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Paper des Monats
- ja (68)
The prediction of the properties of the materials used in the operation of components is of enormous importance, in order to accelerate the development process of new components. To evaluate new materials in terms of their performance (in a component), the development of new innovative methods is necessary. These methods can also be summarized under the term lab-to-field or materials – upscaling, meaning materials being characterised in a laboratory and their properties being upscaled to the component performance by means of e.g. simulation. i-TRIBOMAT is a EU funded project (H2020, GA Nr. 814494) aiming at building an Open Innovation Test Bed for tribological material characterization and offering corresponding services from tribological characterization of new materials to simulation models for predicting the performance of industrial components. By bundling the infrastructure, know-how for characterization and building a digital platform, i-TRIBOMAT becomes the world’s largest open innovation test bed for tribological material characterization.
A technique for calculating the main solidification parameters for a two-dimensional columnar crystal growth during complete penetration laser beam welding of thin steel sheets was developed. Given that the weld pool interface is described by Lamé curves (superellipses) within the horizontal plane of growth, general analytical solutions were derived for the geometry of the crystal axis and the corresponding growth rate and cross-sectional area of the crystal. A dimensionless analysis was performed to provide insights on the dependence of the solidification parameters on the shape and dimensions of the rear part of the weld pool boundary. The derived solutions were applied for the case of complete penetration laser beam keyhole welding of 2 mm thick 316L austenitic chromium-nickel steel sheets. It was shown that the reconstruction of the weld pool boundary with Lamé curves provides higher accuracy and flexibility compared to results obtained with elliptical functions. The validity of the proposed technique and the derived analytical solutions was backed up by a comparison of the obtained solutions to known analytical solutions and experimentally determined shapes and sizes of the crystals on the top surface of the sheet. The dimensions of the calculated crystal axis correlated well with the experimentally obtained results.
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.
The flow properties of powdery or granular filling substances for dangerous goods packagings are safety-relevant parameters. To specify the flow behavior, the angle of repose is measured in the recognized test centers for dangerous goods packagings in Germany. Previous investigations performed on non-hazardous substances revealed that some of the methods currently used have disadvantages in application. Additionally, for occupational health and safety reasons, it was generally viewed critically to carry out measurements of the angle of repose for dangerous goods at all. Instead, the dimensionless Hausner ratio to describe the flow behavior was proposed.
In this work, the investigations were extended to real hazardous substances to concretize the assessment. Five exemplary hazardous substances were tested for their angle of repose using the methods commonly applied in the test centers. The Hausner ratio was also determined. In addition, the influence of a different climatic preconditioning on the angle of repose measurement was examined using three selected non-hazardous bulk materials.
The results show that the measurement of the angle of repose is not fundamentally excluded for dangerous goods. However, for reasons of applicability, repeatability and occupational health and safety, only the ISO method can be applied for dangerous filling substances. This method provides conservative results regarding a safety-related evaluation of flow properties for the transport of dangerous goods.
In principle, both the ISO method and the determination of the Hausner ratio can be used for dangerous goods. It is also essential especially with finely powdered filling goods, to carry out controlled preconditioning.
Composition and Explosibility of Gas Emissions from Lithium-Ion Batteries Undergoing Thermal Runaway
(2023)
Lithium-based batteries have the potential to undergo thermal runaway (TR), during which mixtures of gases are released. The purpose of this study was to assess the explosibility of the gaseous emission from LIBs of an NMC-based cathode during thermal runaway. In the current project, a series of pouch lithium-based battery cells was exposed to abuse conditions (thermal) to study the total amount of gases released and the composition of the gas mixture. First, the battery cells were placed in a closed vessel, and the pressure and temperature rise inside the vessel were measured. In a second step, the composition of gases was analysed using a Fourier transform Infrared (FTIR) spectrometer.
We found that the amount of released gases was up to 102 ± 4 L, with a clear dependence on the battery capacity. This study showed that the concentration of gaseous emissions such as carbon monoxide (CO), methane (CH4), ethylene (C2H4), ethane (C2H6), and hydrogen cyanide (HCN) increased with higher cell capacity. Of the five studied flammable gases, the maximum concentrations of carbon monoxide (16.85 vol%), methane (7.6 vol%), and ethylene (7.86 vol%) were identified to be within their explosible range. Applying Le Chatelier’s law, a calculated lower explosion limit (LEL) of 7% in volume fraction was obtained for the gas mixture. The upper explosion limit (UEL) of the gas mixture was also found to be 31% in volume. A filter comprising pyrobubbles was used for the removal of the studied gas components released during the thermal abuse. The investigation revealed that the pyrobubbles filter was highly effect in the removal of HCN (up to 94% removal) and CO2 (up to 100% removal). Herein, we report the dependency of the method of thermal runaway trigger on the measured maximum temperature.
Asymmetrical Flow Field-Flow Fractionation (AF4), as a cleaning technique, was combined on-line with the multielemental analytical capabilities of an Inductively Coupled Plasma-Time of Flight-Mass Spectrometer (ICP-ToF-MS). In that manner, the heavy ionic matrix effect of untreated cells' samples can be significantly reduced. As a proof of concept, commercial baker's yeast cells were analysed.
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).
We investigated the performance of nitrogen microwave inductively coupled atmospheric-pressure plasma mass spectrometry (MICAP-MS) under matrix effects and its applicability to trace element analysis in steels. Influences of different gas flows and ion optics on the matrix tolerance are studied, indicating that nebulizer gas flow has the most significant impact. Optimization of ion optics improves matrix tolerance for light elements due to the reduction of the inelastic collisional scattering effect. With optimized operating conditions, MICAP-MS achieves an internal standard intensity recovery of over 90% at an Fe concentration of 500 mg L−1. Even at an Fe concentration of 1 g L−1, the recovery remains above 80%. Three certified reference materials – non-alloy, low-alloy and high-alloy steel – were analyzed using MICAP-MS. The determined mass concentrations of the trace and minor components show metrological compatibility to the reference values. No significant differences are observed between the results obtained with aqueous and matrix-matched calibration, demonstrating the strong matrix tolerance of MICAP-MS, and its promising applicability to steel analysis.
Half of global material consumption involves mineral material. The circularity is still low so that the enhanced use of secondary building material is required to close loops. Three different secondary building materials are discussed based on exemplary research results: construction and demolition waste (C&D waste), soil-like material, and incineration bottom ash (IBA). Focus was placed on the environmental compatibility of the materials examined mainly by standardized leaching tests. C&D waste was investigated after a wet treatment using a jigging machine, and soil-like material and IBA were characterized with respect to their material composition. Their environmental compatibilities in particular were studied using standard leaching tests (batch tests and column tests).
It was concluded that soil-like material can mostly be utilized even when the precautionary limit values set are exceeded by a factor of less than two. For C&D waste, the fine fraction below 2 mm and the content of brick material is problematic. IBA fulfills quality level “HMVA-2” following German regulations. Improved levels of utilization might be achievable with better treatment technologies.
Cardiac troponin I (cTnI) is a crucial biomarker for diagnosing cardiac vascular diseases, including acute myocardial infarction (AMI). This study presents a proof-of-concept chemiluminescence-based immunosensor for rapid and accurate measurement of cTnI, with the potential for online monitoring. The immunosensor incorporates a flow cell design and a sensitive complementary metal-oxide-semiconductor (CMOS) camera for optical readout. A microfluidic setup was established to enable selective and quasi-online determination of cTnI within ten minutes. The sensor was tested with recombinant cTnI in phosphate buffer, demonstrating measurements in the concentration range of 2–25 µg/L, with a limit of detection (LoD) of 0.6 µg/L (23 pmol/L) achieved using the optimized system. The immunosensor exhibited high selectivity, as no cross-reactivity was observed with other recombinant proteins such as cTnT and cTnC at a concentration of 16 µg/L. Measurements with diluted blood plasma and serum yielded an LoD of 60 µg/L (2.4 nmol/L) and 70 µg/L (2.9 nmol/L), respectively. This biosensor offers a promising approach for the rapid and sensitive detection of cTnI, contributing to the diagnosis and management of acute myocardial infarction and other cardiac vascular diseases.
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.
Die Brechung von Röntgenstrahlen (Röntgenrefraktion) an Grenzflächen zwischen Materialien unterschiedlicher Dichte ist analog zur Ablenk-ung von sichtbarem Licht an z.B. Glasoberflächen. Es gibt jedoch zwei wesentliche Unterschiede:
a) konvexe Grenzflächen verursachen Divergenz (d.h. der Brechungsindex n ist kleiner als 1), und
b) die Ablenkungswinkel sind sehr klein, und reichen von einigen Bogensekunden bis zu einigen Bogenminuten (d.h. n ist nahe bei 1);
Wie auch bei sichtbarem Licht ist die Ablenkungsrichtung der Röntgenstrahlen abhängig von der Orientierung der durchstrahlten Grenzfläche. Aufgrund dieser Eigenschaften eignen sich Röntgenrefraktionsmethoden hervorragend für:
a) die Erkennung und Quantifizierung von Defekten wie Poren und Mikrorissen und
b) die Bewertung von Porosität und Partikeleigenschaften wie Orientierung, Größe und räumliche Verteilung.
Wir zeigen die Anwendung der Röntgenrefraktionsradiographie (2,5D Technik) und der -tomographie (3D Technik) für die Untersuchung verschiedener Probleme in der Werkstoffwissenschaft und -technologie:
a) Sintern von SiC-Grünkörpern
b) Porositätsanalyse in Dieselpartikelfiltersilikaten
c) Faser-Matrix-Haftung in Metall- und Polymermatrixverbundwerkstoffen
d) Mikrorissbildung in Glaskeramik.
Wir zeigen, dass der Einsatz von Röntgenrefraktionsmethoden quantitative Ergebnisse liefert, die direkt als Parameter in Werkstoffmodellen verwendet werden können.
For the first time, µ-X-ray fluorescence (µ-XRF) mapping combined with fluorine K-edge µ-X-ray absorption near-edge structure (µ-XANES) spectroscopy was applied to depict per- and polyfluoroalkyl substances (PFAS) contamination and inorganic fluoride in samples concentrations down to 100 µg/kg fluoride. To demonstrate the matrix tolerance of the method, several PFAS contaminated soil and sludge samples as well as selected consumer product samples (textiles, food contact paper and permanent baking sheet) were investigated. µ-XRF mapping allows for a unique element-specific visualisation at the sample surface and enables localisation of fluorine containing compounds to a depth of 1 µm. Manually selected fluorine rich spots were subsequently analysed via fluorine K-edge µ-XANES spectroscopy. To support spectral interpretation with respect to inorganic and organic chemical distribution and compound class determination, linear combination (LC) fitting was applied to all recorded µ-XANES spectra. Complementarily, solvent extracts of all samples were target-analysed via LC-MS/MS spectrometry. The detected PFAS sum values range from 20 to 1136 µg/kg dry weight (dw). All environmentally exposed samples revealed higher concentration of PFAS with a chain length >C8 (e.g. 580 µg/kg dw PFOS for Soil1), whereas the consumer product samples showed a more uniform distribution with regard to chain lengths from C4 to C8. Independent from quantified PFAS amounts via target analysis, µ-XRF mapping combined with µ-XANES spectroscopy was successfully applied to detect both point-specific concentration maxima and evenly distributed surface coatings of fluorinated organic contaminants in the corresponding samples.
Although fire safety regulations for buses have been adapted in recent years regarding, for example, fire detection and engine fire suppression systems, the changes in regulations for bus interior materials are minimal. A comparison of fire safety regulations for interior materials in other transport sectors for trains, ships or aircraft reveals a much lower level of requirements for bus materials. Although repeated bus accidents as well as fire statistics show the danger a bus fire can pose to passengers.
In particular, the combination of a fire incident and passengers with reduced mobility led to severe disasters in Germany and other European countries. To enhance the fire safety for passengers, the interior bus materials are crucial as the fire development in the bus cabin determines whether escape and rescue is possible. Against this background, bus interior materials were tested in different fire test scenarios. Measurement of a wide variety of parameters, for example, the mass loss, ignition time, smoke gas composition, heat release rate among others were carried out. Tested materials complied to the newest set of requirements. For this purpose, interior materials and their components had to be identified according to their chemical structure. Parts of the tests were funded by BASt (Federal Highway Research Institute) in the project 82.0723/2018. Experimental results show reaction-to-fire behaviour which lead to very limited times for escape and rescue in case of fire in a bus cabin. Based on the studies on fire behaviour and toxicity assessment, recommendations for improved fire safety regulations for interior materials could be made.
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.
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.
The complex nature of liquid water saturation of polymer electrolyte fuel cell (PEFC) catalyst layers (CLs) greatly affects the device performance. To investigate this problem, we present a method to quantify the presence of liquid water in a PEFC CL using small-angle X-ray scattering (SAXS). This method leverages the differences in electron densities between the solid catalyst matrix and the liquid water filled pores of the CL under both dry and wet conditions. This approach is validated using ex situ wetting experiments, which aid the study of the transient saturation of a CL in a flow cell configuration in situ. The azimuthally integrated scattering data are fitted using 3D morphology models of the CL under dry conditions. Different wetting scenarios are realized in silico, and the corresponding SAXS data are numerically simulated by a direct 3D Fourier transformation. The simulated SAXS profiles of the different wetting scenarios are used to interpret the measured SAXS data which allows the derivation of the most probable wetting mechanism within a flow cell electrode.
We present how mesoporosity can be engineered in transition metal phosphate (TMPs) materials in a template-free manner. The method involves the transformation of a precursor metal phosphate phase, called M-struvite (NH4MPO4·6H2O, M = Mg2+, Ni2+, Co2+, NixCo1−x2+). It relies on the thermal decomposition of crystalline M-struvite precursors to an amorphous and simultaneously mesoporous phase, which forms during degassing of NH3 and H2O. The temporal evolution of mesoporous frameworks and the response of the metal coordination environment were followed by in situ and ex situ scattering and diffraction, as well as X-ray spectroscopy. Despite sharing the same precursor struvite structure, different amorphous and mesoporous structures were obtained depending on the involved transition metal. We highlight the systematic differences in absolute surface area, pore shape, pore size, and phase transitions depending on the metal cation present in the analogous M-struvites. The amorphous structures of thermally decomposed Mg-, Ni- and NixCo1−x-struvites exhibit high surface areas and pore volumes (240 m2 g−1 and 0.32 cm−3 g−1 for Mg and 90 m2 g−1 and 0.13 cm−3 g−1 for Ni). We propose that the low-cost, environmentally friendly M-struvites could be obtained as recycling products from industrial and agricultural wastewaters. These waste products could be then upcycled into mesoporous TMPs through a simple thermal treatment for further application, for instance in (electro)catalysis.
Normung und Standardisierung in der zerstörungsfreien Prüfung finden auf nationaler, europäischer und internationaler Ebene statt. Durch die Übernahme von Leitungsfunktionen in diesen Gremien kann ein deutlicher steuernder Einfluss auf Themen und Inhalte der Normen genommen werden. Unabdingbar für den Erfolg ist zusätzlich das persönliche Engagement der Fachexpert*innen in den nationalen Gremien und den europäischen und internationalen Arbeitsgruppen. Denn wer nicht normt wird genormt und muss letztlich Regeln verwenden, die andere entsprechend ihrer eigenen Interessen gestalten. Voraussetzung für die Teilnahme in europäischen und internationalen Normungsgremien ist die Mitwirkung in den entsprechenden nationalen Spiegelgremien der nationalen Normungsinstitute, welche die europäischen und internationalen Aktivitäten spiegeln und die Fachexperten für die Mitarbeit autorisieren.
Gezeigt werden die relevante Gremienstruktur auf internationaler Ebene (ISO/TC 135 “Non-destructive testing”, ISO/TC 44/SC 5 “Testing and inspection of welds”), auf europäischer Ebene (CEN/TC 138 “Zerstörungsfreie Prüfverfahren”), die Struktur der nationalen deutschen Spiegelgremien, das Zusammenspiel der Gremien, und die Einflussmöglichkeiten.
A well-defined terminology of fire-related variables is important for correct analyses and supporting knowledge-based decisions regarding the evaluation of building fires at the European level. After developing an overview of current practices for fire statistics in Part I, the terminology used and the data collected by the EU Member States and eight other countries regarding fire incidents, property damage and human losses were mapped to increase awareness of their practice and support a comprehensive assessment of several fire statistical datasets. A questionnaire was distributed to relevant authorities responsible for the collection, elaboration/analysis, and fire statistical data publications to define and select the essential variables for an appropriate fire assessment and fire incident description. Based on the results of the questionnaire able to identify the essential fire statistical variables and a detailed analysis of current definitions adopted in the fire statistics of the EU Member States and other countries, a common terminology is proposed to collect the necessary data in the EU Member States and obtain meaningful datasets based on standardised terms and definitions. The results will generate essential outputs to move towards harmonised fire statistics at the EU level and contribute to an appropriate analysis able to improve fire prevention and fire mitigation in building fires.
This study provides an analysis on the fire safety of passengers and the fire protection of coaches and buses. A brief review of major bus fire incidents, an overview of current regulations in Europe, and their limitations are presented. The study finds that the current small-scale fire test methods described in UN ECE Reg No. 118 need to be replaced by test methods that can assess the reaction to fire of materials when exposed to ignition sources of varying sizes. To address these shortcomings, the study proposed an expert recommendation to update the material fire safety requirements and testing for buses. Additional measures are proposed, derived from objectives and strategies applied in other transport sectors, and can be tested through existing European and international standards, which are widely used by several industries. These measures aim to extend the time with tenable conditions for a safe evacuation in case of fire, reduce the degree of damage to buses, reduce the risk for fast and excessive thermal exposure on modern energy carriers needed for a more sustainable transport sector.
The analysis of the current state of fire statistics and data collection in Europe and other countries is needed to increase awareness of how fire incidents affect buildings and to support pan-European fire prevention and fire mitigation measures.
The terminology and data collected regarding fire incidents in buildings in the EU Member States were mapped to obtain meaningful datasets to determine common terminology, collection methodology, and data interpretation system. An extensive literature review showed that fire data collection systems have been instrumental in informing firefighting strategies, evidence-based planning, prevention, and educational programmes. Differences and similarities between fire data collection systems were also investigated. The amount and quality of the information in fire statistical recording systems appear to be influenced by the complexity and structure with which the data are collected. The analysis also examined the existing fire statistics in the EU Member States and a few other countries. Finally, a detailed investigation of the number of fires, fire deaths, and injuries from 2009 to 2018 in several countries was examined based on data from a report by CTIF. The trends showed differences attributable to the existing fire statistical practices in terms of terminology and data
collection, and interpretation. Part II proposes a common terminology for selected fire statistical variables. The results provide relevant information regarding fire safety at the European level and should be used to guide the development of more uniform fire statistics across Europe.
Immobilized metal affinity chromatography (IMAC) is a widely used technique for purifying polyhistidine-tagged recombinant proteins. However, it often has practical limitations that require complex optimizations and additional steps for purification. In this study, we introduce functionalized corundum particles as a novel, efficient, and economical method for purifying recombinant proteins in a column-free format. The corundum surface is modified with amino silane APTES, followed by EDTA dianhydride, and then loaded with nickel ions. We used the Kaiser test to monitor the modification process and ICP-MS to quantify the metal-binding capacity. To evaluate the system, we used His-tagged protein A/G (PAG) mixed with bovine serum albumin (BSA). The corundum particles exhibited a binding capacity of approximately 3 mg of protein per gram of corundum or 2.4 mg per 1 mL of corundum suspension. We also examined cytoplasm obtained from different E. coli strains as an example of a complex matrix. Varying the imidazole concentration in the loading and washing buffers showed that higher concentrations during loading improved purity. Even with sample volumes as large as one liter, we successfully isolated recombinant proteins down to a concentration of 1 µg/mL. We found higher purity levels with corundum when comparing the corundum material to standard Ni–NTA agarose beads. We successfully purified His6-MBP-mSA2, a fusion protein comprising monomeric streptavidin and maltose-binding protein, from E. coli cytoplasm, demonstrating the method's applicability. We also purified SARS-CoV-2-S-RBD-His8 expressed in human Expi293F cells, confirming its suitability for mammalian cell culture supernatants. The material cost of the nickel-loaded corundum material (without regeneration) is estimated to be less than 30 cents per gram of functionalized support or 10 cents per milligram of isolated protein. Another advantage of this system is the exceptional physical and chemical stability of corundum particles. Overall, we have demonstrated that this novel material offers an efficient, robust, and cost-effective purification platform for His-tagged proteins, even in challenging, complex matrices and large sample volumes with low product concentrations. This method has potential applications in both small laboratories and large-scale industrial settings.
We examine the performance of a number of single-atom M−N/C electrocatalysts with a common structure in order to deconvolute the activity of the framework N/C support from the metal M−N4 sites in M−N/Cs. The formation of the N/C framework with oordinating nitrogen sites is performed using zinc as a templating agent. After the formation of the electrically conducting carbon−nitrogen metal-coordinating network, we (trans)metalate with different metals producing a range of different catalysts (Fe−N/C, Co−N/C, Ni−N/C, Sn−N/C, Sb−N/C, and Bi−N/C) without the formation of any metal particles. In these materials, the structure of the carbon/nitrogen framework remains unchanged-only the coordinated metal is substituted. We assess the performance of the subsequent catalysts in acid, near-neutral, and alkaline environments toward the oxygen reduction reaction (ORR) and ascribe and quantify the performance to a combination of metal site activity and activity of the carbon/nitrogen framework. The ORR activity of the carbon/nitrogen framework is about 1000-fold higher in alkaline than it is in acid, suggesting a change in mechanism. At 0.80 VRHE, only Fe and Co contribute ORR activity significantly beyond that provided by the carbon/nitrogen framework at all pH values studied. In acid and near-neutral pH values (pH 0.3 and 5.2, respectively), Fe shows a 30-fold improvement and Co shows a 5-fold improvement, whereas in alkaline pH (pH 13), both Fe and Co show a 7-fold improvement beyond the baseline framework activity. The site density of the single metal atom sites is estimated using the nitrite adsorption and stripping method. This method allows us to deconvolute the framework sites and metal-based active sites. The framework site density of catalysts is estimated as 7.8 × 1018 sites g−1. The metal M−N4 site densities in Fe−N/C and Co−N/C are 9.4 × 1018 sites−1 and 4.8 × 1018 sites g−1, respectively.
Bei der Prüfung von Werkstücken mit empfindlichen Oberflächen oder auch hydrophilen Werkstoffen sind traditionelle ultraschallbasierte zerstörungsfreie Prüfmethoden wie die Kontakttechnik oder die Tauchtechnik in vielen Anwendungsfällen aufgrund der Flüssigkeitsankopplung nicht anwendbar.
Die luft-gekoppelte Ultraschallprüfung umgeht diese Problematik und eröffnet neue Prüfszenarien. Derzeit werden zwei Varianten der Schallerzeugung als vielversprechend angesehen: ferroelektrische Folien und thermoakustische Dünnschichtwandler. Thermoakustische Wandler ermöglichen die resonanzfreie Erzeugung von Ultraschall und somit kurze zeitliche Impulse sowie eine sehr breitbandige Anregung. Durch die Verwendung von gekrümmten Substraten ist sowohl eine Herstellung von planaren als auch fokussierten Wandlern möglich.
Dieser Beitrag präsentiert die letzten Forschungsergebnisse im Bezug auf thermoakustischen Wandlern, welche derzeit in einen thermoakustischen Gruppenstrahler münden. Gruppenstrahler erlauben die simultane Änderung des Einschallwinkels, sowie die Verschiebung des Fokuspunktes während der Verwendung.
Durch die Verbindung beider Schlüsseltechnologien, der thermoakustischen Anregung und des Gruppenstrahlerprinzips, wird das Spektrum der klassischen ZfP-Anwendungen, sowie moderner Ansätze wie der Anregung von geführten Wellen oder der Strukturüberwachung erheblich erweitert und bereichert.
Dabei soll innerhalb dieses Beitrages auf die Modellierung des Schallfeldes, die elementweise Charakterisierung und verschiedene Anwendungsszenarien eingegangen werden.
Phased-Array-Prüfköpfe für luftgekoppelte Ultraschallprüfung auf Basis von zellulären Kunststoffen
(2023)
Luftgekoppelte Ultraschallprüfung setzt sich immer häufiger gegen die konventionelle Ultraschallprüfung von Leichtbaukomponenten durch, und zwar in vielen Industriezweigen von der Holzindustrie bis zur Luftfahrt. Während die Phased-Array-Technik mittlerweile zu dem industriellen Standard im Bereich der Prüfung mit Ankopplung gehört, wird luftgekoppelte Ultraschallprüfung meist mit zwei Wandlern in Durchschallung durchgeführt. Deswegen werden Vorteile der Phased-Array-Technik wie beispielsweise elektronische Fokussierung oder Schwenkung des Einschallwinkels für luftgekoppelte Prüfung selten genutzt.
In diesem Beitrag werden die laufenden Arbeiten an der Entwicklung eines neuen Phased-Array-Geräts vorgestellt, mit dem Schwerpunkt an der Charakterisierung der Prüfköpfe und ihrer Schallfelder. Das Gerät besteht aus einem linearen Phased-Array-Prüfkopf, einer Sende- und einer Empfangseinheit. Die Hauptinnovation unserer Arbeit ist die Anwendung von zellulären Kunststoffen für den Bau eines Arrays, wobei der Sender mit Hochspannung von ca. 1500 V angeregt wird. Geladene zelluläre Polymere werden auch Ferroelektrete oder Piezoelektrete genannt. Sie weisen ein sehr niedriges Elastizitätsmodul und dadurch eine niedrige akustische Impedanz auf, so dass auf den Einbau von Anpassschichten verzichtet werden kann.
Eine sehr niedrige mechanische Kreuzkopplung bei Ferroelektreten ermöglicht eine unabhängige Anregung einzelner Elemente, was bei Piezokompositen deutlich schwieriger wäre. Die Entwicklung der Array-Prüfköpfe wurde durch Berechnungen des Schallfeldes unterstützt, die auf Punktquellensynthese basieren. Die beabsichtigte Anwendung von Phased-Array-Prüfköpfen und des Prüfsystems sind die Durchschallung mit Fokussierung, elektronischer Scan und die Schwenkung des Einschallwinkels zur Anregung von geführten Wellen, angewandt an carbonfaserverstärkten Kunststoffen und ähnlichen Materialien. Die Anwendung von geführten Wellen bietet die Perspektive, Bauteile mit einseitiger Zugänglichkeit zu prüfen.
The peak broadening in neutron diffraction experiments on tensile specimens of pure Al (99.8%) and an Al-Mg alloy pre-deformed at different creep strains is analysed. These results are combined with the kernel angular misorientation of electron backscatter diffraction data from the creep-deformed microstructures. It is found that differently oriented grains possess different microstrains. These microstrains vary with creep strain in pure Al, but not in the Al-Mg alloy. It is proposed that this behaviour can explain the power-law breakdown in pure Al and the large creep strain observed in Al-Mg. The present findings further corroborate a description of the creep-induced dislocation structure as a fractal, predicated on previous work.
The application and benefits of Semantic Web Technologies (SWT) for managing, sharing, and (re-)using of research data are demonstrated in implementations in the field of Materials Science and Engineering (MSE). However, a compilation and classification are needed to fully recognize the scattered published works with its unique added values. Here, the primary use of SWT at the interface with MSE is identified using specifically created categories. This overview highlights promising opportunities for the application of SWT to MSE, such as enhancing the quality of experimental processes, enriching data with contextual information in knowledge graphs, or using ontologies to perform specific queries on semantically structured data. While interdisciplinary work between the two fields is still in its early stages, a great need is identified to facilitate access for nonexperts and develop and provide user-friendly tools and workflows. The full potential of SWT can best be achieved in the long term by the broad acceptance and active participation of the MSE community. In perspective, these technological solutions will advance the field of MSE by making data FAIR. Data-driven approaches will benefit from these data structures and their connections to catalyze knowledge generation in MSE.
The growth kinetics of the adsorbed layer of poly(2-vinylpiridine) on silicon oxide is studied using a leaching technique which is based on the Guiselin brushes approach. The adsorbed layer is grown from a 200 nm thick P2VP film for several annealing time periods at different annealing temperatures. Then the film is solvent-leached, and the height of the remaining adsorbed layer is measured by atomic force microscopy. At the lowest annealing temperature only a linear growth regime is observed, followed by a plateau. Here, the molecular mobility of segments is too low to allow for a logarithmic growth. At higher annealing temperatures, both linear and logarithmic growth regimes are observed, followed by a plateau. At even higher annealing temperatures, the growth kinetics of the adsorbed layer changes.
A linear growth followed by logarithmic growth kinetics is observed for short annealing time periods. For longer annealing time periods, an upturn of the growth kinetics is observed. At the highest annealing temperature, only a logarithmic growth regime is found. The change in the growth kinetics is discussed by an alteration in the structure of the adsorbed layer. Moreover, the interaction between the polymer segments and the substrate becomes weaker due to both enthalpic and entropic effects. Therefore, at high annealing temperatures the polymer segments might more easily desorb from the substrate.
This paper reports a systematic study into the effect of nitrogen on iron-catalyzed graphitization of biomass. Chitin, chitosan, N-acetylglucosamine, gelatin and glycine were selected to represent nitrogen-rich saccharides and amino-acid/polypeptide biomass precursors. The materials were pyrolyzed with an iron catalyst to produce carbons with a wide range of chemical and structural features such as mesoporosity and nitrogen-doping. Many authors have reported the synthesis of nitrogen-doped carbons by pyrolysis and these have diverse applications. However, this is the first systematic study of how nitrogen affects pyrolysis of biomass and importantly the catalytic graphitization step. Our data demonstrates that nitrogen inhibits graphitization but that some nitrogen survives the catalytic graphitization process to become incorporated into various chemical environments in the carbon product.
The obvious benefits derived from the increasing use of engineered nano-, new, and advanced materials and associated products have to be weighed out by a governance process against their possible risks. Differences in risk perception (beliefs about potential harm) among stakeholders, in particular nonscientists, and low transparency of the underlying decision processes can lead to a lack of support and acceptance of nano-, new, and other advanced material enabled products. To integrate scientific outcomes with stakeholders needs, this work develops a new approach comprising a nine-level, stepwise categorization and guidance system entitled “Knowledge, Information, and Data Readiness Levels” (KaRLs), analogous to the NASA Technology Readiness Levels. The KaRL system assesses the type, extent, and usability of the available data, information, and knowledge and integrates the participation of relevant and interested stakeholders in a cocreation/codesign process to improve current risk assessment, communication, and governance. The novelty of the new system is to communicate and share all available and relevant elements on material related risks in a user/stakeholder-friendly, transparent, flexible, and holistic way and so stimulate reflection, awareness, communication, and a deeper understanding that ultimately enables the discursive process that is needed for the sustainable risk governance of new materials.
Nickel alloys are cost intensive materials and generally classified as difficult-to-cut material. However, machining of these materials is needed especially in case of alloy 36 (1.3912), which is commonly used in mould construction for the production of fibre-reinforced composites. With regard to repair, modification and manufacturing of such components, additive manufacturing offers significant economic advantages. Nevertheless, subsequent machining steps are needed to achieve the final component contour and defined surface conditions. Dependent on the material and machining process conditions, detrimental tensile residual stresses may be the result on the machined surface, having negative impact on the component performance and safety. In this investigation, machining experiments were carried out on wire arc additive manufactured components made of alloy 36, varying the cutting speed and the feed rate. In addition, the conventional milling process (CM) was compared with a modern, hybrid machining process, the ultrasonic-assisted milling (US). The cutting forces and the surface-near residual stresses were analysed using X-ray diffraction. A significant improvement of the machinability as well as the surface integrity by using the ultrasonic assistance was observed, especially at low cutting speeds. The CM induced mainly tensile residual stresses, the US mainly compressive residual stresses.
The dataset contains raw data gathered with the ultrasonic pulse-echo method on concrete specimens. The surfaces of the measuring objects were automatically scanned point by point. Pulse-echo measurements were performed at each of these measuring points. The test specimens represent two typical testing tasks in construction industry: the detection of objects and the determination of dimensions to describe the geometry of components. By automating the measurement process, the different test scenarios are examined with a high repeatability, precision and measuring point density. Longitu- dinal and transversal waves were used and the geometrical aperture of the testing system was varied. The low-frequency probes operate in a range of up to approximately 150 kHz. In addition to the specification of the geometrical dimensions of the individual probes, the directivity pattern and the sound field characteristics are provided. The raw data are stored in a universally readable format. The length of each time signal (A-scan) is two milliseconds and the sampling rate is two mega-samples per second. The provided data can be used for comparative studies in signal analysis, imag- ing and interpretation as well as for evaluation pur- poses in different, practically relevant testing scenarios.
The prediction of porosity is a crucial task for metal based additive manufacturing techniques such as laser powder bed fusion. Short wave infrared thermography as an in-situ monitoring tool enables the measurement of the surface radiosity during the laser exposure. Based on the thermogram data, the thermal history of the component can be reconstructed which is closely related to the resulting mechanical properties and to the formation of porosity in the part. In this study, we present a novel framework for the local prediction of porosity based on extracted features from thermogram data. The framework consists of a data pre-processing workflow and a supervised deep learning classifier architecture. The data pre-processing
workflow generates samples from thermogram feature data by including feature information from multiple subsequent layers.
Thereby, the prediction of the occurrence of complex process phenomena such as keyhole pores is enabled. A custom convolutional neural network model is used for classification. Themodel is trained and tested on a dataset from thermographic in-situ monitoring of the manufacturing of an AISI 316L stainless steel test component. The impact of the pre-processing parameters and the local void distribution on the classification performance is studied in detail. The presented model achieves an accuracy of 0.96 and an f1-Score of 0.86 for predicting keyhole porosity in small sub-volumes with a dimension of (700 × 700 × 50) μm3. Furthermore, we show that pre-processing parameters such as the porosity threshold for sample
labeling and the number of included subsequent layers are influential for the model performance. Moreover, the model prediction is shown to be sensitive to local porosity changes although it is trained on binary labeled data that disregards the actual sample porosity.
Photopolymer derived carbon grows in popularity, yet the range in available feature sizes is limited. Here we focus on expanding the field to low surface to volume ratio (SVR) structures. We describe a high temperature acrylic photopolymerizable precursor with FTIR and DSC and develop a thermal inert-gas treatment for producing architected carbon in the mm scale with SVR of 1.38 x10-3 μm-1. Based on TGA and MS, we distinguish two thermal regimes with activation energies of ~79 and 169 kJ mol-1, which we reason with mechanisms during the polymer’s morphologic conversion between 300 - 500 °C. The temperature range of the major dimensional shrinkage (300-440 °C, 50%) does not match the range of the largest alteration in elemental composition (440-600 °C, O/C 0.25-0.087%). The insights lead to an optimized thermal treatment with an initial ramp (2 °C min-1 to 350 °C), isothermal hold (14h), post hold ramp (0.5 °C min-1 to 440 °C) and final ramp (10 °C min-1 to 1000 °C). The resulting carbon structures are dimensionally stable, non-porous at the μm scale, and comprise an unprecedented variation in feature sizes (from mm to μm scale). The findings shall advance architected carbon to industrially relevant scales.
The corner echo is a well-known effect in ultrasonic testing, which allows detection of surface breaking cracks with predominantly perpendicular orientation to the surface as, for example, corrosion cracks in metal pipes or shafts. This echo is formed by two planes, the surface of the crack and the surface which the crack breaks. It can also be classified as a half-skip method, since a reflection of the pulse occurs on the backwall before the reflection at the defect takes place. In combination with the diffraction from the crack tip, the corner echo also allows crack sizing. As shown in this paper, the corner reflection can be used in civil engineering for nondestructive inspection of concrete. Commercially available low frequency ultrasonic arrays with dry point contact sources generate SH transversal waves with sufficient divergence of the sound field in order to detect corner reflections. Ultrasonic line-scans and area-scans were acquired with a linear array on flat concrete specimens, and the data were reconstructed by the Synthetic aperture focusing technique. If the angles and the area of reconstruction are chosen accordingly, the corner echo reflection can be distinguished from other ultrasonic information. The corner echo can thus be used as a method for deciding whether a crack is a partial-depth crack or a full-depth crack and thus for obtaining a statement about crack depth. This paper presents corresponding experimental results obtained on concrete specimens with artificial test defects and cracks induced under controlled conditions.
Two test series were examined using nondestructive measuring methods by six independent laboratories before determining their compressive strength. The nondestructive test methods used were the rebound hammer and ultrasonic pulse velocity measurement. Two types of geometries were investigated: drilled cores and cubes. The measurement procedure for each of these datasets is conditioned to the geometry and is therefore different.
The first series consists of 20 drilled cores (approximately diameter/height = 10 cm/20 cm) from the 55-year-old Lahntal Viaduct near Limburg, Germany. After preparation in the first laboratory, the lateral surface of the drilled cores was tested with the rebound hammer using a given pattern. Every laboratory tested every drilled core at different locations.
Ultrasonic measurements in transmission were performed repeatedly at predefined points on the flat surfaces of the specimen.
The second series consisted of 25 newly manufactured concrete cubes of a mix with a target concrete strength class of C30/37. The edge length was 15 cm. Each laboratory received five specimens of this test series. Thus, contrary to the first series, each specimen was tested by only one laboratory. Two side faces of each cube were tested with the rebound hammer. In addition, ultrasonic measurements were performed by one laboratory. The time of flight was measured between the tested side faces of the rebound hammer at different positions.
For both series, rebound hammers were used to determine the R-value as well as the Q-value. The rebound hammer models within the laboratories were always the same, while they differed between the laboratories. The ultrasonic measurements took place with different measurement systems and couplants. Finally, both specimen series were tested destructively for compressive strength.
The dataset contains the raw data summarized in tabular form. In addition, relevant calculated data are included in some cases. For the ultrasonic measurements, the time of flight has already been converted into the ultrasonic velocity. Besides, in addition to the raw data of the compressive strength test (force, weight, and geometry values), the calculated compressive strengths and densities are also provided.
The glass transition behavior of thin films of poly(bisphenol A carbonate) (PBAC) was studied employing ellipsometry. The glass transition temperature increases with the reduction of the film thickness. This result is attributed to the formation of an adsorbed layer with a reduced mobility compared to bulk PBAC. Therefore, for the first time, the growth kinetics of the adsorbed layer of PBAC was investigated, prepared by leaching samples from a 200 nm thin film which were annealed for several times at three different temperatures. The thickness of each prepared adsorbed layer was measured by multiple scans using atomic force microscopy (AFM). Additionally, an unannealed sample was measured. Comparison of the measurements of the unannealed and the annealed samples provides proof of a pre-growth regime for all annealing temperatures which was not observed for other polymers. For the lowest annealing temperature after the pre-growth stage only a growth regime with a linear time dependence is observed. For higher annealing temperatures the growth kinetics changes from a linear to a logarithmic growth regime at a critical time. At the longest annealing times the films showed signs of dewetting where segments of the adsorbed film were removed from the substrate (dewetting by desorption). The dependence of the surface roughness of the PBAC surface on annealing time also confirmed that the films annealed at highest temperatures for the longest times desorbed from the substrate.
The interaction of microcroplastics (MP) with dissolved organic matter, especially humic substances, is of great importance in understanding the behavior of microplastics in aquatic ecosystems. Surface modification by humic substances plays an essential role in transport and interaction of MP with abiotic and biotic components. Previous studies on the interaction between MP and humic substances were largely based on a model compound, humic acid (Sigma-Aldrich). In our work, we therefore investigated the interaction of natural organic matter (NOM) sampled from a German surface water with low-density polyethylene particles (LDPE). Highpressure size exclusion chromatography (HPSEC) and UV/vis absorption and fluorescence spectroscopy were used to characterize the incubation solutions after modifications due to the presence of LDPE, and Raman spectroscopy was used to characterize the incubated microplastics. While the studies of the solutions generally showed only very small effects, Raman spectroscopic studies allowed clear evidence of the binding of humic fractions to MP. The comparison of the incubation of NOM and a lignite fulvic acid which also was tested further showed that specific signatures of the humic substances used could be detected by Raman spectroscopy. This provides an elegant opportunity to conduct broader studies on this issue in the future.
Using digital twins for decision making is a very promising concept which combines simulation models with corresponding experimental sensor data in order to support maintenance decisions or to investigate the reliability. The quality of the prognosis strongly depends on both the data quality and the quality of the digital twin. The latter comprises both the modeling assumptions as well as the correct parameters of these models. This article discusses the challenges when applying this concept to realmeasurement data for a demonstrator bridge in the lab, including the data management, the iterative development of the simulation model as well as the identification/updating procedure using Bayesian inference with a potentially large number of parameters. The investigated scenarios include both the iterative identification of the structural model parameters as well as scenarios related to a damage identification. In addition, the article aims at providing all models and data in a reproducibleway such that other researcher can use this setup to validate their methodologies.
Critical defects, also known as device killers, in wide bandgap semiconductors significantly affect the performance of power electronic devices. We used the methods imaging ellipsometry (IE) and white light interference microscopy (WLIM) in a hybrid optical metrology study for fast and non-destructive detection, classification, and characterisation of defects in 4H–SiC homoepitaxial layers on 4H–SiC substrates. Ellipsometry measurement results are confirmed by WLIM. They can be successfully applied for wafer characterisation already during production of SiC epilayers and for subsequent industrial quality control.
The damage mechanisms of metallic components produced by process laser powder bed fusion differ significantly from those typically observed in conventionally manufactured variants of the same alloy. This is due to the unique microstructures of additively manufactured materials. Herein, the focus is on the study of the evolution of creep damage in stainless steel 316L specimens produced by laser powder bed fusion. X-ray computed tomography is used to unravel the influence of the process-specific microstructure from the influence of the initial void distribution on creep damage mechanisms. The void distribution of two specimens tested at 600 °C and 650 °C is analyzed before a creep test, after an interruption, and after fracture. The results indicate that the formation of damage is not connected to the initial void distribution. Instead, damage accumulation at grain boundaries resulting from intergranular cracking is observed.
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.
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.
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.
NMR is becoming increasingly popular for the investigation of building materials as it is a non-invasive technology that does not require any sample preparation nor causes damage to the material. Depending on the specific application it can offer insights into properties like porosity and spatial saturation degree as well as pore structure. Moreover it enables the determination of moisture transport properties and the (re-)distribution of internal moisture into different reservoirs or chemical phases upon damage and curing. However, as yet most investigations were carried out using devices originally either designed for geophysical applications or the analysis of rather homogeneous small scale (< 10 mL) samples. This paper describes the capabilities of an NMR tomograph, which has been specifically optimized for the investigation of larger, heterogeneous building material samples (diameters of up to 72 mm, length of up to 700 mm) with a high flexibility due to interchangeable coils allowing for a high SNR and short echo times (50 - 80 m s).
Recovery is an important measure for seal applications representing to which extent the elastomer regains its initial shape after deformation and release of an applied force. Compression set (CS) indicates the degree of recovery. Ethylene propylene diene rubber (EPDM) was aged at 75 ◦C, 100 ◦C, 125 ◦C and 150 ◦C for different ageing times up to five years and compression set measurements were performed at different times after disassembly and after additional tempering. Short- and long-term recovery up to one year after release for samples aged at 125 ◦C and 150 ◦C was also studied. To assess the curvature in the Arrhenius diagram that may occur due to non-sufficiently aged specimens, a degradation-rate based model was fitted to the CS data after tempering. For each ageing temperature, two decay fit functions were proposed, each with an activation energy and a corresponding degradative process. The influence of ageing on the leak-tightness after fast small partial release is investigated and estimated through the analysis of the shift factors from time temperature superposition (TTS) of CS measurements at different times after disassembly. Shift factors of CS measurement after 1 s and after additional tempering are in good agreement.
Comparing the performance of molecular and nanoscale luminophores and luminescent microand nanoparticles and estimating achievable signal amplitudes and limits of detection requires a standardizable intensity scale. This initiated the development of the relative MESF (number of molecules of equivalent soluble fluorochromes) and ERF (equivalent reference fluorophores) scales for flow cytometry and fluorescence microscopy. Both intensity scales rely on fluorescence intensity values assigned to fluorescent calibration beads by an intensity comparison to spectrally closely matching fluorophore solutions of known concentration using a spectrofluorometer. Alternatively, the luminophore or bead brightness (B) can be determined that equals the product of the absorption cross section (σa) at the excitation wavelength (σa(λex)) and the photoluminescence quantum yield (Φpl).
Thereby, an absolute scale based on fundamental and measurable spectroscopic properties can be realized which is independent of particle size, material, and luminophore staining or labeling density and considers the sensitivity of the optical properties of luminophores to their environment. Aiming for establishing such a brightness scale for light-scattering dispersions of luminescent particles with sizes exceeding a few ten nanometers, we demonstrate how the brightness of quasi-monodisperse 25 nm, 100 nm, and 1 μm sized polystyrene particles (PSP), loaded with two different dyes in varying concentrations, can be obtained with a single custom-designed integrating sphere setup that enables the absolute determination of Φpl and transmittance and diffuse reflectance measurements. The resulting Φpl, σa(λex), imaginary parts of the refractive index, and calculated B values of these samples are given in dependence of the number of incorporated dye molecule per particle. Finally, a unitless luminescence efficiency (LE) is defined allowing for the direct comparison of luminescence efficiencies of particles with different sizes.
Photodynamic therapy (PDT) used for treating cancer relies on the generation of highly reactive oxygen species, for example, singlet oxygen 1O2, by light-induced excitation of a photosensitizer (PS) in the presence of molecular oxygen, inducing DNA damage in close proximity of the PS. Although many precious metal complexes have been explored as PS for PDT and received clinical approval, only recently, the potential of photoactive complexes of nonnoble metals as PS has been discovered. Using the DNA origami technology that can absolutely quantify DNA strand break cross sections, we assessed the potential of the luminescent transition metal complex [Cr(ddpd)2]3+ (ddpd=N,N’-dimethyl-N,N’-dipyridine-2-ylpyridine-2,6-diamine) to damage DNA in an air-saturated aqueous environment upon UV/Vis illumination. The quantum yield for strand breakage, that is, the ratio of DNA strand breaks to the number of absorbed photons, was determined to 1–4%, indicating efficient transformation of photons into DNA strand breaks by [Cr(ddpd)2]3+.
The embrittlement of metallic alloys by liquid metals leads to catastrophic material failure and severely impacts their structural integrity. The weakening of grain boundaries by the ingress of liquid metal and preceding segregation in the solid are thought to promote early fracture. However, the potential of balancing between the segregation of cohesion-enhancing interstitial solutes and embrittling elements inducing grain boundary decohesion is not understood. Here, we unveil the mechanisms of how boron segregation mitigates the detrimental effects of the prime embrittler, zinc, in a Σ5 [0 0 1] tilt grain boundary in α −Fe (4 at.% Al). Zinc forms nanoscale segregation patterns inducing structurally and compositionally complex grain boundary states. Ab-initio simulations reveal that boron hinders zinc segregation and compensates for the zinc induced loss in grain boundary cohesion. Our work sheds new light on how interstitial solutes intimately modify grain boundaries, thereby opening pathways to use them as dopants for preventing disastrous material failure.