Christiane A1 - Altenburg, Simon T1 - On the Registration of Thermographic In Situ Monitoring Data and Computed Tomography Reference Data in the Scope of Defect Prediction in Laser Powder Bed Fusion N2 - The detection of internal irregularities is crucial for quality assessment in metal-based additive manufacturing (AM) technologies such as laser powder bed fusion (L-PBF). The utilization of in-process thermography as an in situ monitoring tool in combination with post-process X-ray micro computed tomography (XCT) as a reference technique has shown great potential for this aim. Due to the small irregularity dimensions, a precise registration of the datasets is necessary as a requirement for correlation. In this study, the registration of thermography and XCT reference datasets of a cylindric specimen containing keyhole pores is carried out for the development of a porosity prediction model. The considered datasets show variations in shape, data type and dimensionality, especially due to shrinkage and material elevation effects present in the manufactured part. Since the resulting deformations are challenging for registration, a novel preprocessing methodology is introduced that involves an adaptive volume adjustment algorithm which is based on the porosity distribution in the specimen. Thus, the implementation of a simple three-dimensional image-to-image registration is enabled. The results demonstrate the influence of the part deformation on the resulting porosity location and the importance of registration in terms of irregularity prediction. KW - Selective laser melting (SLM) KW - Laser powder bed fusion (L-PBF) KW - Additive manufacturing (AM) KW - Process monitoring KW - Infrared thermography KW - X-ray computed tomography (XCT) KW - Defect detection KW - Image registration PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549412 DO - https://doi.org/10.3390/met12060947 VL - 12 IS - 6 SP - 1 EP - 21 PB - MDPI AN - OPUS4-54941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sprengel, Maximilian A1 - Mohr, Gunther A1 - Altenburg, Simon A1 - Evans, Alexander A1 - Serrano-Munoz, Itziar A1 - Kromm, Arne A1 - Pirling, T. A1 - Bruno, Giovanni A1 - Kannengießer, Thomas T1 - Triaxial Residual Stress in Laser Powder Bed Fused 316L: Effects of Interlayer Time and Scanning Velocity N2 - The triaxial distribution of the residual stress in laser powder bed fused austenitic steel 316L was determined by X-ray and neutron diffraction. The residual stress analysis results were linked to the thermal history of the specimens, which were manufactured with varying inter-layer-times and scanning velocities. A clear link between the in-process temperature of the specimens and the residual stress was found, based on in-situ monitoring data. KW - Stainless Steel KW - AGIL KW - Residual Stress KW - X-ray and Neutron Diffraction KW - Additive Manufacturing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542620 DO - https://doi.org/10.1002/adem.202101330 SP - 1 EP - 13 PB - Wiley-VCH GmbH AN - OPUS4-54262 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ulbricht, Alexander A1 - Ávila Calderón, Luis A1 - Sommer, Konstantin A1 - Mohr, Gunther A1 - Evans, Alexander A1 - Skrotzki, Birgit A1 - Bruno, Giovanni T1 - Evolution of Creep Damage of 316L Produced by Laser Powder Bed Fusion N2 - The damage mechanisms of metallic components produced by process laser powder bed fusion differ significantly from those typically observed in conventionally manufactured variants of the same alloy. This is due to the unique microstructures of additively manufactured materials. Herein, the focus is on the study of the evolution of creep damage in stainless steel 316L specimens produced by laser powder bed fusion. X-ray computed tomography is used to unravel the influence of the process-specific microstructure from the influence of the initial void distribution on creep damage mechanisms. The void distribution of two specimens tested at 600 °C and 650 °C is analyzed before a creep test, after an interruption, and after fracture. The results indicate that the formation of damage is not connected to the initial void distribution. Instead, damage accumulation at grain boundaries resulting from intergranular cracking is observed. KW - Creep KW - Computed Tomography KW - PBF-LB/M/316L KW - Laser Powder Bed Fusion KW - Microstructure KW - AISI 316L KW - Additive Manufacturing PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-574127 DO - https://doi.org/10.1002/adem.202201581 SP - 1 EP - 9 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-57412 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oesch, Tyler A1 - Weise, Frank A1 - Bruno, Giovanni T1 - Detection and Quantification of Cracking in Concrete Aggregate through Virtual Data Fusion of X-ray Computed Tomography Images N2 - In this work, which is part of a larger research program, a framework called “virtual data fusion“ was developed to provide an automated and consistent crack detection method that allows for the cross-comparison of results from large quantities of X-ray Computed Tomography (CT) data. A partial implementation of this method in a custom program was developed for use in research focused on crack quantification in Alkali-Silica Reaction (ASR)-sensitive concrete aggregates. During the CT image processing, a series of image analyses tailored for detecting specific, individual crack-like characteristics were completed. The results of these analyses were then “fused” in order to identify crack-like objects within the images with much higher accuracy than that yielded by any individual image analysis procedure. The results of this strategy demonstrated the success of the program in effectively identifying crack-like structures and quantifying characteristics, such as surface area and volume. The results demonstrated that the source of aggregate has a very significant impact on the amount of internal cracking, even when the mineralogical characteristics remain very similar. River gravels, for instance, were found to contain significantly higher levels of internal cracking than quarried stone aggregates of the same mineralogical type. KW - X-ray Computed Tomography (CT) KW - Alkali-Silica Reaction (ASR) KW - Crack Detection KW - Damage Quantification KW - ASR-Sensitive Aggregate PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512170 DO - https://doi.org/10.3390/ma13183921 VL - 13 IS - 18 SP - Paper 3921 PB - MDPI CY - Basel, Switzerland AN - OPUS4-51217 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Belli, Renan A1 - Hartmann, Sabine A1 - Lubauer, Julia A1 - Pereira, Raíssa Monteiro A1 - Hurle, Katrin A1 - Yin, Ling A1 - Mieller, Björn A1 - Lohbauer, Ulrich T1 - Improving the chipping resistance of pre-sintered zirconia white-bodies N2 - Objectives: The high occurrence of fractures, cracking and chipping of zirconia pre-sintered blanks and blocks during machining decreases their yield and can transfer lifetime-limiting racks to the final sintered restoration. This study has the objective of characterizing the mechanical and fracture properties of two zirconia compositions while varying temperature and time of pre-sintering, in order to assess the space for possible improvement. Methods: We selected two typical granular powders with 3 mol% (3YSZ, Zpex®, Tosoh) or 5 mol% (5YSZ, Zpex Smile®, Tosoh) yttria-stabilized zirconia and two pre-sintered commercial analogs (IPS e.max® ZirCAD MO, Ivoclar and Katana™ STML, Kuraray). The debinding and pre-sintering stages of the experimental powders were characterized using thermal analyses (differential scanning calorimetry and thermogravimetry), and the crystal phase composition was quantified using X-ray diffraction (XRD). Physical and mechanical properties such as density, hardness, flexural modulus, biaxial flexural strength and fracture toughness were measured for two pre-sintering temperatures (1000 ◦C, 1100 ◦C) and increasing holding times at those temperatures (2 h, 4 h, 6 h). The chipping resistance for those conditions was quantified using the edge chipping test using a Vickers diamond indenter. Results: Thermal analyses revealed that both powders show comparable debinding behavior and contained approx. 3.8 mass % organic binder, which burns-out completely between 300 and 400 ◦C. The crystallographic phase changes occurring during the 2–6 h at 1000 ◦C and 1100 ◦C was not detectable in the DSC signal, but quantifiable by XRD. Namely, a major content of monoclinic phase in both powders transforms completely into the two tetragonal phases, starting below 1000 ◦C and concluding above 1100 ◦C. All physical and mechanical properties increased with holding time for both temperatures, though more steeply for pre-sintering at 1100◦C. Edge chipping resistance response was well aligned with other fracture properties, with a more marked improvement for 3YSZ pre-sintered at 1100 ◦C. For all properties, the 3YSZ zirconia showed statistically-higher values for the same temperature-time conditions, in agreement with the values obtained for the commercial materials as well. Significance: The results demonstrate the weakness of pre-sintered zirconia products concerning fracture properties, but also the potential for improvement as related to type of zirconia and pre-sintering conditions. This study outlines the use of a set of mechanical tests that can characterize chipping resistance and guide future research engaging in optimizing the machining resistance of pre-sintered zirconia products. KW - Zirconia KW - Fracture KW - White body KW - Dental materials KW - Pre-sintering PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653457 DO - https://doi.org/10.1016/j.dental.2025.12.012 SN - 0109-5641 SP - 1 EP - 12 PB - Elsevier Inc. AN - OPUS4-65345 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jamro, R. A1 - Mente, Tobias A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Al-Falahat, Ala'A. M. A1 - Woracek, R. A1 - Manke, I. A1 - Griesche, Axel T1 - Temperature distribution during welding measured by neutron imaging N2 - This study was carried out to investigate the neutron transmission signal as a function of sample temperature during a welding process. A theoretical description that includes the Debye-Waller factor was used to describe the temperature influence on the neutron crosssections. Neutron imaging using a monochromatic beam helps to observe transmission variations related to the material temperature. In-situ neutron imaging of welding experiments show the distribution of the temperature in bulk steel samples. The performed finite element modelling of expected temperature distributions shows good agreement with the obtained experimental data. KW - Neutron imaging KW - Debye-Waller-Faktor PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586268 DO - https://doi.org/10.1088/1742-6596/2605/1/012026 VL - 2605 SP - 1 EP - 10 PB - IOP Publishing Ltd. AN - OPUS4-58626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schilling, Markus A1 - Bayerlein, Bernd A1 - von Hartrott, Philipp A1 - Waitelonis, Jörg A1 - Birkholz, Henk A1 - Portella, Pedro Dolabella A1 - Skrotzki, Birgit T1 - FAIR and Structured Data: A Domain Ontology Aligned with Standard‐Compliant Tensile Testing N2 - The digitalization of materials science and engineering (MSE) is currently leading to remarkable advancements in materials research, design, and optimization, fueled by computer‐driven simulations, artificial intelligence, and machine learning. While these developments promise to accelerate materials innovation, challenges in quality assurance, data interoperability, and data management have to be addressed. In response, the adoption of semantic web technologies has emerged as a powerful solution in MSE. Ontologies provide structured and machine‐actionable knowledge representations that enable data integration, harmonization, and improved research collaboration. This study focuses on the tensile test ontology (TTO), which semantically represents the mechanical tensile test method and is developed within the project Plattform MaterialDigital (PMD) in connection with the PMD Core Ontology. Based on ISO 6892‐1, the test standard‐compliant TTO offers a structured vocabulary for tensile test data, ensuring data interoperability, transparency, and reproducibility. By categorizing measurement data and metadata, it facilitates comprehensive data analysis, interpretation, and systematic search in databases. The path from developing an ontology in accordance with an associated test standard, converting selected tensile test data into the interoperable resource description framework format, up to connecting the ontology and data is presented. Such a semantic connection using a data mapping procedure leads to an enhanced ability of querying. The TTO provides a valuable resource for materials researchers and engineers, promoting data and metadata standardization and sharing. Its usage ensures the generation of finable, accessible, interoperable, and reusable data while maintaining both human and machine actionability. KW - Data Interoperability KW - Domain Ontology Development KW - FAIR Data Management KW - Knowledge Representation KW - Tensile Test Ontology KW - Semantic Web Technologies PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598142 DO - https://doi.org/10.1002/adem.202400138 SN - 1438-1656 SP - 1 EP - 19 PB - Wiley VHC-Verlag AN - OPUS4-59814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rossi, Andrea A1 - Corrao, Elena A1 - Alladio, Eugenio A1 - Drobne, Damjana A1 - Hodoroaba, Vasile-Dan A1 - Jurkschat, Kerstin A1 - Kononenko, Veno A1 - Madbouly, Loay Akmal A1 - Mrkwitschka, Paul A1 - Yasamin, Nakhli A1 - Novak, Sara A1 - Radnik, Jörg A1 - Saje, Špela A1 - Santalucia, Rosangela A1 - Sordello, Fabrizio A1 - Pellegrino, Francesco T1 - Multivariate optimization and characterization of graphene oxide via design of experiments and chemometric analysis N2 - Controlling the structure and properties of graphene oxide (GO) remains a challenge due to the poor reproducibility of conventional synthetic protocols and limited understanding of parameter-property relationships. In this study, we present an integrated analytical framework that combines Design of Experiments (DoE) with chemometric modelling to systematically assess the effects of eight synthesis variables on GO’s physicochemical and functional features. A Plackett–Burman experimental design enabled efficient screening of synthesis conditions, while comprehensive characterization (spanning UV–Vis spectroscopy, XPS, SEM–EDX, TEM–EDX, and XRD) was coupled with multivariate tools (Principal Component Analysis and Multiple Linear Regression) to identify statistically significant correlations between synthetic inputs and material responses. Notably, we demonstrate that UV–Vis spectra can serve as a robust proxy for oxidation state, offering a rapid and accessible alternative to surface-sensitive methods. The approach yields a predictive analytical toolkit for guiding GO synthesis and highlights a generalizable strategy for the rational design of flat nanomaterials. This work supports reproducible, resource-efficient material development aligned with Safe and Sustainable by Design (SSbD) principles. KW - Graphene oxide KW - 2D-materials KW - Design of Experiment KW - Synthesis KW - Chemometric analysis PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652576 DO - https://doi.org/10.1016/j.flatc.2025.100988 SN - 2452-2627 VL - 55 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-65257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Silbernagl, Dorothee A1 - Kömmling, Anja A1 - Zaghdoudi, Maha A1 - Ghasem Zadeh Khorasani, Media A1 - Jaunich, Matthias T1 - Data-driven nanomechanical study of filled fluoroelastomer aged in air and hydrogen atmosphere N2 - Fluoroelastomer (FKM) composites are typically used as sealing materials in challenging non-ambient environments. Depending on the environment, two main aging mechanisms, chemical aging, and physical aging, can be identified. Chemical aging, the degradation of the elastomer, is present for example in thermal-oxidative conditions and can be directly observed as it affects the bulk. Physical aging, relaxation and rearrangement of the elastomers segmental conformation is commonly observed at elevated temperatures and effects predominantly the elastomer interphase. As a highly localized nanoscopic effect it is usually observed indirectly by phenomological approaches and not systematically understood. In this study, as a typical example for chemical aging, filled FKM was aged in air (150°C, 100 days). Physical aging of FKM was realized by exposure to chemically inert H2 (150°C, 50 bar, 100 days), since temperature and gas-induced swelling is known to promote physical aging. The effects of both conditions are directly compared with the initial unaged material. We use atomic force microscopy (AFM) force spectroscopy as a method to resolve nanoscopic heterogeneous FKM. With this method the effect of aging on the spatially distinguishable material phases was directly observed. In thermal oxidative aged FKM the matrix shows a decrease in van der Waals interactions and stiffness, indicating dehydrofluorination and chain scission. In H2 aged FKM, the development of an immobilized amorphous interphase (IAP) was observed, indicating physical aging. By additionally evaluating a larger data set with supervised machine learning, these observations were validated for a larger, statistically representative sample area, allowing conclusions to be drawn about the macroscopic behaviour of the material. KW - Fluoroelastomer KW - Atomic force microscopy KW - Data-driven KW - Hydrogen KW - Ageing mechanism KW - Physical aging KW - Polymer interphase PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-648154 DO - https://doi.org/10.1016/j.polymdegradstab.2025.111715 SN - 0141-3910 VL - 242 SP - 1 EP - 10 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-64815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bhadeliya, Ashok A1 - Rehmer, Birgit A1 - Fedelich, Bernard A1 - Jokisch, T. A1 - Skrotzki, Birgit A1 - Olbricht, Jürgen T1 - Fatigue and fracture in dual-material specimens of nickel-based alloys fabricated by hybrid additive manufacturing N2 - The integration of additive manufacturing with traditional processes, termed hybrid additive manufacturing, has expanded its application domain, particularly in the repair of gas turbine blade tips. However, process-related defects in additively manufactured materials, interface formation, and material property mismatches in dual-material structures can significantly impact the fatigue performance of components. This investigation examines the low cycle fatigue and fatigue crack growth behaviors in dual-material specimens of nickel-based alloys, specifically the additively manufactured STAL15 and the cast alloy 247DS, at elevated temperatures. Low cycle fatigue experiments were conducted at temperatures of 950 °C and 1000 °C under a range of strain levels (0.3%–0.8%) and fatigue crack growth tests were conducted at 950 °C with stress ratios of 0.1 and −1. Fractographic and microscopic analyses were performed to comprehend fatigue crack initiation and crack growth mechanisms in the dual-material structure. The results consistently indicated crack initiation and fatigue fracture in the additively manufactured STAL15 material. Notably, fatigue crack growth retardation was observed near the interface when the crack extended from the additively manufactured STAL15 material to the perpendicularly positioned interface. This study highlights the importance of considering yield strength mismatch, as well as the potential effects of residual stresses and grain structure differences, in the interpretation of fatigue crack growth behavior at the interface. KW - Hybrid additive manufacturing KW - Dual-material nickel-based alloys KW - High-temperature fatigue crack growth KW - Low cycle fatigue PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-609340 DO - https://doi.org/10.1016/j.jmrt.2024.08.211 SN - 2238-7854 VL - 32 SP - 3737 EP - 3749 PB - Elsevier B.V. AN - OPUS4-60934 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hülagü, Deniz A1 - Tobias, Charlie A1 - Dao, Radek A1 - Komarov, Pavel A1 - Rurack, Knut A1 - Hodoroaba, Vasile-Dan T1 - Towards 3D determination of the surface roughness of core–shell microparticles as a routine quality control procedure by scanning electron microscopy N2 - AbstractRecently, we have developed an algorithm to quantitatively evaluate the roughness of spherical microparticles using scanning electron microscopy (SEM) images. The algorithm calculates the root-mean-squared profile roughness (RMS-RQ) of a single particle by analyzing the particle’s boundary. The information extracted from a single SEM image yields however only two-dimensional (2D) profile roughness data from the horizontal plane of a particle. The present study offers a practical procedure and the necessary software tools to gain quasi three-dimensional (3D) information from 2D particle contours recorded at different particle inclinations by tilting the sample (stage). This new approach was tested on a set of polystyrene core-iron oxide shell-silica shell particles as few micrometer-sized beads with different (tailored) surface roughness, providing the proof of principle that validates the applicability of the proposed method. SEM images of these particles were analyzed by the latest version of the developed algorithm, which allows to determine the analysis of particles in terms of roughness both within a batch and across the batches as a routine quality control procedure. A separate set of particles has been analyzed by atomic force microscopy (AFM) as a powerful complementary surface analysis technique integrated into SEM, and the roughness results have been compared. KW - Core–shell particles KW - Image analysis KW - Roughness KW - Scanning electron microscopy KW - Atomic force microscopy KW - Tilting KW - Batch analysis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-607590 DO - https://doi.org/10.1038/s41598-024-68797-7 SN - 2045-2322 VL - 14 IS - 1 SP - 1 EP - 13 PB - Springer Science and Business Media LLC AN - OPUS4-60759 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beygi Nasrabadi, Hossein A1 - Norouzi, Ebrahim A1 - Sack, Harald A1 - Skrotzki, Birgit T1 - Performance Evaluation of Upper‐Level Ontologies in Developing Materials Science Ontologies and Knowledge Graphs N2 - This study tackles a significant challenge in ontology development for materials science: selecting the most appropriate upper‐level ontologies for creating application‐level ontologies and knowledge graphs. Focusing on the use case of Brinell hardness testing, the research assesses the performance of various top‐level ontologies (TLOs)—basic formal ontology (BFO), elementary multiperspective material ontology (EMMO), and provenance ontology (PROVO)—in developing Brinell testing ontologies (BTOs). Consequently, three versions of BTOs are created using combinations of these TLOs along with their integrated mid‐ and domain‐level ontologies. The performance of these ontologies is evaluated based on ten parameters: semantic richness, domain coverage, extensibility, complexity, mapping efficiency, query efficiency, integration with other ontologies, adaptability to different data contexts, community acceptance, and documentation and maintainability. The results show that all candidate TLOs can effectively develop BTOs, each with its distinct advantages. BFO provides a well‐structured, understandable hierarchy, and excellent query efficiency, making it suitable for integration across various ontologies and applications. PROVO demonstrates balanced performance with strong integration capabilities. Meanwhile, EMMO offers high semantic richness and domain coverage, though its complex structure impacts query efficiency and integration with other ontologies. KW - Materials Science KW - Ontology KW - Knowledge Graph PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612227 DO - https://doi.org/10.1002/adem.202401534 SN - 1527-2648 SP - 1 EP - 18 PB - Wiley AN - OPUS4-61222 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sonntag, Nadja A1 - Piesker, Benjamin A1 - Ávila Calderón, Luis A1 - Mohr, Gunther A1 - Rehmer, Birgit A1 - Agudo Jácome, Leonardo A1 - Hilgenberg, Kai A1 - Evans, Alexander A1 - Skrotzki, Birgit T1 - Tensile and Low‐Cycle Fatigue Behavior of Laser Powder Bed Fused Inconel 718 at Room and High Temperature N2 - This study investigates the room‐ and high‐temperature (650 °C) tensile and low‐cycle‐fatigue behavior of Inconel 718 produced by laser powder bed fusion (PBF‐LB/M) with a four‐step heat treatment and compares the results to the conventional wrought material. The microstructure after heat treatment is characterized on different length scales. Compared to the wrought variant, the elastic and yield properties are comparable at both test temperatures while tensile strength, ductility, and strain hardening capacity are lower. The fatigue life of the PBF‐LB/M variant at room temperature is slightly lower than that of the wrought material, while at 650 °C, it is vice versa. The cyclic stress response for both material variants is characterized by cyclic softening, which is more pronounced at the higher test temperature. High strain amplitudes (≥0.7%) at room temperature and especially a high testing temperature result in the formation of multiple secondary cracks at the transitions of regions comprising predominantly elongated grain morphology and columns of stacked grains with ripple patterns in the PBF‐LB/M material. This observation and pronounced crack branching and deflection indicate that the cracks are controlled by sharp micromechanical gradients and local crystallite clusters. KW - Additive manufacturing KW - Fatigue damage KW - Heat treatment KW - Inconel 718 KW - Laser powder bed fusion KW - Low-cycle fatigue KW - Tensile strength PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-599316 DO - https://doi.org/10.1002/adem.202302122 SN - 1527-2648 SP - 1 EP - 17 PB - Wiley AN - OPUS4-59931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bhadeliya, Ashok A1 - Rehmer, Birgit A1 - Fedelich, Bernard A1 - Jokisch, T. A1 - Skrotzki, Birgit A1 - Olbricht, Jürgen T1 - Fatigue crack growth behavior of Alloy 247DS brazed joints at high temperatures N2 - Gas turbine components made of nickel-based alloys can be repaired through diffusion brazing. However, process-induced imperfections, defects within the brazing zone, and material property mismatches between the braze alloy and base material may facilitate crack initiation and propagation, ultimately leading to early component failure. To gain insight into the crack growth mechanism and quantitatively characterize fatigue crack growth behavior within brazing zones, fatigue crack growth (FCG) experiments were conducted on brazed joint specimens of nickel-based alloy Alloy 247DS at a temperature of 950 ◦C and a stress ratio R = 0.1. The FCG tests were complemented by fractographic and microstructural analyses, to elucidate the relationship between crack growth mechanisms and the microstructure of the brazed joint. The results demonstrate stable crack propagation within the brazing zone and the nickel-based braze alloy. The latter contains brittle eutectic boride phases and intermetallic phases that reduce the resistance to crack propagation compared to the parent material. This study demonstrates the applicability of standard FCG experimental procedures to fusion zones, thereby enabling a preliminary understanding of crack growth behavior in brazing zones. KW - Diffusion brazing KW - High-temperature fatigue crack growth KW - Nickel-based alloys KW - Alloy 247DS PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615250 DO - https://doi.org/10.1016/j.msea.2024.147488 SN - 0921-5093 VL - 918 SP - 1 EP - 15 PB - Elsevier B.V. AN - OPUS4-61525 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beygi Nasrabadi, Hossein A1 - Hanke, Thomas A1 - Skrotzki, Birgit T1 - Semantic Representation of Low‐Cycle‐Fatigue Testing Data Using a Fatigue Test Ontology and ckan.kupferdigital Data Management System N2 - Addressing a strategy for publishing open and digital research data, this article presents the approach for streamlining and automating the process of storage and conversion of research data to those of semantically queryable data on the web. As the use case for demonstrating and evaluating the digitalization process, the primary datasets from low‐cycle‐fatigue testing of several copper alloys are prepared. The fatigue test ontology (FTO) and ckan.kupferdigital data management system are developed as two main prerequisites of the data digitalization process. FTO has been modeled according to the content of the fatigue testing standard and by reusing the basic formal ontology, industrial ontology foundry core ontology, and material science and engineering ontology. The ckan.kupferdigital data management system is also constructed in such a way that enables the users to prepare the protocols for mapping the datasets into the knowledge graph and automatically convert all the primary datasets to those machine‐readable data which are represented by the web ontology language. The retrievability of the converted digital data is also evaluated by querying the example competency questions, confirming that ckan.kupferdigital enables publishing open data that can be highly reused in the semantic web. KW - Accessible KW - CKAN KW - Interoperable KW - Digitalizations KW - Ontologies KW - Reusable data KW - Fatigue testing PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-604991 UR - https://onlinelibrary.wiley.com/doi/10.1002/adem.202400675 DO - https://doi.org/10.1002/adem.202400675 SN - 1527-2648 SP - 1 EP - 11 PB - Wiley AN - OPUS4-60499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Kai A1 - Mirabella, Francesca A1 - Knigge, Xenia A1 - Mezera, Marek A1 - Weise, Matthias A1 - Sahre, Mario A1 - Wasmuth, Karsten A1 - Voss, Heike A1 - Hertwig, Andreas A1 - Krüger, Jörg A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan A1 - Bonse, Jörn T1 - Chemical and topographical changes upon sub-100-nm laser-induced periodic surface structure formation on titanium alloy: the influence of laser pulse repetition rate and number of over-scans N2 - Titanium and its alloys are known to allow the straightforward laser-based manufacturing of ordered surface nanostructures, so-called high spatial frequency laser-induced periodic surface structures (HSFL). These structures exhibit sub-100 nm spatial periods – far below the optical diffraction limit. The resulting surface functionalities are usually enabled by both, topographic and chemical alterations of the nanostructured surfaces. For exploring these effects, multi-method characterizations were performed here for HSFL processed on Ti–6Al–4V alloy upon irradiation with near-infrared ps-laser pulses (1030 nm, ≈1 ps pulse duration, 1–400 kHz) under different laser scan processing conditions, i.e., by systematically varying the pulse repetition frequency and the number of laser irradiation passes. The sample characterization involved morphological and topographical investigations by scanning electron microscopy (SEM), atomic force microscopy (AFM), tactile stylus profilometry, as well as near-surface chemical analyses hard X-ray photoelectron spectroscopy (HAXPES) and depth-profiling time-of-flight secondary ion mass spectrometry (ToF-SIMS). This provides a quantification of the laser ablation depth, the geometrical HSFL characteristics and enables new insights into the depth extent and the nature of the non-ablative laser-induced near-surface oxidation accompanying these nanostructures. This allows to answer the questions how the processing of HSFL can be industrially scaled up, and whether the latter is limited by heat-accumulation effects. T2 - 2023 E-MRS Spring Meeting, Symposium L "Making light matter: lasers in material sciences and photonics" CY - Strasbourg, France DA - 29.05.2023 KW - Laser-induced periodic surface structures (LIPSS) KW - Ultrashort laser pulses KW - Laser processing KW - Hard X-ray photoelectron spectroscopy (HAXPES) KW - Time-of-flight secondary ion mass spectrometry (ToF-SIMS) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589902 UR - https://onlinelibrary.wiley.com/doi/full/10.1002/pssa.202300719 DO - https://doi.org/10.1002/pssa.202300719 SN - 1862-6319 VL - 221 IS - 15 SP - 1 EP - 12 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-58990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stockmann, Jörg Manfred A1 - Radnik, Jörg A1 - Bütefisch, Sebastian A1 - Weimann, Thomas A1 - Hodoroaba, Vasile-Dan T1 - A New XPS Test Material for More Reliable Analysis of Microstructures N2 - A reference material is required for small‐area XPS because it has been used more frequently for surface control in recent years and many operators use incorrect field of views. To address this problem, we developed a test material starting in 2019. We optimised this XPS test material dedicated to the control of analysis position on the sample, with respect to the following factors: type of XPS instruments available on the market, the manufacturing process and sample handling. Test structures are now aligned along lines instead of on a circle radius, so that the individual structures can be accessed more quickly and easily. In addition, a larger test structure of 300 μm and another one in an intermediate size of 18 μm were added. Smaller test structures under 50 μm have been annotated with finder grids/arrows around them so that they are easier to find. Further, the manufacturing process was changed from e‐beam lithography to a mask process to be able to offer the test material at a favourable price. The use of masks also had to be adapted for the new manufacturing process so that the smallest square structures are also realised as such and do not show any distortion of the structure boundaries. The quality control using a metrological SEM confirmed a very reproducible manufacturing process. It is demonstrated that the test material can be successfully employed to find the most suitable beam size of the XPS system used for the analysis of small (μm range) surface features. KW - Small-area measurements KW - Test material KW - XPS KW - XPS imaging PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-616577 DO - https://doi.org/10.1002/sia.7367 SP - 1 EP - 6 PB - Wiley AN - OPUS4-61657 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wasmer, Paul A1 - Bulling, Jannis A1 - Gravenkamp, H. A1 - Prager, Jens T1 - Acoustic-structure interaction in the Scaled Boundary Finite Element Method for primsatic geometries N2 - Due to the short wavelength compared to the dimensions of the structure, the simulation of ultrasonic waves is still a challenging task. A numerical method well suited for this purpose is the semi-analytical Scaled Boundary Finite Element Method (SBFEM). When applying this method, only the boundary of a computational domain is discretized using finite elements, while the interior is described by an analytical ansatz. Hence, the number of degrees of freedom is reduced significantly compared to the classical Finite Element Method (FEM). In recent years, a particular formulation of the SBFEM for the simulation of ultrasonic guided waves was developed. The method constitutes an efficient algorithm for prismatic structures of arbitrary length, such as plates, pipes, or beams. Wave propagation phenomena in such structures can be modeled for isotropic and anisotropic inhomogeneous waveguides. Even though the method is an efficient tool for the simulation of guided waves in solid media, a reliable model for the simulation of acoustic wave propagation in fluids as well as acoustic-structure interaction in terms of SBFEM is still missing. In principle, the fluid can be described by a displacement-based formulation and thus be implemented in existing SBFEM algorithms for solid bodies. However, due to the discretization with classical finite elements, spurious modes occur, which cannot be separated from the physical modes straightforwardly. The spurious modes can be suppressed using a penalty parameter. Although very accurate results were achieved for some problems, this procedure has been proven unreliable for certain cases. For this reason, we propose a different approach in this contribution. We employ a pressure model to simulate the acoustic behavior of fluids. The implementation of the pressure model results in a higher effort due to the necessity of incorporating coupling terms, but it presents a stable alternative without spurious modes. The accuracy of the method is demonstrated in comparison with analytical solutions and results obtained using the FEM. T2 - GACM 2019 CY - Kassel, Germany DA - 28.08.2019 KW - Scaled Boundary Finite Element Method KW - Guided Waves KW - Ultrasound KW - Acoustic-Structure Interaction PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-497364 UR - https://www.upress.uni-kassel.de/katalog/abstract.php?978-3-7376-5093-9 SN - 978-3-86219-5093-9 DO - https://doi.org/10.19211/KUP9783737650939 SP - 347 EP - 350 AN - OPUS4-49736 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -