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- VP Vizepräsident (22)
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- 7.3 Brandingenieurwesen (9)
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- S.3 Ökodesign und Energieverbrauchskennzeichnung (7)
- 3.6 Elektrochemische Energiematerialien (6)
- S.1 Qualität im Prüfwesen (5)
- 3.0 Abteilungsleitung und andere (4)
- 8.3 Thermografische Verfahren (4)
- 4.6 Molekulare und angewandte Entomologie (3)
- 2.0 Abteilungsleitung und andere (2)
- 2.2 Prozesssimulation (2)
- 2.3 Einstufung von Gefahrstoffen und -gütern (1)
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Paper des Monats
- ja (68)
Mechanical flexibility in molecular crystals is a fascinating behavior with potential for developing advanced technologies. However, the phenomenon of mechanical bending is poorly understood. We explore for the first time the atomistic origin of elastic bending in a single component organic crystal using a combination of μ-focus synchrotron X-ray diffraction and ab initio simulation.
An amorphous Lewis-acidic zirconium chlorofluoride as HF shuttle: C–F bond activation and formation
(2023)
An exceptional HF transfer reaction by C–F bond activation of fluoropentane and a subsequent hydrofluorination of alkynes at room temperature is reported. An amorphous Lewis-acidic Zr chlorofluoride serves as heterogeneous catalyst, which is characterised by an eightfold coordination environment at Zr including chlorine atoms. The studies are seminal in establishing sustainable fluorine chemistry.
Characterization is a very important step in dealing with materials and waste streams generated during the operational and decommissioning phases of nuclear installations, including nuclear power plants. Characterization allows differentiation between materials that can be released from regulatory control and those that require further treatment and conditioning to become a stable waste form suitable for future storage and final disposal according to its waste classification. Characterization is also needed in the pre-disposal stages of radioactive waste management to demonstrate compliance with the waste acceptance criteria of the facilities that will accept the different waste forms. This work will present the strategies developed and implemented by the three projects for in-depth and accurate waste characterization and investigation of the different radioactive waste packages considered. CHANCE, MICADO, and PREDIS will present their goals, the methods developed, the technologies used and the (preliminary) results contributing to the improvement of the safety and the data and information quality of the waste packages analyzed at the different stages of the waste management process. Special emphasis will also be given to complementary approaches highlighting the usability of the technologies, the accessibility of the data, and the problem-solving of the three projects within the European panorama.
Metarhizium robertsii DSM 1490 is a generalist entomopathogenic fungus.
The mechanisms of pathogenesis of such fungi in insects like termites are not completely understood. Here, we report the draft genome sequence, as sequenced on the Oxford Nanopore platform. The genome has a GC% of 47.82 and a size of 45,688,865 bp
Elemental composition and thickness determination of thin films by electron probe microanalysis
(2023)
Electron probe microanalysis (EPMA) applies to solid samples of homogenous (bulk) chemical composition and can usually not be applied to structures which are inhomogeneous in the micrometer range such as thin film systems down to a few nm. However, in combination with the established thin film software Stratagem, the thickness as well as the elemental composition of thin films on a substrate can be determined. This has been recently successfully demonstrated for Fe-Ni on Si and Si-Ge on Al2O3 thin film systems. For both systems five samples of different elemental composition and a reference were produced and characterised by inductively coupled plasma mass spectrometry (ICP-MS), Rutherford backscattering (RBS), and transmission electron microscopy (TEM) as reference values. Last year, a new and open-source thin film evaluation programme called BadgerFilm has been released. It can also be used to determine thin film composition and thickness from intensity ratios of the unknown sample and standards (k-ratios). In this contribution, we reevaluated the data acquired for the Fe-Ni and Si-Ge systems using the BadgerFilm software package and compared the obtained elemental compositions and thickness values with the results of the Stratagem software and the reference methods. The conclusion is that the BadgerFilm software shows good agreement with the elemental composition and thickness calculated by Stratagem (mostly <2% for both composition and thickness) and with the reference values for two representative thin film systems (<1%–2% for composition and <10%–20% for thickness).
Comparative study of the co-assembly behaviour of 3-chloro-4-hydroxy-phenylazo dyes with DTAB
(2023)
The co-assembly of three one-fold negatively charged 3-chloro-4-hydroxy-phenylazo dyes (Yellow, Blue and Red) with the cationic surfactant dodecyltrimethylammoniumbromide (DTAB) was studied to probe dye–DTAB binding stoichiometry and assembly morphology. For each dye, phase separation was observed above a given dye : DTAB ratio with the ratio depending on the dye. While Yellow and DTAB showed liquid/liquid phase separation above Yellow : DTAB = 1 : 1.67, crystalline dye–DTAB complexes were observed for Blue–DTAB and Red–DTAB above Blue : DTAB = 1 : 2.56 and Red : DTAB = 1 : 2.94 respecively. In homogeneous solution, UV/vis spectroscopic investigations suggest stochiometries of Yellow : DTAB = 1 : 2, Blue : DTAB = 1 : 3 and Red : DTAB = 1 : 4. It was concluded, that Yellow exhibits the highest dye : DTAB binding stoichiometry in both, dye–surfactant complexes in the 2-phase region and in solution, whereas the lowest dye : DTAB binding stoichiometry was observed for Red–DTAB in both cases. The observed stoichiometries are inversely correlated to the impact dye addition has on the morphology of DTAB micelles. Generally, addition of dye to DTAB micelles leads to a reduction in spontaneous curvature of these micelles and to the formation of triaxial ellipsoidal or cylindrical micelles from oblate ellipsoidal DTAB micelles. At a DTAB concentration of 30 mM and a dye concentration of 5 mM, this effect was most pronounced for Red and least pronounced for Yellow, whilst Blue showed an intermediate effect.
For dangerous goods packagings, drop testing onto an essential unyielding target can be used to assess the mechanical resistance to impact loads. Adopted regulations like ADR/RID require that the impact surface provided shall be integral with a mass at least 50 times than that of the heaviest package to be tested. The problem is that many manufacturers do not possess impact targets that satisfy the required 50 times mass ratio for regulative drop tests during series production. The objective of this work is to verify existing and define improved criteria for impact target structures based on systematic investigations. Previous evidence highlights the relevance of other parameters in addition to the mass ratio. Therefore, in this research, a variation of drop test parameters was carried out experimentally. Furthermore, numerical vibration analysis was applied to investigate the deformability of the impact surface. The results conclude that the mass ratio of 1:50 cannot be defined as a decisive criterion. In order to determine the influence of further drop test parameters, the research findings were used to validate a parametric model which assesses impact target deflection. An approximation quality of over 90 % was achieved. As a result, new evaluation criteria are proposed. Firstly, a method for identifying critical impact target designs is provided. Secondly, a new comprehensive formula compares the approximated maximum deflection of a real impact target to the respective theoretical threshold derived from a worst-case assumption. In practice, this leads to great advantages in the evaluation of already installed impact targets for dangerous goods packagings.
The osseointegration in/around additively manufactured (AM) lattice structures of a new titanium alloy, Ti–19Nb–14Zr, was evaluated. Different lattices with increasingly high sidewalls gradually closing them were manufactured and implanted in sheep. After removal, the bone–interface implant (BII) and bone–implant contact (BIC) were studied from 3D X-ray computed tomography images. Measured BII of less than 10 µm and BIC of 95% are evidence of excellent osseointegration.
Since AMnaturally leads to a high-roughness surface finish, the wettability of the implant is increased.
The new alloy possesses an increased affinity to the bone. The lattice provides crevices in which the biological tissue can jump in and cling. The combination of these factors is pushing ossification beyond its natural limits. Therefore, the quality and speed of the ossification and osseointegration in/around these Ti–19Nb–14Zr laterally closed lattice implants open the possibility of bone spline key of prostheses. This enables the stabilization of the implant into the bone while keeping the possibility of punctual hooks allowing the implant to be removed more easily if required. Thus, this new titanium alloy and such laterally closed lattice structures are appropriate candidates to be implemented in a new generation of implants.
This paper reports the results of an international interlaboratory study sponsored by the Versailles Project on Advanced Materials and Standards (VAMAS) and led by the National Institute of Standards and Technology (NIST) on the measurement of water vapor sorption isotherms at 25 °C on a pelletized nanoporous carbon (BAM-P109, a certified reference material). Thirteen laboratories participated in the study and contributed nine pure water vapor isotherms and four relative humidity isotherms, using nitrogen as the carrier gas. From these data, reference isotherms, along with the 95% uncertainty interval (Uk=2), were determined and are reported in a tabular format.
In Leichtbauanwendungen sind Materialien mit geringen Dichten und hohen Festigkeiten gefragt. Insbesondere Faser-Kunststoff-Verbunde (FKV) erfüllen diese Anforderungen und werden zunehmend für Strukturbauteile eingesetzt. Die Oberflächen moderner Rotorblätter von Windkraftanlagen werden aus FKV gefertigt. Das Versagen dieser Materialien hat massiven Einfluss auf die Einsatzfähigkeit der gesamten Windkraftanlage. Daher ist die Kenntnis des Versagensverhaltens dieser Komponenten unter statischer und zyklischer Belastung von großem Interesse, um die Betriebsbeanspruchung abzuschätzen. Im Idealfall wird die Schadensentwicklung unter Betriebslast mit zerstörungsfreien in-situ-Prüfverfahren ermittelt. Hier berichten wir über die Beobachtung der Rissentwicklung in Carbon-Faserverstärkten Kunststoffen (CFK) unter kontinuierlicher Zugbelastung durch in-situ Synchrotron-Röntgenrefraktionsradiographie. Eine selbst entwickelte elektromechanische Zugprüfmaschine mit einem Kraftbereich bis zu 15 kN wurde in den Strahlengang an der BAMline (BESSY II) integriert. Da in herkömmlichen (Absorptions-) Radiographien Defekte wie Zwischenfaserbrüche oder Faser-Matrix-Enthaftung keinen ausreichenden Kontrast verursachen, wird zur Kontrastanhebung die Röntgenrefraktion benutzt. Hier wird das sogenannte Diffraction Enhanced Imaging (DEI) angewandt, um Primär- und gebrochene Strahlung mit Hilfe eines Analysatorkristalls zu trennen. Diese Technik ermöglicht schnelle Messungen mit einem Gesichtsfeld von einigen Quadratmillimetern (hier: 14 mm × 7.2 mm) und ist ideal für in-situ Untersuchungen. Die Bildgebung und der Zugversuch erfolgen mit einer Bildfrequenz von 0.7 / s und einer Dehnrate von 0.00055 / s . Bei 0°/90° Fasergelegen treten die ersten Zwischenfaserrisse bei 380 MPa (Dehnung 0.8 %) auf. Vor dem Versagen bei ca. 760 MPa (Dehnung 2.0 %) beobachten wir die Ausbildung eines nahezu äquidistanten Rissmusters (Risse in ca. 1 mm Abstand), das sich im geschädigten Zustand über die gesamte Probe erstreckt.
One of the main challenges for the synthesis and application of the promising hard-magnetic compound CeFe11Ti is the formation of Laves phases that are detrimental for their thermodynamic stability and magnetic properties. In this paper, we present an ab initio based approach to modify the stability of these phases in the Ce-Fe-Ti system by additions of 3d and 4d elements. We combine highly accurate free-energy calculations with an efficient screening technique to determine the critical annealing temperature for the formation of Ce(Fe,X)11Ti. The central findings are the dominant role of the formation enthalpy at T = 0 K on chemical trends and the major relevance of partial chemical decompositions. Based on these insights, promising transition metals to promote the stability of the hard-magnetic phase, such as Zn and Tc, were predicted. The comparison with suction casting and reactive crucible melting experiments for Ce-Fe-Ti-X (X = Cu, Ga, Co, and Cr) highlights the relevance of additional phases and quaternary elements.
The release of hazardous compounds from construction products can harm human health and the environment. To improve the sustainability of construction materials, the leaching of substances from construction products and their potential environmental impact should be assessed. Twenty-seven construction products from different product groups were examined with a combination of standardized leaching tests (dynamic surface leaching test and percolation test) and biotests (algae, daphnia, fish egg, luminescent bacteria, umu and Ames fluctuation tests). To identify the released substances, extensive qualitative and quantitative chemical analyses were performed, including gas chromatographic and liquid chromatographic screening techniques.
Results: Many of the tested eluates caused signifcant ecotoxic efects. Particularly high ecotoxicities were observed for grouts (lowest ineffective dilution (LID) up to 16384) and cork granules (LID up to 24578). The results of ecotoxicity tests allow the prioritization of the eluates that should be subjected to detailed chemical analyses. Organic screening by different methods and ranking the identifed substances based on recorded hazard classification is a suitable approach to identify the relevant toxic substances.
Conclusions: Determining the ecotoxicity of eluates from construction products records the summary effect of all leachable substances. This instrument is especially useful for construction products of complex and largely unknown composition. The ecotoxicological and the chemical–analytical approach complement each other in an ideal way to characterize the potential hazard of eluates from construction products and to identify the environmentally hazardous components in these eluates. Our results confirm that the proposed harmonized methods for testing eluate toxicity are an adequate and applicable procedure to move toward a more sustainable way of building and to reduce toxic effects of construction products in their use phase in the environment.
A facile yet robust synthesis is reported herein to simultaneously incorporate atomically dispersed Co-Nₓ sites with graphitic layer-protected Co₉S₈ nanoparticles (denoted as Co SACs+Co₉S₈) as an efficient electrocatalyst for oxygen reduction in acidic solution. The Co SACs+Co₉S₈ catalyst shows low H₂O₂ selectivity (∼5 %) with high half-wave potential (E1/2) of ∼0.78 V(RHE) in 0.5 M H₂SO₄. The atomic sites of the catalyst were quantified by a nitrite stripping method and the corresponding site density of the catalyst is calculated to be 3.2×10¹⁸ sites g⁻¹. Besides, we also found the presence of a reasonable amount of Co₉S₈ nanoparticles is beneficial for the oxygen electrocatalysis. Finally, the catalyst was assembled into a membrane electrode assembly (MEA) for evaluating its performance under more practical conditions in proton exchange membrane fuel cell (PEMFC) system.
Creep-resistant steels such as the 13CrMoV9-10, used in the construction of thick-walled pressure vessels, are most commonly submerged arc welded (SAW). These steels can develop stress relief cracks (SRC) if the mandatory post weld heat treatment (PWHT) is performed improperly. Current PWHT parameters, such as heating rate and holding time at a specific holding temperature, are based on both empirical experience and conventional free shrinking welding experiments to characterize the SRC-susceptibility of the weld. These cannot adequately depict the higher residual stresses caused by the structurally induced stiffness of the surrounding construction. This study discusses the development of a repeatable, precise, and time-efficient methodology to study the effects of different stress levels and heating rates on the SRC susceptibility of the coarse grain heat-affected zone (CGHAZ). For that purpose, samples were thermically treated to simulate a coarse grain heat-affected zone (CGHAZ) and subsequently exposed to representative levels of stress during the heating phase of a PWHT. The recorded stress and heating rate–dependent strains were mathematically analyzed via curve tracing/calculus to identify interdependent effects. This procedure facilitates the measurement of material characteristics such as carbide growth on grain boundaries at the µm-scale via an integrated value over the entire sample volume. The first and second derivatives show a slight, precipitate-dependent, increase in hardness of the sample, depending on the heating rate and applied stress. This new methodology generates an improved assessment of the SRC susceptibility of SAW microstructures of creep-resistant CrMoV steels.
In the present paper, an approach for updating the continuous stress range distribution of a welded connection of a wind turbine support structure with predicted information from strain measurements is presented. Environmental conditions, such as wind or, in offshore fields, waves and currents, in combination with rotor excitations generate cyclic stresses affecting the reliability of welded joints of the support structure over the service life. Using strain measurements, these conditions can be monitored, and the resulting stress ranges, under consideration of measurement, mechanical and material uncertainties, can be reconstructed. These stress ranges can be used as an input for updating the prior probability density function (PDF) of the stress ranges predicted by the overall dynamics and a detailed design analysis. Applying Bayesian probability theory and decision theoretical implications, the predicted posterior probability density of the stress ranges is calculated based on the design information and uncertainties. This approach is exemplified, and it is shown how the predicted stress ranges and the design stress ranges are distributed. The prior and the predicted posterior stress ranges are used for a reliability calculation for potentially entering a pre-posterior decision analysis
The electron density and temperature of a laser-induced plasma can be determined from the width and intensity of the spectral lines, provided that the corresponding optical transitions are optically thin. However, the lines in laser induced plasma are often self-absorbed. One of the methods of correction of this effect is based on the use of the Planck function and an iterative numerical calculation of the plasma temperature. In this study, the method is further explored and its inherent errors and limitations are evaluated. For this, synthetic spectra are used that fully correspond to the assumed conditions of a homogeneous isothermal plasma at local thermodynamic equilibrium. Based on the error analysis, the advantages and disadvantages of the method are discussed in comparison with other methods of self-absorption correction.
Wire arc additive manufacturing (WAAM) enables the efficient production of weight-optimized modern engineering structures. Further increases in efficiency can be achieved by using high-strength structural steels. Commercial welding consumables for WAAM are already available on the market. Lack of knowledge and guidelines regarding welding residual stress and component safety during production and operation leads to severely limited use for industry applications. The sensitive microstructure of high-strength steels carries a high risk of cold cracking; therefore, residual stresses play a crucial role. For this reason, the influences of the material, the WAAM process, and the design on the formation of residual stresses and the risk of cold cracking are being investigated. The material used has a yield strength of over 800 MPa. This strength is adjusted via solid solution strengthening and a martensitic phase transformation. The volume expansion associated with martensite formation has a significant influence on the residual stresses. The focus of the present investigation is on the additive welding parameters and component design on their influence on hardness and residual stresses, which are analyzed by means of X-ray diffraction (XRD). Reference specimens (hollow cuboids) are welded fully automated with a systematic variation of heat control and design. Welding parameters and AM geometry are correlated with the resulting microstructure, hardness, and residual stress state. Increased heat input leads to lower tensile residual stresses which causes unfavorable microstructure and mechanical properties. The component design affects heat dissipation conditions and the intensity of restraint during welding and has a significant influence on the residual stress.
Ein großer Teil unserer Brücken wurden in den 1950er bis 1970er Jahren als Spannbetonbrücken gebaut. Mit der damals noch relativ jungen Technologie entstanden elegante, teilweise gewagte Bauwerke mit großen Spannweiten, welche die Vorteile der Materialien Stahl und Beton geschickt kombinieren. Die Standsicherheit einiger dieser Brücken ist heute gefährdet. Die Ursachen liegen in der enorm gewachsenen Belastung durch Schwerverkehr, teilweise ungenügender Wartung und in konstruktiven und Materialschwächen, die der mangelnden Erfahrung mit der Technologie in der Bauzeit geschuldet sind. Ein neuralgischer Punkt der Bauwerke sind die in den Beton integrierten Spannglieder.
Infolge von Korrosion und Ermüdung können Elemente der Spannglieder reißen, wodurch die für das Tragwerk notwendige Spannung und somit die Tragfähigkeit reduziert werden. Nicht bei allen Brücken kündigen sichtbare Risse im Beton oder auffällige Verformungen den Tragfähigkeitsverlust bzw. das finale Versagen rechtzeitig an.
Die Schallemissionsanalyse ist die derzeit einzige Methode, das Reißen einzelner Spannstähle zuverlässig und mit wirtschaftlich vertretbarem Aufwand zu detektieren. Trotzdem es schon einige Spannbetonbauwerke gibt, die mit Schallemissionsanalyse überwacht werden, ist das Verfahren noch wenig bekannt.
Außerdem fehlen technische Richtlinien, was die Ausschreibung und Vergabe von entsprechenden Aufträgen und die Bewertung der Angebote sehr erschwert. Um sowohl Baulastträger als auch Dienstleistungsanbieter in den Vergabeverfahren und im Betrieb der Monitoringsysteme zu unterstützen, hat sich eine Gruppe von Experten aus den Bereichen Bauingenieurwesen und Schallemission zum Entwurf einer Richtlinie „Detektion von Spanndrahtbrüchen mit Schallemission“ zusammengefunden. Mit diesem Beitrag wird die Richtlinie vorgestellt, deren Bearbeitung bis zur SCHALL 23 abgeschlossen sein soll.
problem. One reason is the sensitivity to stress corrosion cracking of the prestressing steel. Failure of prestressing wires can result in collapse of the entire structure without premature indication by transverse bending cracks or considerable deformation. The response of a structure to significant number of prestressing wire breaks was studied on a bridge in Brandenburg, Germany. Two thirds of the prestressing wires in concentrated tendons of two girders were cut before the bridge was demolished. Acoustic Emission Analysis was used to detect the wire breaks. Thus, the number of wire breaks was correlated with results of other measurement techniques, in particular strain measurements on the girders. In preparation of the measurements, the acoustic properties of the bridge were determined and the suitability of Schmidt hammer impacts as an acoustic reference source was validated.
Ergot alkaloids are a group of mycotoxins occurring in products derived from various grasses (e.g., rye) and have been regulated in the EU recently. The new maximum levels refer to the sum of the six most common ergot alkaloids in their two stereoisomeric forms in different food matrices. Typically, these twelve compounds are individually quantified via HPLC-MS/MS or -FLD and subsequently summed up to evaluate food safety in a time-consuming process. Since all these structures share the same ergoline backbone, we developed a novel sum parameter method (SPM) targeting all ergot alkaloids simultaneously via lysergic acid hydrazide. After extraction and clean-up, in analogy to the current European standard method EN 17425 (ESM) for ergot alkaloid quantitation, the samples were derivatized by an optimized hydrazinolysis protocol, which allowed quantitative conversion after 20 min at 100 °C. The new SPM was evaluated against another established HPLC-FLD-based method (LFGB) and the HPLC-MS/MS-based ESM using six naturally contaminated rye and wheat matrix reference materials. While the SPM provided comparable values to the ESM, LFGB showed deviating results. Determined recovery rates, limits of detection and quantification of all three employed methods confirm that the new SPM is a promising alternative to the classical approaches for ergot alkaloid screening in food.