TY - JOUR A1 - Kuhlich, Paul A1 - Emmerling, Franziska A1 - Kraus, Werner A1 - Nehls, Irene A1 - Piechotta, Christian T1 - 1-(4-bromo-3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydronaphthalen-2-yl)ethan-1-one: a precursor for phase-I metabolite of AHTN JF - Acta crystallographica E N2 - The title compound, C18H25BrO, crystallized as a racemate with four independent molecules in the asymmetric unit. In the crystal, three of these four molecules are linked via C-Br...Br-C halogen bonds [Br...Br = 3.662 (2) and 3.652 (2) Å], forming dimers. PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-279935 DO - https://doi.org/10.1107/S1600536813006934 SN - 1600-5368 VL - 69 IS - 4 SP - o545, sup-1 EP - sup-17 PB - Munksgaard CY - Copenhagen AN - OPUS4-27993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kasper, J. A1 - Hermanns, M. A1 - Bantz, C. A1 - Maskos, Michael A1 - Stauber, R. A1 - Pohl, C. A1 - Unger, R. E. A1 - Kirkpatrick, J.C. T1 - Inflammatory and cytotoxic responses of an alveolar-capillary coculture model to silica nanoparticles: comparison with conventional monocultures JF - Particle and fibre toxicology N2 - To date silica nanoparticles (SNPs) play an important role in modern technology and nanomedicine. SNPs are present in various materials (tyres, electrical and thermal insulation material, photovoltaic facilities). They are also used in products that are directly exposed to humans such as cosmetics or toothpaste. For that reason it is of great concern to evaluate the possible hazards of these engineered particles for human health. Attention should primarily be focussed on SNP effects on biological barriers. Accidentally released SNP could, for example, encounter the alveolar-capillary barrier by inhalation. In this study we examined the inflammatory and cytotoxic responses of monodisperse amorphous silica nanoparticles (aSNPs) of 30 nm in size on an in vitro coculture model mimicking the alveolar-capillary barrier and compared these to conventional monocultures. Methods Thus, the epithelial cell line, H441, and the endothelial cell line, ISO-HAS-1, were used in monoculture and in coculture on opposite sides of a filter membrane. Cytotoxicity was evaluated by the MTS assay, detection of membrane integrity (LDH release), and TER (Transepithelial Electrical Resistance) measurement. Additionally, parameters of inflammation (sICAM-1, IL-6 and IL-8 release) and apoptosis markers were investigated. Results Regarding toxic effects (viability, membrane integrity, TER) the coculture model was less sensitive to apical aSNP exposure than the conventional monocultures of the appropriate cells. On the other hand, the in vitro coculture model responded with the release of inflammatory markers in a much more sensitive fashion than the conventional monoculture. At concentrations that were 10-100fold less than the toxic concentrations the apically exposed coculture showed a release of IL-6 and IL-8 to the basolateral side. This may mimic the early inflammatory events that take place in the pulmonary alveoli after aSNP inhalation. Furthermore, a number of apoptosis markers belonging to the intrinsic pathway were upregulated in the coculture following aSNP treatment. Analysis of the individual markers indicated that the cells suffered from DNA damage, hypoxia and ER-stress. Conclusion We present evidence that our in vitro coculture model of the alveolar-capillary barrier is clearly advantageous compared to conventional monocultures in evaluating the extent of damage caused by hazardous material encountering the principle biological barrier in the lower respiratory tract. KW - Silica nanoparticles KW - Alveolar-capillary coculture model KW - Cytotoxicity PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-254217 DO - https://doi.org/10.1186/1743-8977-8-6 SN - 1743-8977 VL - 8 IS - 6 SP - 1 EP - 16(?) PB - BioMed Central CY - London AN - OPUS4-25421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schukar, Vivien A1 - Kusche, Nadine A1 - Kalinka, Gerhard A1 - Habel, Wolfgang T1 - Field deployable fiber bragg grating strain patch for long-term stable health monitoring applications JF - Applied sciences N2 - A fiber Bragg grating (FBG) strain patch specially adapted for long-term and high-strain applications has been developed and characterized. The design concept for the patch is based on a glass-fiber reinforced plastic (gfrp) carrier material. The developed concept for the FBG integration into the carrier material was derived from reliable integration procedure of FBG sensors into composite structures. The patches' temperature sensitivity, strain gauge factor, fiber–matrix interface adhesion and fatigue behavior were characterized. As a result, FBG strain patches with linear temperature and strain behavior, as well as excellent fatigue resistance, were developed and can be used as part of a monitoring system for advanced composite materials in aerospace structures or wind turbine power plants. KW - Fiber Bragg grating KW - Patch KW - Strain gauge factor KW - Temperature sensitivity KW - Push-out test KW - Validation KW - Fatigue behavior PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-276271 DO - https://doi.org/10.3390/app3010039 SN - 2076-3417 VL - 3 IS - 1 SP - 39 EP - 54 PB - MDPI CY - Basel AN - OPUS4-27627 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weller, Michael G. T1 - A unifying review of bioassay-guided fractionation, effect-directed analysis and related techniques JF - Sensors N2 - The success of modern methods in analytical chemistry sometimes obscures the problem that the ever increasing amount of analytical data does not necessarily give more insight of practical relevance. As alternative approaches, toxicity- and bioactivity-based assays can deliver valuable information about biological effects of complex materials in humans, other species or even ecosystems. However, the observed effects often cannot be clearly assigned to specific chemical compounds. In these cases, the establishment of an unambiguous cause-effect relationship is not possible. Effect-directed analysis tries to interconnect instrumental analytical techniques with a biological/biochemical entity, which identifies or isolates substances of biological relevance. Successful application has been demonstrated in many fields, either as proof-of-principle studies or even for complex samples. This review discusses the different approaches, advantages and limitations and finally shows some practical examples. The broad emergence of effect-directed analytical concepts might lead to a true paradigm shift in analytical chemistry, away from ever growing lists of chemical compounds. The connection of biological effects with the identification and quantification of molecular entities leads to relevant answers to many real life questions. KW - Toxicity KW - Drug discovery KW - Natural products KW - Environmental analysis KW - Lead identification PY - 2012 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-262960 DO - https://doi.org/10.3390/s120709181 SN - 1424-8220 VL - 12 IS - 7 SP - 9181 EP - 9209 PB - MDPI CY - Basel AN - OPUS4-26296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cervino, C. A1 - Knopp, D. A1 - Weller, Michael G. A1 - Niessner, R. T1 - Novel Aflatoxin derivatives and protein conjugates JF - Molecules N2 - Aflatoxins, a group of structurally related mycotoxins, are well known for their toxic and carcinogenic effects in humans and animals. Aflatoxin derivatives and protein conjugates are needed for diverse analytical applications. This work describes a reliable and fast synthesis of novel aflatoxin derivatives, purification by preparative HPLC and characterisation by ESI-MS and one- and two-dimensional NMR. Novel aflatoxin bovine serum albumin conjugates were prepared and characterised by UV absorption and MALDI-MS. These aflatoxin protein conjugates are potentially interesting as immunogens for the generation of aflatoxin selective antibodies with novel specificities. KW - Aflatoxin KW - Mycotoxin KW - Hapten KW - Protein conjugation KW - Immunogen KW - Antigen KW - Antibody PY - 2007 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-147572 UR - http://www.mdpi.org/molecules/papers/12030641.pdf UR - http://www.mdpi.org/molecules/papers/12030641sm.pdf DO - https://doi.org/10.3390/12030641 SN - 1420-3049 VL - 12 IS - 3 SP - 641 EP - 653 PB - MDPI CY - Basel AN - OPUS4-14757 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiggenhauser, Herbert A1 - Niederleithinger, Ernst T1 - Innovative ultrasonic techniques for inspection and monitoring of large concrete structures JF - The European physical journal - Web of Conferences : proceedings N2 - Ultrasonic echo and transmission techniques are used in civil engineering on a regular basis. New sensors and data processing techniques have lead to many new applications in the structural investigation as well as quality control. But concrete structures in the nuclear sector have special features and parameters, which pose problems for the methods and instrumentation currently available, e.g. extreme thickness, dense reinforcement, steel liners or special materials. Several innovative ultrasonic techniques have been developed to deal with these issues at least partly in lab experiments and pilot studies. Modern imaging techniques as multi-offset SAFT have been used e. g. to map delaminations. Thick concrete walls have successfully been inspected, partly through a steel liner. Embedded ultrasonic sensors have been designed which will be used in monitoring networks of large concrete structures above and below ground. In addition, sensitive mathematical methods as coda wave interferometry have been successfully evaluated to detect subtle changes in material properties. Examples of measurements and data evaluation are presented. KW - Automated scanning systems KW - Multi-Offset Array KW - Enhanced Imaging KW - Embedded ultrasonic sensors PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-290513 DO - https://doi.org/10.1051/epjconf/20135604004 SN - 2100-014X VL - 56 SP - 04004-1 EP - 04004-9 PB - EDP Sciences CY - Les Ulis AN - OPUS4-29051 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Orts Gil, Guillermo A1 - Natte, Kishore A1 - Österle, Werner T1 - Multi-parametric reference nanomaterials for toxicology: state of the art, future challenges and potential candidates JF - RSC Advances N2 - A major requirement for the validation of methods assessing the risk associated with engineered nanoparticles (ENPs) is the use of reference materials (RMs). In the present contribution we review available RMs, ongoing projects and characterisation trends in the field. The conclusion is that actual approaches to RMs mostly deal with metrological considerations about single properties of the ENPs, typically their primary size, which can hardly be representative of nanoparticles characteristics in real testing media and therefore, not valid for reliable and comparable toxicological studies. As an alternative, we discussed the convenience and feasibility of establishing multi-parametric RMs for a series of ENPs, focusing on silica nanoparticles (SNPs). As a future perspective, the need to develop RMs based on hybrid nanoparticles is also discussed. KW - Referenzmaterialien KW - Nanopartikel KW - Toxikologie KW - Metrologie PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-292997 DO - https://doi.org/10.1039/c3ra42112k SN - 2046-2069 VL - 3 IS - 40 SP - 18202 EP - 18215 PB - RSC Publishing CY - London AN - OPUS4-29299 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moreira, E.V. A1 - Rabello, J.M.B. A1 - Pereira, M.d.S. A1 - Lopes, R.T. A1 - Zscherpel, Uwe T1 - Digital radiography using digital detector arrays fulfills critical applications for offshore pipelines JF - EURASIP journal on advances in signal processing N2 - Digital radiography in the inspection of welded pipes to be installed under deep water offshore gas and oil pipelines, like a presalt in Brazil, in the paper has been investigated. The aim is to use digital radiography for nondestructive testing of welds as it is already in use in the medical, aerospace, security, automotive, and petrochemical sectors. Among the current options, the DDA (Digital Detector Array) is considered as one of the best solutions to replace industrial films, as well as to increase the sensitivity to reduce the inspection cycle time. This paper shows the results of this new technique, comparing it to radiography with industrial films systems. In this paper, 20 test specimens of longitudinal welded pipe joints, specially prepared with artificial defects like cracks, lack of fusion, lack of penetration, and porosities and slag inclusions with varying dimensions and in 06 different base metal wall thicknesses, were tested and a comparison of the techniques was made. These experiments verified the purposed rules for parameter definitions and selections to control the required digital radiographic image quality as described in the draft international standard ISO/DIS 10893-7. This draft is first standard establishing the parameters for digital radiography on weld seam of welded steel pipes for pressure purposes to be used on gas and oil pipelines. KW - Zerstörungsfreie Prüfung von Schweißnähten KW - Durchstrahlungsprüfung KW - Digitale Radiologie PY - 2010 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-225319 DO - https://doi.org/10.1155/2010/894643 SN - 1687-6172 VL - 2010 IS - Article ID 894643 SP - 1 EP - 7 PB - Hindawi Publ. CY - New York, NY, USA AN - OPUS4-22531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tölle, Florian A1 - Gumenyuk, Andrey A1 - Gebhardt, Moritz Oliver A1 - Rethmeier, Michael T1 - Post-weld residual stress mitigation by scanning of a defocused laser beam JF - Physics Procedia N2 - High welding residual stresses can cause service life reducing consequences. Even though many processes have been developed to reduce these stresses, they are only applicable for wider welds and simple component geometries or are cost-intensive, respectively. The presented method uses a defocused beam after welding for heating the material regions on both sides of the weld. In this way, the welding stresses are decreased without contacting the surfaces using the available equipment. Different process parameters could be used depending on the component geometry and the laser power. The mechanism and the influence of the process parameters were investigated by FEM-simulation and experiments on S355J2+N steel and showed a stress reduction of about 73%. T2 - Lasers in Manufacturing 2011 - Proceedings of the Sixth International WLT Conference on Lasers in Manufacturing CY - Munich, Germany DA - 23.05.2011 KW - Residual stresses KW - Stress reduction KW - High energy beam welding KW - Post-weld heat treatment KW - Laser scanner optics PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-238482 DO - https://doi.org/10.1016/j.phpro.2011.03.052 SN - 1875-3892 VL - 12 IS - 1 SP - 410 EP - 418 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-23848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pelkner, Matthias A1 - Neubauer, Andreas A1 - Reimund, Verena A1 - Kreutzbruck, Marc T1 - Routes for GMR-sensor design in non-destructive testing JF - Sensors N2 - GMR sensors are widely used in many industrial segments such as information technology, automotive, automation and production, and safety applications. Each area requires an adaption of the sensor arrangement in terms of size adaption and alignment with respect to the field source involved. This paper deals with an analysis of geometric sensor parameters and the arrangement of GMR sensors providing a design roadmap for non-destructive testing (NDT) applications. For this purpose we use an analytical model simulating the magnetic flux leakage (MFL) distribution of surface breaking defects and investigate the flux leakage signal as a function of various sensor parameters. Our calculations show both the influence of sensor length and height and that when detecting the magnetic flux leakage of µm sized defects a gradiometer base line of 250 µm leads to a signal strength loss of less than 10% in comparison with a magnetometer response. To validate the simulation results we finally performed measurements with a GMR magnetometer sensor on a test plate with artificial µm-range cracks. The differences between simulation and measurement are below 6%. We report on the routes for a GMR gradiometer design as a basis for the fabrication of NDT-adapted sensor arrays. The results are also helpful for the use of GMR in other application when it comes to measure positions, lengths, angles or electrical currents. KW - Giant magneto resistance KW - Non-destructive testing KW - Magnetic flux leakage KW - Sensor array PY - 2012 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-271325 DO - https://doi.org/10.3390/s120912169 SN - 1424-8220 VL - 12 IS - 9 SP - 12169 EP - 12183 PB - MDPI CY - Basel AN - OPUS4-27132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lopez-Heredia, M.A. A1 - Gildenhaar, Renate A1 - Berger, Georg A1 - Linow, Ulf A1 - Wirth, Cynthia A1 - Günster, Jens A1 - Houshmand, A. A1 - Stiller, M. A1 - Knabe-Ducheyne, C. T1 - Effect of stressed and unstressed cell culture environments on the viability of MC3T3 cells with calcium phosphates JF - Bioceramics development and applications T2 - ISACB-6 - International symposium on apatite and correlative biomaterials CY - Nantes, France DA - 2013-06-05 KW - Cell culture media KW - Fetal bovine serum KW - Stressed KW - Unstressed KW - Calcium alkaline orthophosphates PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-299387 DO - https://doi.org/10.4172/2090-5025.S1-002 SN - 2090-5017 SN - 2090-5025 N1 - Geburtsname von Wirth, Cynthia: Gomes, C. M. - Birth name of Wirth, Cynthia: Gomes, C. M. SP - 1 EP - 3(?) PB - Ashdin AN - OPUS4-29938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hanelt, Sven A1 - Friedrich, Jörg Florian A1 - Meyer-Plath, Asmus T1 - UV spectrometric indirect analysis of brominated MWCNTs with UV active thiols and an alkene-reaction kinetics, quantification and differentiation of adsorbed bromine and oxygen JF - Materials N2 - Indirect UV-absorption spectrometry was shown to be a valuable tool for chemical characterization of functionalized carbon nanotubes (CNTs). It complements data from X-ray photoelectron spectroscopy (XPS) or FTIR analysis since it helps to clarify the type and concentration of functional groups. The principles of indirect application of UV-spectrometry and its mathematical interpretation are discussed. Their facile application, together with their adequate sensitivity and high flexibility, make UV-absorption-based approaches a valuable alternative to fluorescence spectrometry. Here, the approach was applied to the chemical analysis of oxidizing substances on CNTs. For this, pristine CNTs of low but finite oxygen content as well as brominated CNTs were analyzed by reaction in suspension with UV-active thiol reagents and a styrene derivative. It was shown that carefully selected reagents allow differentiation and quantification of bromine and generally oxidizing entities like oxygen. For brominated CNTs, it was shown that physisorbed bromine may dominate the overall bromine content. KW - Carbon nanotubes KW - CNTs KW - UV-spectrometry KW - Bromination KW - Thiols KW - Mercaptans KW - Disulfides KW - Quantification KW - Kinetics PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-289077 DO - https://doi.org/10.3390/ma6083035 SN - 1996-1944 VL - 6 IS - 8 SP - 3035 EP - 3063 PB - MDPI CY - Basel AN - OPUS4-28907 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Patrick P. A1 - Asadi, S. A1 - Hernandez Bennetts, V. A1 - Lilienthal, A.J. A1 - Bartholmai, Matthias T1 - Monitoring of CCS areas using micro unmanned aerial vehicles (MUAVs) JF - Energy procedia N2 - Carbon capture & storage (CCS) is one of the most promising technologies for greenhouse gas (GHG) management. However, an unsolved issue of CCS is the development of appropriate long-term monitoring systems for leak detection of the stored CO2. To complement already existing monitoring infrastructure for CO2 storage areas, and to increase the granularity of gas concentration measurements, a quickly deployable, mobile measurement device is needed. In this paper, we present an autonomous gas-sensitive micro-drone, which can be used to monitor GHG emissions, more specifically, CO2. Two different measurement strategies are proposed to address this task. First, the use of predefined sensing trajectories is evaluated for the task of gas distribution mapping using the micro-drone. Alternatively, we present an adaptive strategy, which suggests sampling points based on an artificial potential field (APF). The results of real-world experiments demonstrate the feasibility of using gas-sensitive micro-drones for GHG monitoring missions. Thus, we suggest a multi-layered surveillance system for CO2 storage areas. T2 - GHGT 11 - Greenhouse gas control technologies conference CY - Kyoto, Japan DA - 18.11.2012 KW - Gas-sensitive micro-drone KW - Gas distribution mapping KW - Sensor planning KW - Artificial potential field KW - CCS PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-289119 DO - https://doi.org/10.1016/j.egypro.2013.06.320 SN - 1876-6102 VL - 37 SP - 4182 EP - 4190 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-28911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Würth, Christian A1 - Grabolle, Markus A1 - Pauli, Jutta A1 - Spieles, Monika A1 - Resch-Genger, Ute T1 - Relative and absolute determination of fluorescence quantum yields of transparent samples JF - Nature protocols N2 - Luminescence techniques are among the most widely used detection methods in the life and material sciences. At the core of these methods is an ever-increasing variety of fluorescent reporters (i.e., simple dyes, fluorescent labels, probes, sensors and switches) from different fluorophore classes ranging from small organic dyes and metal ion complexes, quantum dots and upconversion nanocrystals to differently sized fluorophore-doped or fluorophore-labeled polymeric particles. A key parameter for fluorophore comparison is the fluorescence quantum yield (Φf), which is the direct measure for the efficiency of the conversion of absorbed light into emitted light. In this protocol, we describe procedures for relative and absolute determinations of Φf values of fluorophores in transparent solution using optical methods, and we address typical sources of uncertainty and fluorophore class-specific challenges. For relative determinations of Φf, the sample is analyzed using a conventional fluorescence spectrometer. For absolute determinations of Φf, a calibrated stand-alone integrating sphere setup is used. To reduce standard-related uncertainties for relative measurements, we introduce a series of eight candidate quantum yield standards for the wavelength region of ~350–950 nm, which we have assessed with commercial and custom-designed instrumentation. With these protocols and standards, uncertainties of 5–10% can be achieved within 2 h. PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-294202 DO - https://doi.org/10.1038/nprot.2013.087 SN - 1754-2189 SN - 1750-2799 VL - 8 IS - 8 SP - 1535 EP - 1550 PB - Nature Publishing Group CY - Basingstoke AN - OPUS4-29420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weller, Michael G. T1 - Immunoassays and biosensors for the detection of cyanobacterial toxins in water JF - Sensors N2 - Algal blooms are a frequent phenomenon in nearly all kinds of fresh water. Global warming and eutrophication by waste water, air pollution and fertilizers seem to lead to an increased frequency of occurrence. Many cyanobacteria produce hazardous and quite persistent toxins, which can contaminate the respective water bodies. This may limit the use of the raw water for many purposes. The purification of the contaminated water might be quite costly, which makes a continuous and large scale treatment economically unfeasible in many cases. Due to the obvious risks of algal toxins, an online or mobile detection method would be highly desirable. Several biosensor systems have been presented in the literature for this purpose. In this review, their mode of operation, performance and general suitability for the intended purpose will be described and critically discussed. Finally, an outlook on current developments and future prospects will be given. KW - Algal toxins KW - Cyanotoxins KW - Biotoxins KW - Blue-green algae KW - Harmful algal blooms KW - Microcystins KW - Nodularins KW - Anatoxin-a KW - Anatoxin-a(s) KW - Cylindrospermopsin KW - Saxitoxins PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-294728 DO - https://doi.org/10.3390/s131115085 SN - 1424-8220 VL - 13 IS - 11 SP - 15085 EP - 15112 PB - MDPI CY - Basel AN - OPUS4-29472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neuschaefer-Rube, U. A1 - Illemann, J. A1 - Sturm, M. A1 - Bircher, B. A1 - Meli, F. A1 - Bellon, Carsten A1 - Evsevleev, Sergei T1 - Validation of a fast and traceable radiographic scale calibration of dimensional computed tomography JF - Measurement Science and Technology N2 - A fast and highly precise method of determining the geometrical scale factor of computed tomography (CT) measurements has been validated successfully by Bundesanstalt für Materialforschung und -prüfung (BAM), the Federal Institute of Metrology (METAS) and Physikalisch-Technische Bundesanstalt (PTB) within the scope of AdvanCT (Advanced Computed Tomography for dimensional and surface measurements in industry), a project funded in the European Metrology Programme for Innovation and Research (EMPIR). The method has been developed by PTB and requires only two radiographic images of a calibrated thin 2D standard (hole grid standard) from two opposite directions. The mean grid distance is determined from both radiographs. From this and with the help of the calibration result, the radiographic scale and therefore the voxel size is determined. The procedure takes only a few minutes and avoids a time-consuming CT scan. To validate the method, the voxel sizes determined via this method were compared with voxel sizes determined from CT scans of calibrated objects. Relative deviations between the voxel sizes in the range of 10−5 were achieved with minimal effort using cone-beam CT systems at moderate magnifications. KW - Dimensional metrology KW - Voxel size KW - Industrial CT KW - Geometrical magnification PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553271 DO - https://doi.org/10.1088/1361-6501/ac74a3 SN - 0957-0233 VL - 33 IS - 9 SP - 1 EP - 9 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-55327 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lengas, Nikolaos A1 - Schlick-Hasper, Eva A1 - Müller, Karsten A1 - Neitsch, Marcel A1 - Johann, Sergej A1 - Zehn, M. T1 - Development of an analysis and testing concept for the evaluation of impact targets in the mechanical safety testing of dangerous goods packagings JF - Packaging technology and science N2 - The mechanical and geometrical properties of impact targets greatly influence the outcome of a drop test. The International Agreement concerning the International Carriage of Dangerous Goods by Road (ADR) as well as ISO 2248 describe the characteristics of impact targets for drop tests of dangerous goods packagings. According to these regulations, the impact target’s surface needs to be unyielding, under testing conditions non-deformable, flat, and integral with a mass at least 50 times that of the heaviest packaging to be tested. The problem is that many production facilities, especially manufacturers of corrugated fibreboard boxes, do not have their own testing device with the required 50 times mass ratio of the impact target for a regulation compliant drop test during series production. Furthermore, at UN level it is considered necessary to revise these requirements. In the present paper, the impact target requirements are examined in detail and compared with those in other technical areas (e.g., impact target for container for the transport of radioactive materials). A research method is being developed to investigate the dependency between the mass ratio of the packaging and the target as well as the damage resistance of a drop tested package in relation to specific design characteristics. The results are of high relevance for industry purposes and intended to ensure a uniform level of safety assessment for the mechanical testing of dangerous goods packagings. KW - Corrugated fibreboard boxes KW - Dangerous goods packagings KW - Drop test KW - Impact target KW - Structural dynamics PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549660 DO - https://doi.org/10.1002/pts.2656 SN - 0894-3214 SN - 1099-1522 VL - 35 IS - 9 SP - 689 EP - 700 PB - Wiley CY - New York, NY AN - OPUS4-54966 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arinchtein, A. A1 - Ye, M.-Y. A1 - Yang, Q. A1 - Kreyenschulte, C. A1 - Wagner, Andreas A1 - Frisch, M. A1 - Brückner, A. A1 - Kondratenko, E. A1 - Kraehnert, R. T1 - Dynamics of Reaction-Induced Changes of Model-Type Iron Oxide Phases in the CO2-Fischer-Tropsch-Synthesis JF - ChemCatChem N2 - Iron-based catalysts are employed in CO2-FTS due to their ability to convert CO2 into CO in a first step and their selectivity towards higher hydrocarbons in a second CO hydrogenation step. According to the literature, iron carbides represent the active phase for hydrocarbon formation and are claimed to emerge in the presence of CO. We propose nanostructured FeOx films as model systems to assess information about the complex phase transformations during CO2-FTS. Mesoporous hematite, ferrihydrite, maghemite, maghemite/magnetite films were exposed to CO2-FTS atmospheres at 20 bar and 300°C. Up to three distinct phases were observed depending on the timeon-stream (TOS): a sintered maghemite/magnetite phase, a carbidic core-shell structure, and a low-crystalline, needle-type oxide phase. Our findings indicate that the formation of an intermediary maghemite/magnetite phase, predominant after short TOS (30 h), precedes the evolution of the carbide phase. Yet, even after prolonged TOS (185 h), no full conversion into a bulk carbide is observed. KW - Nanostructured FeOx films KW - CO2 KW - Scanning Auger Spectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549709 DO - https://doi.org/10.1002/cctc.202200240 SN - 1867-3880 VL - 14 IS - 14 SP - 1 EP - 11 PB - Wiley-VCH AN - OPUS4-54970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koyutürk, B. A1 - Farber, E. A1 - Wagner, F. A1 - Fellinger, Tim-Patrick A1 - Eisenberg, D. T1 - A simple decagram-scale synthesis of an atomically dispersed, hierarchically porous Fe–N–C catalyst for acidic ORR JF - Journal of Materials Chemistry A N2 - Carbons doped with iron and nitrogen (Fe–N–Cs) are highly promising electrocatalysts for energy conversion reactions in the oxygen, nitrogen and carbon cycles. Containing no platinum group metals, they nevertheless compete with platinum-based catalysts in crucial fuel cell reactions, such as oxygen reduction in acid. Yet deployment of Fe–N–Cs in fuel cells requires also a flow-enhancing pore structure, and a scalable synthesis procedure – a rarely-met combination of requirements. We now report such a simple synthesis of over 10 g of an Fe–N–C catalyst with high activity towards oxygen reduction in acid. Atomically-dispersed Fe–N4 active sites were designed orthogonally and simultaneously with hierarchical micro-, meso- and macroporosity, by exploiting a dual role of magnesium ions during pyrolysis. Combining the “active site imprinting” and “self-templating” strategies in a single novel magnesium iminodiacetate precursor yielded a catalyst with high specific surface area (SSA > 1600 m2 g−1), a flow-enhancing hierarchical porosity, and high relative abundance of the most desirable D1-type Fe–N4 sites (43%, by Mössbauer spectroscopy at 4.2 K). Despite the relatively low iron contents, the catalysts feature halfwave potentials up to 0.70 V vs. RHE at pH 1 and a mass activity of 1.22 A g−1 at 0.8 V vs. RHE in RDE experiments. Thanks to the simple and scalable synthesis, this active and stable catalyst may serve as a workhorse in academic and industrial research into atomically-dispersed ORR electrocatalysis. KW - Catalysis KW - Fe-N-C catalysts KW - Fuel Cells KW - Electrochemistry PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550113 DO - https://doi.org/10.1039/d2ta00925k SN - 2050-7488 SP - 1 EP - 10 PB - Royal Society of Chemistry AN - OPUS4-55011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Titirici, M. A1 - Baird, S. G. A1 - Sparks, T. D. A1 - Yang, S. M. A1 - Brandt-Talbot, A. A1 - Hosseinaei, O. A1 - Harper, D. P. A1 - Parker, R. M. A1 - Vignolini, S. A1 - Berglund, L. A. A1 - Li, Y. A1 - Gao, H.-L. A1 - Mao, L.-B. A1 - Yu, S.-H. A1 - Díez, N. A1 - Ferrero, G. A. A1 - Sevilla, M. A1 - Szilágyi, P. Á. A1 - Stubbs, C. J. A1 - Worch, J. C. A1 - Huang, Y. A1 - Luscombe, C. K. A1 - Lee, K.-Y. A1 - Luo, H. A1 - Platts, M. J. A1 - Tiwari, D. A1 - Kovalevskiy, D. A1 - Fermin, D. J. A1 - Au, H. A1 - Alptekin, H. A1 - Crespo-Ribadeneyra, M. A1 - Ting, V. P. A1 - Fellinger, Tim-Patrick A1 - Barrio, J. A1 - Westhead, O. A1 - Roy, C. A1 - Stephens, I. E. L. A1 - Nicolae, S. A. A1 - Sarma, S. C. A1 - Oates, R. P. A1 - Wang, C.-G. A1 - Li, Z. A1 - Loh, X. J. A1 - Myers, R. J. A1 - Heeren, N. A1 - Grégoire, A. A1 - Périssé, C. A1 - Zhao, X. A1 - Vodovotz, Y. A1 - Earley, B. A1 - Finnveden, G. A1 - Björklund, A. A1 - Harper, G. D. J. A1 - Walton, A. A1 - Anderson, P. A. T1 - The sustainable materials roadmap JF - Journal of physics: Materials N2 - Our ability to produce and transform engineered materials over the past 150 years is responsible for our high standards of living today, especially in the developed economies. Yet, we must carefully think of the effects our addiction to creating and using materials at this fast rate will have on the future generations. The way we currently make and use materials detrimentally affects the planet Earth, creating many severe environmental problems. It affects the next generations by putting in danger the future of economy, energy, and climate. We are at the point where something must drastically change, and it must change NOW. We must create more sustainable materials alternatives using natural raw materials and inspiration from Nature while making sure not to deplete important resources, i.e. in competition with the food chain supply. We must use less materials, eliminate the use of toxic materials and create a circular materials economy where reuse and recycle are priorities. We must develop sustainable methods for materials recycling and encourage design for disassembly. We must look across the whole materials life cycle from raw resources till end of life and apply thorough life cycle assessments based on reliable and relevant data to quantify sustainability. KW - Electrochemistry KW - Fe-N-C catalysts KW - Fuel cells KW - Catalysis PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550126 DO - https://doi.org/10.1088/2515-7639/ac4ee5 SN - 2515-7639 VL - 5 IS - 3 SP - 1 EP - 98 PB - IOP Publishing CY - Bristol AN - OPUS4-55012 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Falkenhagen, Jana T1 - Combined impact of UV radiation and nitric acid on high‐density polyethylene containers as a laboratory test JF - Packaging Technology and Science N2 - In a laboratory test, transparent high‐density polyethylene (HDPE) jerrycans have been exposed to both UV radiation and 55 wt‐% nitric acid solution at (41 ± 2)°C, for up to 20 days. For comparison, UV radiant exposure (21 days) and nitric acid exposure (up to 6 weeks) were performed separately, at nearly equal temperatures. The damages are compared with FTIR spectroscopy in ATR and HT‐gel permeation chromatography(GPC) on a molecular level and with hydraulic internal pressure testing as a component test. For the used jerrycans, relevant oxidation can only be found after the combined exposure. This is caused by the decomposition of nitric acid into nitrous gases by UV radiation, which is also observed at lower concentrations (28 wt‐%). After 6 days of laboratory exposure, this is rated as critical, which corresponds to about 1/10 year in Central Europe, according to the UV radiant exposure. The gradual increase in oxidative damage shows the reproducibility of the test. KW - Molecular mass distribution KW - High-density polyethylene KW - Nitric acid KW - UV radiation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550141 DO - https://doi.org/10.1002/pts.2673 SN - 0894-3214 SP - 1 EP - 7 PB - John Wiley & Sons Ltd AN - OPUS4-55014 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Belenguer, A. A1 - Lampronti, G. A1 - Michalchuk, Adam A1 - Emmerling, Franziska A1 - Sanders, J. T1 - Quantitative reversible one pot interconversion of three crystalline polymorphs by ball mill grinding JF - Crystengcomm N2 - We demonstrate here using a disulfide system the first example of reversible, selective, and quantitative transformation between three crystalline polymorphs by ball mill grinding. This includes the discovery of a previously unknown polymorph. Each polymorph is reproducibly obtained under well-defined neat or liquid-assisted grinding conditions, revealing subtle control over the apparent thermodynamic stability. We discovered that the presence of a contaminant as low as 1.5% mol mol−1 acting as a template is required to enable all these three polymorph transformations. The relative stabilities of the polymorphs are determined by the sizes of the nanocrystals produced under different conditions and by surface interactions with small amounts of added solvent. For the first time, we show evidence that each of the three polymorphs is obtained with a unique and reproducible crystalline size. This mechanochemical approach gives access to bulk quantities of metastable polymorphs that are inaccessible through recrystallisation. KW - Mechanochemistry KW - Polymorph KW - XRD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549934 DO - https://doi.org/10.1039/D2CE00393G SP - 1 EP - 7 PB - Royal Society of Chemistry AN - OPUS4-54993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Silbernagl, Dorothee A1 - Sturm, Heinz A1 - Plajer, A. J. T1 - Thioanhydride/isothiocyanate/epoxide ring-opening terpolymerisation: sequence selective enchainment of monomer mixtures and switchable catalysis JF - Polymer Chemistry N2 - We report a new sequence selective terpolymerisation in which three monomers (butylene oxide (BO) A, PhNCS B and phtalic thioanhydride (PTA) C) are selectively enchained into an (ABA′C)n sequence. PTA/PhNCS/BO ring-opening terpolymerisation ROTERP can be coupled with CS2 ROTERP to generate tetrapolymers and with εDL ROP in switchable catalysis for blockpolymer synthesis. KW - Blockcopolymer KW - 1H-NMR KW - TGA KW - DSC KW - AFM PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552339 DO - https://doi.org/10.1039/d2py00629d SP - 1 EP - 5 PB - Royal Society of Chemistry CY - Cambridge, UK AN - OPUS4-55233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gupta, P. A1 - Karnaushenko, D. D. A1 - Becker, C. A1 - Okur, I. E. A1 - Melzer, M. A1 - Özer, B. A1 - Schmidt, O. G. A1 - Karnaushenko, D. T1 - Large Scale Exchange Coupled Metallic Multilayers by Roll-to-Roll (R2R) Process for Advanced Printed Magnetoelectronics JF - Advanced Materials Technologies N2 - Till now application of printed magnetoelectronics is hindered by lack of large area exchange coupled metallic multilayers required to produce printable magneto-sensory inks. Large-scale roll-to-roll (R2R) fabrication process is an attractive approach owing to its capabilities for high volume, high throughput, and large area manufacturing. Precise and high performance R2R sputtering technology is developed to fabricate large area giant magnetoresistive (GMR) thin-films stacks that contain 30 metallic bilayers prepared by continuous R2R sputtering of Co and Cu sequential on a hundred meters long polyethylene terephthalate (PET) web. The R2R sputtered Co/Cu multilayer on a 0.2 × 100 m2 PET web exhibits a GMR ratio of ≈40% achieving the largest area exchange coupled room temperature magneto-sensitive system demonstrated to date. The prepared GMR thin-film is converted to magnetosensitive ink that enables printing of magnetic sensors with high performance in a cost-efficient way, which promotes integration with printed electronics. An average GMR ratio of ≈18% is obtained for 370 printed magnetic sensors. The realized precise R2R sputtering approach can also be extended to a wide range of hybrid thin-film material systems opening up a path for new functional inks applied with printing technologies. KW - Printed Electronics KW - Flexible Magnetic Sensors KW - Roll-to-Roll Processing KW - Functional Materials KW - Upscaling PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552344 DO - https://doi.org/10.1002/admt.202200190 SN - 2365-709X SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim, Deutschland AN - OPUS4-55234 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fernádez-Canteli, A. A1 - Castillo, E. A1 - Blasón, Sergio T1 - A methodology for phenomenological analysis of cumulative damage processes. Application to fatigue and fracture phenomena JF - International Journal of Fatigue N2 - Sample functions, i.e., stochastic process realizations, are used to define cumulative damage phenomena which end into an observable terminal state or failure. The complexity inherent to such phenomena justifies the use of phenomenological models associated with the evolution of a physical magnitude feasible to be monitored during the test. Sample functions representing the damage evolution may be identified, once normalized to the interval [0,1], with cumulative distribution functions (cdfs), generally, of the generalized extreme value (GEV) family. Though usually only a fraction of the whole damage evolution, according to the specific problem handled, is available from the test record, the phenomenological models proposed allow the whole damage process to be recovered. In this way, down- and upwards extrapolations of the whole damage process beyond the scope of the experimental program are provided as a fundamental tool for failure prediction in the practical design. The proposed methodology is detailed and its utility and generality confirmed by its successive application to representative well-known problems in fatigue and fracture characterization. The excellent fittings, the physical interpretation of the model parameters and the good expectations to achieve a complete probabilistic analysis of these phenomena justify the interest of the proposed phenomenological approach with possible applications to other cumulative damage processes. KW - Bayesian technique KW - Sample random results KW - Stochastic sample functions KW - Probabilistic assessment PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552371 DO - https://doi.org/10.1016/j.ijfatigue.2021.106311 SN - 0142-1123 VL - 150 SP - 106311 PB - Elsevier Ltd. AN - OPUS4-55237 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Margreiter, R. A1 - Baumann, J. A1 - Mantouvalou, I. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Strub, E. T1 - Investigations on fire-gilding JF - Archaeometry N2 - Fire-gilding is a historic technique for the application of golden layers on a number of different base materials utilizing a gold amalgam. This technique leaves a significant amount of Hg in the golden layer, giving archeometrists a reliable indicator to identify firegildings. Recent findings on presumably fire-gilded objects have shown in several cases significantly lower Hg content than previously studied objects. This prompted a synchrotron-based X-ray fluorescence investigation into the Hg distribution along the material–gilding interface, as well as a series of measurements regarding the Hg content development in fire-gilded samples during artificial aging. This work presents findings on laboratory-prepared fire-gildings, indicating an Hg enrichment at the interface of firegilded silver samples. Notably, such an enrichment is missing in fire-gilded copper samples. Further, it is confirmed that fire-gilded layers typically do not undercut an Hg bulk content of 5%. In this light, it seems improbable that ancient samples that contain <5% Hg are fire-gilded. The results presented in this study might lead to a non-destructive method to identify the Hg enrichment at the interface. This might be obtained by a combination of different non-destructive measurements and might also work unambiguously in samples in which the gold top layer is altered. KW - BAMline KW - X-Ray Fluorescence KW - Gilding KW - Depth profile KW - Archaeometry PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552885 DO - https://doi.org/10.1111/arcm.12797 SN - 0003-813X SP - 1 EP - 14 PB - Wiley online library AN - OPUS4-55288 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 JF - Journal of applied crystallography 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 - Üstündag, Ömer A1 - Bakir, Nasim A1 - Gook, S. A1 - Gumenyuk, Andrey A1 - Rethmeier, Michael T1 - Hybrid laser‑arc welding of laser‑ and plasma‑cut 20‑mm‑thick structural steels JF - Welding in the World 2022 N2 - It is already known that the laser beam welding (LBW) or hybrid laser-arc welding (HLAW) processes are sensitive to manufacturing tolerances such as gaps and misalignment of the edges, especially at welding of thick-walled steels due to its narrow beam diameter. Therefore, the joining parts preferably have to be milled. The study deals with the influence of the edge quality, the gap and the misalignment of edges on the weld seam quality of hybrid laser-arc welded 20-mm-thick structural steel plates which were prepared by laser and plasma cutting. Single-pass welds were conducted in butt joint configuration. An AC magnet was used as a contactless backing. It was positioned under the workpiece during the welding process to prevent sagging. The profile of the edges and the gap between the workpieces were measured before welding by a profile scanner or a digital camera, respectively. With a laser beam power of just 13.7 kW, the single-pass welds could be performed. A gap bridgeability up to 1 mm at laser-cut and 2 mm at plasma-cut samples could be reached respectively. Furthermore, a misalignment of the edges up to 2 mm could be welded in a single pass. The new findings may eliminate the need for cost and time-consuming preparation of the edges. KW - Hybrid laser-arc welding KW - Thick-walled steel KW - Edge quality KW - Gap bridgeability KW - Laser cutting KW - Plasma cutting PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552013 DO - https://doi.org/10.1007/s40194-022-01255-y SN - 0043-2288 VL - 66 SP - 507 EP - 514 PB - Springer AN - OPUS4-55201 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Clark, P.C.J A1 - Andresen, Elina A1 - Sear, M. J. A1 - Favaro, M. A1 - Girardi, L. A1 - van de Krol, R. A1 - Resch-Genger, Ute A1 - Starr, D.E. T1 - Quantification of the Activator and Sensitizer Ion Distributions in NaYF4:Yb3+, Er3+ Upconverting Nanoparticles Via Depth-Profiling with Tender X-Ray Photoemission JF - Small N2 - The spatial distribution and concentration of lanthanide activator and sensitizer dopant ions are of key importance for the luminescence color and efficiency of upconverting nanoparticles (UCNPs). Quantifying dopant ion distributions and intermixing, and correlating them with synthesis methods require suitable analytical techniques. Here, X-ray photoelectron spectroscopy depth-profiling with tender X-rays (2000–6000 eV), providing probe depths ideally matched to UCNP sizes, is used to measure the depth-dependent concentration ratios of Er3+ to Yb3+, [Er3+]/[Yb3+], in three types of UCNPs prepared using different reagents and synthesis methods. This is combined with data simulations and inductively coupled plasma-optical emission spectroscopy (ICP-OES) measurements of the lanthanide ion concentrations to construct models of the UCNPs’ dopant ion distributions. The UCNP sizes and architectures are chosen to demonstrate the potential of this approach. Core-only UCNPs synthesized with XCl3·6H2O precursors (β-phase) exhibit a homogeneous distribution of lanthanide ions, but a slightly surface-enhanced [Er3+]/[Yb3+] is observed for UCNPs prepared with trifluroacetate precursors (α-phase). Examination of Yb-core@Er-shell UCNPs reveals a co-doped, intermixed region between the single-doped core and shell. The impact of these different dopant ion distributions on the UCNP's optical properties is discussed to highlight their importance for UCNP functionality and the design of efficient UCNPs. KW - Shell KW - Nanomaterial KW - Nano KW - Upconversion nanoparticle KW - Lanthanide KW - Photoluminescence KW - Quantum yield KW - Photophysics KW - Excitation power density KW - Surface KW - Coating KW - Core-shell KW - XPS KW - Intermixing KW - HAXPES KW - Method PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552075 DO - https://doi.org/10.1002/smll.202107976 SN - 1613-6813 SP - 1 EP - 13 PB - Wiley-VCH-Verlag CY - Weinheim, Germany AN - OPUS4-55207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schönherr, J. A. A1 - Duarte, Larissa A1 - Madia, Mauro A1 - Zerbst, Uwe A1 - Geilen, M. B. A1 - Klein, M. A1 - Oechsner, M. T1 - Robust determination of fatigue crack propagation thresholds from crack growth data JF - Materials N2 - The robust determination of the threshold against fatigue crack propagation DKth is of paramount importance in fracture mechanics based fatigue assessment procedures. The standards ASTM E647 and ISO 12108 introduce operational definitions of DKth based on the crack propagation rate da/dN and suggest linear fits of logarithmic DK– da/dN test data to calculate DKth. Since these fits typically suffer from a poor representation of the actual curvature of the crack propagation curve, a method for evaluating DKth using a nonlinear function is proposed. It is shown that the proposed method reduces the artificial conservativeness induced by the evaluation method as well as the susceptibility to scatter in test data and the influence of test data density. KW - Fatigue crack propagation threshold KW - ISO 12108 KW - ASTM E647 KW - Data evaluation methods KW - Experimental determination PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552153 DO - https://doi.org/10.3390/ma15144737 SN - 1996-1944 VL - 15 IS - 14 SP - 1 EP - 21 PB - MDPI CY - Basel AN - OPUS4-55215 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sternbaek, L. A1 - Kimani, Martha Wamaitha A1 - Gawlitza, Kornelia A1 - Rurack, Knut A1 - Janicke, B. A1 - Alm, K. A1 - Gjörloff-Wingren, A. A1 - Eriksson, H. T1 - Molecularly Imprinted Polymers Exhibit Low Cytotoxic and Inflammatory Properties in Macrophages In Vitro JF - Applied Sciences N2 - Molecularly imprinted polymers (MIPs) against sialic acid (SA) have been developed as a detection tool to target cancer cells. Before proceeding to in vivo studies, a better knowledge of the overall effects of MIPs on the innate immune system is needed. The aim of this study thus was to exemplarily assess whether SA-MIPs lead to inflammatory and/or cytotoxic responses when administered to phagocytosing cells in the innate immune system. The response of monocytic/macrophage cell lines to two different reference particles, Alhydrogel and PLGA, was compared to their response to SA-MIPs. In vitro culture showed a cellular association of SA-MIPs and Alhydrogel, as analyzed by flow cytometry. The reference particle Alhydrogel induced secretion of IL-1b from the monocytic cell line THP-1, whereas almost no secretion was provoked for SA-MIPs. A reduced number of both THP-1 and RAW 264.7 cells were observed after incubation with SA-MIPs and this was not caused by cytotoxicity. Digital holographic cytometry showed that SA-MIP treatment affected cell division, with much fewer cells dividing. Thus, the reduced number of cells after SA-MIP treatment was not linked to SA-MIPs cytotoxicity. In conclusion, SA-MIPs have a low degree of inflammatory properties, are not cytotoxic, and can be applicable for future in vivo studies. KW - Molecularly imprinted polymers KW - Digital holographic cytometry KW - Cytotoxicity KW - Proinflammatory cytokines PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552250 DO - https://doi.org/10.3390/app12126091 SN - 2076-3417 VL - 12 IS - 12 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-55225 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Blaeß, Carsten A1 - Müller, Ralf T1 - Sintering and foaming of bioactive glasses JF - Journal of American Ceramic Society N2 - Sintering, crystallization, and foaming of 44.8SiO2–2.5P2O3–36.5CaO–6.6Na2O–6.6K2O–3.0CaF2 (F3) and 54.6SiO2–1.7P2O3–22.1CaO–6.0Na2O–7.9K2O–7.7MgO (13–93) bioactive glass powders milled in isopropanol and CO2 were studied via heating microscopy, differential thermal analysis, vacuum hot extraction (VHE), Infrared spectroscopy, and time-of-flight secondary ion mass spectrometry. Full densification was reached in any case and followed by significant foaming. VHE studies show that foaming is driven by carbon gases and carbonates were detected by Infrared spectroscopy to provide the major foaming source. Carbonates could be detected even after heating to 750◦C, which hints on a thermally very stable species or mechanical trapping. Otherwise, dark gray compact colors for milling in isopropanol indicate the presence of residual carbon as well. Its significant contribution to foaming, however, could not be proved and might be limited by the diffusivity of oxygen needed for carbon oxidation to carbon gas. KW - Bioactive Glass KW - Crystallization KW - Foaming KW - Sintering PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552454 DO - https://doi.org/10.1111/jace.18626 SN - 0002-7820 SP - 1 EP - 11 PB - Wiley online library AN - OPUS4-55245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fritsch, Tobias A1 - Kurpiers, J. A1 - Roland, S. A1 - Tokmoldin, N. A1 - Shoaee, S. A1 - Ferron, T. A1 - Collins, B. A. A1 - Janietz, S. A1 - Vandewal, K. A1 - Fritsch, D. T1 - On the Interplay between CT and Singlet Exciton Emission in Organic Solar Cells with Small Driving Force and Its Impact on Voltage Loss JF - Advanced Energy Materials N2 - The interplay between free charge carriers, charge transfer (CT) states and singlet excitons (S1) determines the recombination pathway and the resulting open circuit voltage (VOC) of organic solar cells. By combining a well-aggregated low bandgap polymer with different blend ratios of the fullerenes PCBM and ICBA, the energy of the CT state (ECT) is varied by 130 meV while leaving the S1 energy of the polymer (ES1) unaffected. It is found that the polymer exciton dominates the radiative properties of the blend when ECT approaches ES1, while the VOC remains limited by the non-radiative decay of the CT state. It is concluded that an increasing strength of the exciton in the optical spectra of organic solar cells will generally decrease the non-radiative voltage loss because it lowers the radiative VOC limit (VOC,rad), but not because it is more emissive. The analysis further suggests that electronic coupling between the CT state and the S1 will not improve the VOC, but rather reduce the VOC,rad. It is anticipated that only at very low CT state absorption combined with a fairly high CT radiative efficiency the solar cell benefit from the radiative properties of the singlet excitons. KW - Organic Solar Cell KW - Open Circuit Voltage KW - Voltage Loss KW - Ternary PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552518 DO - https://doi.org/10.1002/aenm.202200641 SN - 1614-6832 SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-55251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tengattini, A A1 - Kardjilov, N A1 - Helfen, L A1 - Douissard, P A A1 - Lenoir, N A1 - Markötter, Henning A1 - Hilger, A A1 - Arlt, T A1 - Paulisch, M A1 - Turek, T A1 - Manke, Ingo T1 - Compact and versatile neutron imaging detector with sub-4μm spatial resolution based on a single-crystal thin-film scintillator JF - Optics Express N2 - A large and increasing number of scientific domains pushes for high neutron imaging resolution achieved in reasonable times. Here we present the principle, design and performance of a detector based on infinity corrected optics combined with a crystalline Gd3Ga5O12 : Eu scintillator, which provides an isotropic sub-4 μm true resolution. The exposure times are only of a few minutes per image. This is made possible also by the uniquely intense cold neutron flux available at the imaging beamline NeXT-Grenoble. These comparatively rapid acquisitions are compatible with multiple high quality tomographic acquisitions, opening new venues for in-operando testing, as briefly exemplified here. KW - Neutron imaging KW - Scintillator KW - Resolution PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549836 DO - https://doi.org/10.1364/oe.448932 VL - 30 IS - 9 SP - 14461 EP - 14477 PB - Optica CY - Washington, DC AN - OPUS4-54983 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Franchin, G. A1 - Zocca, Andrea A1 - Karl, D. A1 - Yun, H. A1 - Tian, X. T1 - Editorial: Advances in additive manufacturing of ceramics JF - Open ceramics N2 - Recently, additive manufacturing of ceramics has achieved the maturity to be transferred from scientific laboratories to industrial applications. At the same time, research is progressing to expand the boundaries of this field into the territory of novel materials and applications. This feature issue addresses current progress in all aspects of additive manufacturing of ceramics, from parts design to feedstock selection, from technological development to characterization of printed components. KW - Additive manufacturing KW - Ceramic PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549361 DO - https://doi.org/10.1016/j.oceram.2022.100277 SN - 2666-5395 VL - 10 SP - 1 EP - 2 PB - Elsevier CY - Amsterdam AN - OPUS4-54936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weise, Frank A1 - von Werder, Julia A1 - Manninger, Tanja A1 - Maier, Bärbel A1 - Fladt, Matthias A1 - Simon, Sebastian A1 - Gardei, Andre A1 - Höhnel, Desirée A1 - Pirskawetz, Stephan A1 - Meng, Birgit T1 - A multiscale and multimethod approach to assess and mitigate concrete damage due to alkali-silica reaction JF - Advanced engineering materials N2 - Alkali-silica reaction (ASR) is a chemical reaction within concrete which can lead over time to cracking and spalling. Due to the complexity of the problem, it still causes damage to concrete constructions worldwide. The publication aims to illustrate the interdisciplinary research of the German Federal Institute for Materials Research and Testing (BAM) within the last 20 years, considering all aspects of ASR topics from the macro to the micro level. First, methods for characterization and assessment of ASR risks and reaction products used at BAM are explained and classified in the international context. Subsequently the added value of the research approach by combining different, preferably nondestructive, methods across all scales is explained using specific examples from a variety of research projects. Aspects covered range from the development of new test-setups to assess aggregate reactivity, to analysis of microstructure and reaction products using microscopical, spectroscopical and X-ray methods, to the development of a testing methodology for existing concrete pavements including in-depth analysis of the visual damage indicator and the de-icing salt input using innovative testing techniques. Finally, research regarding a novel avoidance strategy that makes use of internal hydrophobization of the concrete mix is presented. KW - Mitigation strategies KW - Concrete KW - Damage analysis KW - Alkali silica reaction KW - Road pavement KW - Accelerated testing KW - Non-destructive testing KW - Microstructure PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:101:1-2022052515100075090235 DO - https://doi.org/10.1002/adem.202101346 SN - 1527-2648 VL - 24 IS - 6 SP - 1 EP - 36 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54951 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Harald A1 - Hodoroaba, Vasile-Dan A1 - Schmidt, Alexandra A1 - Rasmussen, K. A1 - Rauscher, H. T1 - Counting Small Particles in Electron Microscopy Images — Proposal for Rules and Their Application in Practice JF - Nanomaterials N2 - Electron microscopy (EM) is the gold standard for the characterisation of the morphology (size and shape) of nanoparticles. Visual observation of objects under examination is always a necessary first step in the characterisation process. Several questions arise when undertaking to identify and count particles to measure their size and shape distribution. In addition to challenges with the dispersion and identification of the particles, more than one protocol for counting particles is in use. This paper focuses on precise rules for the counting of particles in EM micrographs, as this influences the measurement accuracy of the number of particles, thus implicitly affecting the size values of the counted particles. We review and compare four different, commonly used methods for counting, which we then apply in case studies. The impact of the selected counting rule on the obtained final particle size distribution is highlighted. One main aim of this analysis is to support the application of a specific, well-defined counting approach in accordance with regulatory requirements to contribute to achieving more reliable and reproducible results. It is also useful for the new harmonised measurement procedures for determining the particle size and particle size distribution of nanomaterials. KW - Nano KW - Particle size distribution KW - Nanoparticle KW - Nanomaterial KW - OECD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551891 DO - https://doi.org/10.3390/nano12132238 SN - 2079-4991 VL - 12 IS - 13 SP - 2238 PB - MDPI CY - Basel AN - OPUS4-55189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kittner, Maria A1 - Kerndorff, A. A1 - Ricking, M. A1 - Bednarz, M. A1 - Obermaier, N. A1 - Lukas, M. A1 - Asenova, M. A1 - Bordós, G. A1 - Eisentraut, Paul A1 - Hohenblum, P. A1 - Hudcova, H. A1 - Humer, F. A1 - István, T. G. A1 - Kirchner, M. A1 - Marushevska, O. A1 - Nemejcová, D. A1 - Oswald, P. A1 - Paunovic, M. A1 - Sengl, M. A1 - Slobodnik, J. A1 - Spanowsky, K. A1 - Tudorache, M. A1 - Wagensonner, H. A1 - Liska, I. A1 - Braun, U. A1 - Bannick, C. G. T1 - Microplastics in the Danube River Basin: A First Comprehensive Screening with a Harmonized Analytical Approach JF - ACS ES&T Water N2 - In this study, carried out within the Joint Danube Survey 4, a comprehensive microplastic screening in the water column within a large European river basin from its source to estuary, including major tributaries, was realized. The objective was to develop principles of a systematic and practicable microplastic monitoring strategy using sedimentation boxes for collection of suspended particulate matter followed by its subsequent analysis using thermal extraction desorption-gas chromatography/mass spectrometry. In total, 18 sampling sites in the Danube River Basin were investigated. The obtained suspended particulate matter samples were subdivided into the fractions of >100 μm and <100 μm and subsequently analyzed for microplastic mass contents. The results showed that microplastics were detected in all samples, with polyethylene being the predominant polymer with maximum contents of 22.24 μg/mg, 3.23 μg/mg for polystyrene, 1.03 μg/mg for styrene-butadiene-rubber, and 0.45 μg/mg for polypropylene. Further, polymers such as different sorts of polyester, polyacrylates, polylactide, and natural rubber were not detected or below the detection limit. Additional investigations on possible interference of polyethylene signals by algae-derived fatty acids were assessed. In the context of targeted monitoring, repeated measurements provide more certainty in the interpretation of the results for the individual sites. Nevertheless, it can be stated that the chosen approach using an integrative sampling and determination of total plastic content proved to be successful. KW - Thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS), monitoring KW - Microplastics KW - River KW - Suspended particulate matter (SPM) KW - Sedimentation box (SB) PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551444 DO - https://doi.org/10.1021/acsestwater.1c00439 VL - 2 IS - 7 SP - 1174 EP - 1181 PB - ACS Publications AN - OPUS4-55144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Segovia, J. J. A1 - Tuma, Dirk A1 - Lozano-Martín, D. A1 - Moreau, A. A1 - Martín, M. C. A1 - Vega-Maza, D. T1 - Speed of sound data and acoustic virial coefficients of two binary (N2 + H2) mixtures at temperatures between (260 and 350) K and at pressures between (0.5 and 20) MPa JF - Journal of Chemical Thermodynamics N2 - This work aims to address the technical concerns related to the thermodynamic characterization of gas mixtures blended with hydrogen for the implementation of hydrogen as a new energy vector. For this purpose, new experimental speed of sound measurements have been done in gaseous and supercritical phases of two binary mixtures of nitrogen and hydrogen using the most accurate technique available, i.e., the spherical acoustic resonator, yielding an experimental expanded (k = 2) uncertainty of only 220 parts in 106 (0.022%). The measurements cover the pressure range between (0.5 and 20) MPa, the temperature range between (260 and 350) K, and the composition range with a nominal mole percentage of hydrogen of (5 and 10) mol%, respectively. From the speed of sound data sets, thermophysical properties that are relevant for the characterization of the mixture, namely the second βa and third γa acoustic virial coefficients, are derived. These results are thoroughly compared and discussed with the established reference mixture models valid for mixtures of nitrogen and hydrogen, such as the AGA8-DC92 EoS, the GERG-2008 EoS, and the recently developed adaptation of the GERG-2008 EoS, here denoted GERG-H2_improved EoS. Special attention has been given to the effect of hydrogen concentration on those properties, showing that only the GERG-H2_improved EoS is consistent with the data sets within the experimental uncertainty in most measuring conditions. KW - Speed of sound KW - Acoustic resonance KW - Binary gas mixture PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551482 DO - https://doi.org/10.1016/j.jct.2022.106791 SN - 0021-9614 VL - 171 SP - 1 EP - 13 PB - Elsevier B. V. CY - Amsterdam AN - OPUS4-55148 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogler, Nico A1 - Lehmann, Jens A1 - Bohlmann, Tatjana A1 - Kronemann, Jens T1 - Gel-bound Colourants as a Substitute for the Sprayed Application of pH-Indicator Solution JF - American Journal of Civil Engineering N2 - In general, pH-sensitive colorants such as phenolphthalein are applied on freshly split surfaces of building structures to determine the state of carbonation. For years, it has been known that the aerosols of phenolphthalein are suspected of being carcinogenic. Hence, more work has currently being done on alternative indicators for the use in research and the use on construction sites. Over the past years, mainly pH indicators from other research areas and natural dyes were investigated for their usability to cementitious systems. This paper presents the experimental results of using phenolphthalein solution bound in agar-agar gel. This gel-bound indicator allows the future use of the already known phenolphthalein dye without the health hazards for the user. To demonstrate the flexibility of the gel-bound colorant, different application forms of the indicator were carried out and assessed. In addition, the results obtained by the different methods were statistically evaluated to ensure validity. The accuracy of the results was confirmed by thermogravimetric analysis and IR spectroscopic studies as reference methods. It has also succeeded to demonstrate the comparability of the results achieved by the gel-bound colorant with the results of the common sprayed application method. As an additional gain in knowledge, comparative results of indicator tests, TGA analysis, and FTIR investigation are shown. KW - Concrete Carbonation KW - Gel-bound Colorants KW - pH Indicator KW - Thermal Gravimetric Analysis KW - FTIR-ATR Measurements PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551493 UR - http://www.sciencepublishinggroup.com/j/ajce DO - https://doi.org/10.11648/j.ajce.20221003.16 SN - 2330-8729 SN - 2330-8737 VL - 10 IS - 3 SP - 135 EP - 144 PB - Science Publishing Group CY - New York, NY AN - OPUS4-55149 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hurtado-Hurtado, G. A1 - Morales-Velazquez, L. A1 - Valtierra-Rodríguez, M. A1 - Otremba, Frank A1 - Jáuregui-Correa, J. C. T1 - Frequency Analysis of the Railway Track under Loads Caused by the Hunting Phenomenon JF - Mathematics N2 - Hunting is a potentially dangerous phenomenon related to the lateral oscillation of the wheels that impacts the rails and causes the wear of the infrastructure’s components. Therefore, the analysis and timely detection of hunting can lead to the application of corrective maintenance tasks, reducing damages, and costs and even derailments as a result. In this work, the vibration response of a finite element model of a rail with hunting-induced loads by a single wheel is analyzed in three directions: longitudinal, lateral, and vertical. The contact patch forces are calculated by means of Simpack® using the Kalker linear theory and the contact Hertz theory. The system is solved by using the Newmark-_ approach. The results of the deflection and vibration analysis, following the proposed methodology, show how the different characteristics of the loads impact the rail. KW - Continuous wavelet transform KW - Empirical mode decomposition KW - Finite element method KW - Frequency analysis KW - Hunting phenomenon KW - Mechanical modelling KW - Rail vibrations PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551517 UR - https://www.mdpi.com/2227-7390/10/13/2286/htm# DO - https://doi.org/10.3390/math10132286 VL - 10 IS - 13 SP - 1 EP - 17 PB - MDPI AN - OPUS4-55151 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Würth, Christian A1 - Grauel, Bettina A1 - Pons, Monika A1 - Frenzel, Florian A1 - Rissiek, P. A1 - Rücker, Kerstin A1 - Haase, Markus A1 - Resch-Genger, Ute T1 - Yb- and Er concentration dependence of the upconversion luminescence of highly doped NaYF4:Yb,Er/NaYF4:Lu core/shell nanocrystals prepared by a water-free synthesis JF - Nano Research N2 - High sensitizer and activator concentrations have been increasingly examined to improve the performance of multi-color emissive upconversion (UC) nanocrystals (UCNC) like NaYF4:Yb,Er and first strategies were reported to reduce concentration quenching in highly doped UCNC. UC luminescence (UCL) is, however, controlled not only by dopant concentration, yet by an interplay of different parameters including size, crystal and shell quality, and excitation power density (P). Thus, identifying optimum dopant concentrations requires systematic studies of UCNC designed to minimize additional quenching pathways and quantitative spectroscopy. Here, we quantify the dopant concentration dependence of the UCL quantum yield (ΦUC) of solid NaYF4:Yb,Er/NaYF4:Lu upconversion core/shell nanocrystals of varying Yb3+ and Er3+ concentrations (Yb3+ series: 20%‒98% Yb3+; 2% Er3+; Er3+ series: 60% Yb3+; 2%‒40% Er3+). To circumvent other luminescence quenching processes, an elaborate synthesis yielding OH-free UCNC with record ΦUC of ~9% and ~25 nm core particles with a thick surface shell were used. High Yb3+ concentrations barely reduce ΦUC from ~9% (20% Yb3+) to ~7% (98% Yb3+) for an Er3+ concentration of 2%, thereby allowing to strongly increase the particle absorption cross section and UCNC brightness. Although an increased Er3+ concentration reduces ΦUC from ~7% (2% Er3+) to 1% (40%) for 60% Yb3+. Nevertheless, at very high P (> 1 MW/cm2) used for microscopic studies, highly Er3+-doped UCNC display a high brightness because of reduced saturation. These findings underline the importance of synthesis control and will pave the road to many fundamental studies of UC materials. KW - Upconverion KW - Nanoparticle KW - Lanthanides KW - Quantum yield PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551346 DO - https://doi.org/10.1007/s12274-022-4570-5 SP - 1 EP - 8 PB - Springer AN - OPUS4-55134 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - George, Janine A1 - Petretto, G. A1 - Naik, Aakash Ashok A1 - Esters, M. A1 - Jackson, A. J. A1 - Nelson, R. A1 - Dronskowski, R. A1 - Rignanese, G.-M. A1 - Hautier, G. T1 - Automated bonding analysis with crystal orbital Hamilton populuations JF - ChemPlusChem N2 - Automated bonding analysis software has been developed based on Crystal Orbital Hamilton Populations to facilitate high-throughput bonding analysis and machine-learning of bonding features. This work presents the software and discusses its applications to simple and complex materials such as GaN, NaCl, the oxynitrides XTaO2N (X=Ca, Ba, Sr) and Yb14Mn1Sb11. KW - Chemical bonds KW - Automation KW - High-throughput PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551641 DO - https://doi.org/10.1002/cplu.202200123 SN - 2192-6506 SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-55164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hesse, R. A1 - Denecke, R. A1 - Radnik, Jörg T1 - Testing and validating the improved estimation of the spectrometer-transmission function with UNIFIT 2022 JF - Surface and Interface Analysis N2 - Recent developments of X-ray photoelectron spectroscopy using excitation energies different from the usual lab-sources Mg Kα and Al Kα, thus covering larger and different kinetic energy ranges, require more flexible approaches for determining the transmission function than the well-established ones using reference spectra. Therefore, the approach using quantified peak areas (QPA) was refined allowing a more precise estimation of the transmission function. This refinement was tested by comparing the results obtained with the new version with former calculations. Furthermore, the obtained transmission function was validated by comparing the results with a transmission function using the reference spectrum of polyethylene. Additionally, an ionic liquid was used as reference for estimating the transmission function at the energy resolved HE-SGM beamline at BESSY II. Comparison between the measured and stoichiometric composition shows that a transmission function was determined, which allows a reasonable quantification. KW - XPS KW - Quantification KW - Software UNIFIT 2022 KW - Synchrotron radiation KW - Transmission function IERF PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551671 DO - https://doi.org/10.1002/sia.7131 SN - 0142-2421 SP - 1 EP - 7 PB - Wiley-VCH AN - OPUS4-55167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sachse, René A1 - Hodoroaba, Vasile-Dan A1 - Kraehnert, R. A1 - Hertwig, Andreas T1 - Multilevel effective material approximation for modeling ellipsometric measurements on complex porous thin films JF - Advanced optical technologies N2 - Catalysts are important components in chemical processes because they lower the activation energy and thus determine the rate, efficiency and selectivity of a chemical reaction. This property plays an important role in many of today’s processes, including the electrochemical splitting of water. Due to the continuous development of catalyst materials, they are becoming more complex, which makes a reliable evaluation of physicochemical properties challenging even for modern analytical measurement techniques and industrial manufacturing. We present a fast, vacuum-free and non-destructive analytical approach using multi-sample spectroscopic ellipsometry to determine relevant material parameters such as film thickness, porosity and composition of mesoporous IrOx–TiOy films. Mesoporous IrOx–TiOy films were deposited on Si wafers by sol–gel synthesis, varying the composition of the mixed oxide films between 0 and 100 wt%Ir. The ellipsometric modeling is based on an anisotropic Bruggeman effective medium approximation (a-BEMA) to determine the film thickness and volume fraction of the material and pores. The volume fraction of the material was again modeled using a Bruggeman EMA to determine the chemical composition of the materials. The ellipsometric fitting results were compared with complementary methods, such as scanning electron microscopy (SEM), electron probe microanalysis (EPMA) as well as environmental ellipsometric porosimetry (EEP). KW - Electrochemical catalysts KW - Mixed metal oxide KW - Multi-sample analysis KW - Spectroscopic ellipsometry KW - Thin mesoporous films PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551026 DO - https://doi.org/10.1515/aot-2022-0007 SN - 2192-8584 SN - 2192-8576 VL - 11 IS - 3-4 (Topical issue: Ellipsometry) SP - 137 EP - 147 PB - De Gruyter CY - Berlin AN - OPUS4-55102 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Das, Chayanika A1 - Kastania, Eleni A1 - Witt, Julia A1 - Özcan Sandikcioglu, Özlem T1 - Corrosion protection properties of poly(4-vinyl pyridine) containing multilayer polymeric coatings on magnesium alloy AZ31 JF - Materials and Corrosion N2 - The aim of this study is to develop polymeric thin films for corrosion protection of magnesium alloy AZ31. As polymer matrix, poly(4-vinyl pyridine) (P4VP) is selected due to its semiconducting properties and protonic conductivity. Polyacrylic acid is tested as crosslinking layers to improve interfacial adhesion. The macroscopic corrosion properties of the multilayer coatings are investigated by means of electrochemical methods, such as linear sweep voltammetry and electrochemical impedance spectroscopy (EIS), in corrosive media simulating technical and biomedical applications. It is demonstrated that thin multilayer coatings can suppress the corrosion rates of magnesium alloys. To our best knowledge, this is the first demonstration of the use of P4VP as a conducting polymer film with protonic conductivity for corrosion protection of magnesium alloys. KW - Multilayercoatings KW - AZ31 KW - Corrosion protection KW - Intrinsically conducting polymers KW - Magnesium alloys PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551799 DO - https://doi.org/10.1002/maco.202112708 SN - 0947-5117 VL - 73 IS - 3 SP - 427 EP - 435 PB - Wiley VHC-Verlag AN - OPUS4-55179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholtz, Lena A1 - Eckert, J. G. A1 - Elahi, T. A1 - Lübkemann, F. A1 - Hübner, Oskar A1 - Bigall, N. C. A1 - Resch-Genger, Ute T1 - Luminescence encoding of polymer microbeads with organic dyes and semiconductor quantum dots during polymerization JF - Scientific reports N2 - Luminescence-encoded microbeads are important tools for many applications in the life and material sciences that utilize luminescence detection as well as multiplexing and barcoding strategies. The preparation of such beads often involves the staining of premanufactured beads with molecular luminophores using simple swelling procedures or surface functionalization with layer-by-layer (LbL) techniques. Alternatively, these luminophores are sterically incorporated during the polymerization reaction yielding the polymer beads. The favorable optical properties of semiconductor quantum dots (QDs), which present broadly excitable, size-tunable, narrow emission bands and low photobleaching sensitivity, triggered the preparation of beads stained with QDs. However, the colloidal nature and the surface chemistry of these QDs, which largely controls their luminescence properties, introduce new challenges to bead encoding that have been barely systematically assessed. To establish a straightforward approach for the bead encoding with QDs with minimized loss in luminescence, we systematically assessed the incorporation of oleic acid/oleylamine-stabilized CdSe/CdS-core/shell-QDs into 0.5–2.5 μm-sized polystyrene (PS) microspheres by a simple dispersion polymerization synthesis that was first optimized with the organic dye Nile Red. Parameters addressed for the preparation of luminophore-encoded beads include the use of a polymer-compatible ligand such as benzyldimethyloctadecylammonium chloride (OBDAC) for the QDs, and crosslinking to prevent luminophore leakage. The physico-chemical and optical properties of the resulting beads were investigated with electron microscopy, dynamic light scattering, optical spectroscopy, and fluorescence microscopy. Particle size distribution, fluorescence quantum yield of the encapsulated QDs, and QD leaking stability were used as measures for bead quality. The derived optimized bead encoding procedure enables the reproducible preparation of bright PS microbeads encoded with organic dyes as well as with CdSe/CdS-QDs. Although these beads show a reduced photoluminescence quantum yield compared to the initially very strongly luminescent QDs, with values of about 35%, their photoluminescence quantum yield is nevertheless still moderate. KW - Polymerization KW - Quantum dots KW - Microbeads KW - Fluorescence PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553430 DO - https://doi.org/10.1038/s41598-022-16065-x SN - 2045-2322 VL - 12 SP - 1 EP - 16 PB - Nature Publishing Group CY - London AN - OPUS4-55343 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thuy, Maximilian A1 - Pedragosa-Rincon, M. A1 - Niebergall, Ute A1 - Oehler, H. A1 - Alig, I. A1 - Böhning, Martin T1 - Environmental Stress Cracking of High-Density Polyethylene Applying Linear Elastic Fracture Mechanics JF - Polymers N2 - The crack propagation rate of environmental stress cracking was studied on high-density polyethylene compact tension specimens under static loading. Selected environmental liquids are distilled water, 2 wt% aqueous Arkopal N100 solution, and two model liquid mixtures, one based on solvents and one on detergents, representing stress cracking test liquids for commercial crop protection products. The different surface tensions and solubilities, which affect the energetic facilitation of void nucleation and craze development, are studied. Crack growth in surface-active media is strongly accelerated as the solvents induce plasticization, followed by strong blunting significantly retarding both crack initiation and crack propagation. The crack propagation rate for static load as a function of the stress intensity factor within all environments is found to follow the Paris–Erdogan law. Scanning electron micrographs of the fracture surface highlight more pronounced structures with both extensive degrees of plasticization and reduced crack propagation rate, addressing the distinct creep behavior of fibrils. Additionally, the limitations of linear elastic fracture mechanisms for visco-elastic polymers exposed to environmental liquids are discussed. KW - Crack propagation KW - Environmental stress cracking KW - Fracture toughness KW - Crop protection products KW - High-density polyethylene KW - Craze–crack mechanism KW - Linear elastic fracture mechanics KW - Stress intensity factor PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550476 DO - https://doi.org/10.3390/polym14122415 SN - 2073-4360 VL - 14 IS - 12 SP - 1 EP - 21 PB - MDPI CY - Basel AN - OPUS4-55047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jiang, C. A1 - Xie, G. A1 - Wu, Dejian A1 - Yan, T. A1 - Chen, S. A1 - Zhao, P. A1 - Wu, Z. A1 - Li, W. T1 - Experimental investigation on an energy-efficient floor heating system with intelligent control: A case study in Chengdu, China JF - Case Studies in Thermal Engineering N2 - The space heating system accounts for 20%~50% of building energy consumption, and may lead to energy waste due to unreasonable controls. In this study, an energy-efficient floor heating system with intelligent control was proposed to improve energy efficiency of the system. In order to validate the concept of the proposed intelligent control, an experimental system was designed and constructed in Chengdu, China. Temperature, control cycle and energy consumption were then studied under different control strategies. The result shows that a larger flow rate of supply water will result in a longer control cycle and a lower control frequency, i.e., the average control cycle at 7 L min−1 is 1.7 h during the test day, while it is 1.5 h at 5 L min−1. Moreover, adopting water with a higher temperature and flow rate could achieve a higher efficiency of the system. The energy consumptions in case 1 (5 L min−1, 50 °C), case 2 (5 L min−1, 55 °C), case 5 (7 L min−1, 55 °C) and case 6 (7 L min−1, 60 °C) are 4746 kJ, 3534 kJ, 3093 kJ and 3028 kJ, respectively. Based on the experimental data, the supply water temperature is suggested to set lower than 60 °C considering human comfort. KW - Floor heating KW - Intelligent control KW - Experimental KW - Energy consumption KW - Control strategy PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550522 DO - https://doi.org/10.1016/j.csite.2021.101094 SN - 2214-157X VL - 26 SP - 1 EP - 14 PB - Elsevier Ltd. AN - OPUS4-55052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Accorsi, M. A1 - Tiemann, M. A1 - Wehrhan, L. A1 - Finn, Lauren M. A1 - Cruz, R. A1 - Rautenberg, Max A1 - Emmerling, Franziska A1 - Heberle, J. A1 - Keller, B. G. A1 - Rademann, J. T1 - Pentafluorophosphato-Phenylalanines: Amphiphilic Phosphotyrosine Mimetics Displaying Fluorine-Specific Protein Interactions JF - Angewandte Chemie International Edition N2 - Phosphotyrosine residues are essential functional switches in health and disease. Thus, phosphotyrosine biomimetics are crucial for the development of chemical tools and drug molecules. We report here the discovery and investigation of pentafluorophosphato amino acids as novel phosphotyrosine biomimetics. A mild acidic pentafluorination protocol was developed and two PF5-amino acids were prepared and employed in peptide synthesis. Their structures, reactivities, and fluorine-specific interactions were studied by NMR and IR spectroscopy, X-ray diffraction, and in bioactivity assays. The mono-anionic PF5 motif displayed an amphiphilic character binding to hydrophobic surfaces, to water molecules, and to protein-binding sites, exploiting charge and H−F-bonding interactions. The novel motifs bind 25- to 30-fold stronger to the phosphotyrosine binding site of the protein tyrosine phosphatase PTP1B than the best current biomimetics, as rationalized by computational methods, including molecular dynamics simulations. KW - Chemical Biology KW - Drug Development KW - Pentafluorophosphates KW - Phosphotyrosine Biomimetics KW - Protein Tyrosine Phosphatases PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549984 DO - https://doi.org/10.1002/anie.202203579 SN - 1433-7851 VL - 134 IS - 25 SP - 1 EP - 6 PB - Wiley-VCH GmbH AN - OPUS4-54998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -