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Guaranteeing safety and security of citizens requires a significant effort and innovative tools from national and international agencies and governments, especially when it comes to the field of explosives detection. The need to detect Improvised Explosive Devices (IEDs) and Home-made Explosives (HMEs) at a point of suspicion, has grown rapidly due to the ease with which the precursors can be obtained and the reagents synthesised. The limited availability of immunoanalytical tools for HME detection presents an opportunity for the development of new devices, which enable a rapid detection and recognise the target analyte with high specificity and sensitivity. In this work, we introduce an optical biosensor for highly specific and sensitive HME detection. The immunoassay system is placed in a hydrogel environment permeable to the analyte and transparent to light interrogating the fluorescently labelled antibodies. The readout of the immunoanalytical system is realized with Supercritical Angle Fluorescence (SAF), an advanced microscopy technique. To accomplish this, we made use of recent, commercial high resolution (< 22 µm) Liquid Crystal Display 3D printers to fabricate a parabolic optical element with high refractive index (RI>1.5) and transmission values (>90%) from photo-resin. Aiming at a new generation of sensors, which not only can meet the requirements of trace detection, but can also be used for substance identification, the combination of immunoanalytical recognition with SAF detection offers a modularity and versatility that is principally well suitable for the measurements of target analytes at trace levels.
Bei Geräten und Maschinen zur bestimmungsgemäßen Verwendung in explosionsgefährdeten Bereichen gemäß 2014/34/EU muss in der europäischen Union eine Zündgefahrenbewertung durchgeführt werden. Dabei müssen unter anderem die Gefahren von nichtelektrischen Zündquellen betrachtet werden, zu denen auch die mechanischen Schlagvorgänge gehören.
Bei mechanischen Schlagvorgängen kommt es infolge des Zusammenstoßes zweier Werkstücke bzw. Bauteile zu einer Umwandlung der kinetischen Energie. Dabei erhöht sich die Temperatur der Werkstoffe an der Kontaktstelle und es kommt unter Umständen zu einem Abtrennvorgang kleiner Partikel erhöhter Temperatur. Sowohl die heißen Kontaktstellen (Zündquelle "heiße Oberflächen") als auch die abgetrennten Partikel (Zündquelle "mechanisch erzeugte Funken") können eine wirksame Zündquelle für ein explosionsfähiges Gasgemisch darstellen.
Zur Festlegung von Grenzwerten wurden in der Norm DIN EN ISO 80079-36:2016 die Gasgemische anhand ihrer Explosionsgruppe klassifiziert und zu jeder Gruppe die maximale Energie des Schlagvorgangs festgelegt, unter derer die Entstehung einer wirksamen Zündquelle als unwahrscheinlich angenommen werden kann.
Weitere Festlegungen von Grenzwerten für die kinetische Schlagenergie und geeignete Werkstoffpaarungen finden sich u.a. in der DIN EN 1755 (ex-geschützte Flurförderzeuge) und in der DIN EN 14986 (ex-geschützte Ventilatoren).
The global plastic industry relies on fossil-based materials, presenting environmental challenges. A sustainable polymer namely poly(limonene carbonate) (PLimC), made of limonene and CO2 as two monomers from non-food sources, shows advances in various applications where additives such as flame retardants (FRs) are crucial to comply with fire safety measures.
The variety of FRs is wide, and therefore the approach involved conducting a comparative study of four different halogen-free flame retardant systems that are conventionally used in polycarbonates and polyolefins to understand which FR enhances the flame resistance of PLimC most effectively. The primary task of the project is to conduct experimental evaluations to analyze the thermal properties, flammability, and fire behavior of each system. This data will offer valuable insights towards the advancement of safer and more sustainable materials.
Skłodowska, Anna Maria ; Lay, Vera ; Baensch, Franziska ; Niederleithinger, Ernst ; Kühne, Hans-Carsten
To safely dispose of nuclear waste in underground facilities, engineered barrier systems are needed to seal shafts and galleries. The material used in these barriers must be adapted to the host rock parameters. Shrinking and cracking must be avoided to provide a barrier with almost zero permeability. For repositories in salt rock environments, several types of salt concrete (SC) are possible construction materials.
Within the project SealWasteSafe, we compared the behavior of an innovative alkali-activated material (AAM) with standard SC in their hydration and hardening phase. To monitor the microstructural changes within the two materials SC and AAM, acoustic emission (AE) signals have been recorded for up to ~250 days on 340-liter-cubic specimens.
The phenomenon of AE is defined as the emission of elastic waves in materials due to the release of localized internal energy. Such energy release can be caused by the nucleation of micro-fracture, e.g., in concrete while curing or when exposed to load. The occurrence of AE events gives first rough indications of microstructural changes and potentially occurring cracking and thus, provides insights for structural health monitoring (SHM).
The results show, that for the first 28 days after casting, less AE activity was detected in the AAM compared to SC. After 61 days, in the AAM material, the number of AE events exceeded those observed in the SC. However, the majority of the AE detected and located in AAM was related to surface effects, and not to microstructural changes or occurring cracks within the bulk volume. Additionally, the source location analysis indicated, that despite lower activity in SC, we observed some clustering of the events. In contrast, in AAM, the activity inside the specimen is randomly distributed over the whole volume. The monitoring results help to estimate the material’s sealing properties which are crucial to assess their applicability as sealing material for engineered barriers.
The crucial part of nuclear waste storage is the construction of sealing structures made of reliable, well-understood, and safe materials. Within the SealWasteSafe project, we compared the performance of an innovative alkali-activated material (AAM) and standard salt concrete (SC), as potential materials for sealing structures for nuclear waste repositories. Two 340-liter-cubic specimens were studied for up to ~250 days by a multisensory monitoring setup. Specifically, the long-term acoustic emission monitoring aimed to analyze the development of microstructural changes within materials.
The monitoring analysis showed fewer acoustic emission events in AAM compared to SC in the first 61 days. After approximately two months of monitoring, the number of AE events in AAM significantly exceeded the number of events in SC. The analysis showed, however, that the increased AE activity was mainly caused by surface effects of the AAM material and not by the formation of cracks within the material.
This contribution presents the use of acoustic emission analysis, both in the time and frequency domains, for monitoring and characterization of materials with potential use as engineering barriers for nuclear waste repositories.
Skłodowska, Anna Maria ; Lay, Vera ; Baensch, Franziska ; Niederleithinger, Ernst ; Kühne, Hans-Carsten
One of the major tasks in nuclear waste management is to design safe and reliable sealing structures for radioactive waste repositories. Particularly for salt as a host rock, engineered barrier systems for underground waste disposal must be constructed of well-understood (cementitious) materials that will sustain environmental conditions and ensure high durability.
Within the SealWasteSafe project, we studied two materials with a potential for sealing structures for nuclear waste repositories: an innovative alkali-activated material (AAM) and standard salt concrete (SC). To analyze the development of microstructural changes within the materials, we monitored microseismicity (aka acoustic emission monitoring) occurring during the hardening and setting period in two 340-liter-cubic specimens for up to ~250 days.
The monitoring results showed, that in the first 61 days, fewer events occurred in AAM compared to SC. After this time the number of events in AAM sharply increased and significantly exceeded those observed in SC. However, the source localization analysis revealed that the increase of microseismicity in AAM material was not related to the formation of macro-cracks within the material but was mainly caused by the surface effects. Accompanying analysis of the test specimens with additional methods (such as e.g., X-ray CT) proved that no macro-cracks were observed inside the AAM specimen. Further analysis in the time and frequency domains helped to characterize the tested materials and to estimate their potential to be used for engineered barriers in nuclear waste repositories.
Overall, our study shows the potential of microseismicity monitoring for feasibility studies and quality assurance in a broad range of applications, also in structural health monitoring.
Standardised methods need validation. The main validation parameters like trueness, repeatability and intermediate precision and reproducibility are presented. Furthermore, different methods for the validation are disussed: (certified) reference materials, representative testing materials and interlaboratory comparisons. At last, the need of proficiency testing is stressed.
Revealing surface functionalities of micro- and nanoplastic particles’ surface by means of XPS
(2024)
Over the last 20 years, many researchers, politicians, and citizens themselves have become increasingly aware of the growing plastic problem of our time. Inadequate recycling concepts, collection points, and careless dumping of plastic products in the environment lead to an accumulation of plastic. External weather influences can cause these to degrade and fractionate, so that today microplastics (1-1000 µm, ISO/TR 21960:2020) [1] of different polymer materials can be detected in all parts of the world.
The precautionary principle applies to microplastics. The particles can break down further to form nanoplastics (<1 µm, ISO/TR 21960:2020) [1]. Whether microplastics or nanoplastics pose a toxicological hazard is being investigated in a variety of ways. Valid results are still pending, however, investigations into the frequency, transport, possible sinks and entry paths must be taken into account. This is why monitoring of microplastics is already required in the revision of the Drinking Water Framework Directive [2]. The same is still pending in the final version of the revision of the Waste Water Framework Directive this year, but is expected.
Nanoplastics are particularly under discussion for having a toxic effect on humans and animals, as these particles are small enough to be absorbed by cells. For targeted toxicological studies, it is important to have test and reference materials that resemble the particles found in the environment. To mimic environmental samples, these materials should also have an irregular shape and show aging at the surface, which can be detected with XPS or SEM/EDS.
BAM in collaboration with the EMPIR project "PlasticTrace" works on a reference material candidate of nano-sized polypropylene (nano-PP) [3]. The nano-PP vials were tested for homogeneity with PTA and further characterized with bulk and surface-sensitive techniques. An SEM image and a corresponding XPS spectrum are presented in Figure 1. Raman measurements as well as XPS indicate an aged surface.
Wasserstoff stellt einen potenziellen Energieträger für den großskaligen Import von Energie nach Europa dar. Von seinen verschiedenen Speicherformen eignet sich hierfür insbesondere verflüssigter Wasserstoff, mit dem sich auf gleichem Volumen deutlich mehr Energie speichern lässt als bei der druckbasierten Speicherung. Verflüssigter Wasserstoff wird bei minus 253°C gespeichert und muss für dessen Transport lange bei dieser niedrigen Temperatur gehalten werden. Dies stellt besondere Herausforderungen an die thermische Isolation von Tanks. Der Erforschung nachhaltiger, kosten- und energieeffizienter sowie sicherer thermischen Isolationen wird im NICOLHy Projekt, unter Leitung der BAM, nachgegangen.
Small-area XPS analysis is one of the most popular and powerful methods for analysing the surface of features in the micro-range. When measuring microstructures, the ques-tion arises whether the measuring point is really located at the point intended to be ana-lysed. Information in a measured spectrum might originate within the field of view (FoV) on the surface of the sample, from outside the FoV, or even from inherent contamination. To ensure that small structures can be measured correctly regardless of user and instru-ment, certain instrument and sample settings must be known and selected correctly: beam and aperture size as well as the aperture settings and the approximate dimensions of the structure to be analysed. This is the only way to ensure that the information in the spectrum originates only from the FoV on the analysed structure.
To test the performance of the XPS instruments, a dedicated test material was developed that consists of a gold surface on which 8 circles and 8 squares of chrome are incorpo-rated using a masking process, so that the Au substrate and the Cr structure surfaces are in the same surface plane. In order to be able to test as many as possible instruments from different manufacturers, the structures have been designed with a size ranging from 300 µm down to 7 µm. The layout of the test material has been optimised in regard of the handling. The structures are arranged along lines instead of a circumference, marking arrows around the smaller structures (≤50 µm) are added, and the lithography mask is optimised regarding edge and diffraction effects. Furthermore, the manufacturing process was changed from electron-beam deposition to mask lithography due to costs reasons. The structures on the test material were measured with a metrological SEM to determine their accurate dimensions and check the repeatability of the manufacturing process. XPS investigations with a Kratos AXIS Ultra DLD and an ULVAC-Phi Quantes demonstrates the suitability of this new test material for measuring the analysed area.
Ni-Fe oxide nanoparticles have gained a lot of interest because of their high activity in the oxygen evolution reaction (OER) which is crucial for water splitting. [1] Although there have been great efforts in the last years, the understanding of the synergistic effect between Fe and Ni is still under discussion.
Therefore, we prepared different Ni-Fe oxide nanoparticles with different compositions from pure iron oxide to pure nickel oxide adapting a known procedure. [2,3] Size and morphology of the nanoparticles depend on the composition which was shown with Transmission Electron Microscopy (TEM). The compositions of the nanoparticles were measured with a comparative approach using X-ray Photoelectron Spectroscopy (XPS), Hard X-ray Photoelectron Spectroscopy (HAXPES), and Energy Dispersive X-Ray Spectroscopy (EDS) coupled with the TEM providing detailed chemical information of the nanoparticles in different sample regions. EDS reveals that the different sample regions are dominated by one of the components, Fe or Ni, but a slight mixing between the components can be found (see Figure 1), which was confirmed with X-ray Diffraction (XRD). XPS indicates the enrichment of Fe at the sample surface, while HAXPES and EDS data agree on the stoichiometry of the bulk. High-resolution XPS and HAXPES exhibit some differences in the valence states of Fe and Ni, whereas Ni seems to be easier to reduce than Fe. Further investigations combining these different techniques and additionally Secondary Ion Mass Spectrometry (ToF-SIMS) are ongoing by using in situ approaches and coupling cyclic voltammetry to the analytical techniques.
Bei Geräten und Maschinen zur bestimmungsgemäßen Verwendung in explosionsgefährdeten Bereichen gemäß 2014/34/EU muss in der europäischen Union eine Zündgefahrenbewertung durchgeführt werden. Dabei müssen unter anderem die Gefahren von nichtelektrischen Zündquellen betrachtet werden, zu denen auch die mechanischen Schlagvorgänge gehören.
Bei mechanischen Schlagvorgängen kommt es infolge des Zusammenstoßes zweier Werkstücke bzw. Bauteile zu einer Umwandlung der kinetischen Energie. Dabei erhöht sich die Temperatur der Werkstoffe an der Kontaktstelle und es kommt unter Umständen zu einem Abtrennvorgang kleiner Partikel erhöhter Temperatur. Sowohl die heißen Kontaktstellen (Zündquelle "heiße Oberflächen") als auch die abgetrennten Partikel (Zündquelle "mechanisch erzeugte Funken") können eine wirksame Zündquelle für ein explosionsfähiges Gasgemisch darstellen.
Zur Festlegung von Grenzwerten wurden in der Norm DIN EN ISO 80079-36:2016 die Gasgemische anhand ihrer Explosionsgruppe klassifiziert und zu jeder Gruppe die maximale Energie des Schlagvorgangs festgelegt, unter derer die Entstehung einer wirksamen Zündquelle als unwahrscheinlich angenommen werden kann.
Weitere Festlegungen von Grenzwerten für die kinetische Schlagenergie und geeignete Werkstoffpaarungen finden sich u.a. in der DIN EN 1755 (ex-geschützte Flurförderzeuge) und in der DIN EN 14986 (ex-geschützte Ventilatoren).
The main properties and main methods which are needed for the physico-chemical characterisation of graphene related 2D materials are discussed. As expample for standardization, protocols for the measurement of the chemical composition with XPS are discussed. The results of an interlaboratory comparisons led to new recommendations for the reliable measurments protocols.
The key for a transition into clean energy sources is based on the construction of safe energy infrastructure, such as transportation pipelines for Hydrogen. Duplex Stainless Steels (DSS) are an essential component used nowadays in the construction of transportation pipelines because of their many distinctive qualities. The choice of DSS for a particular hydrogen application mainly depends on its susceptibility level to Hydrogen Embrittlement (HE) or Hydrogen Assisted Cracking (HAC). Since the 20th century, the literature indicates three factors that must be considered: the microstructure of the alloy steel, the hydrogen concentration, and the mechanical load. Several mechanisms have been also proposed to describe the occurring microscale processes behind HE or HAC, and these include metastable phase transformation, Hydrogen Enhanced Localized Plasticity (HELP), and Hydrogen Enhanced Decohesion (HEDE).
The following contribution describes the path to ascertain if DSS is suitable for high-pressure gaseous hydrogen applications. The interplay between several critical factors that result in HAC was examined using high-pressure gaseous hydrogen charging, Electron Backscatter Diffraction (EBSD), and hydrogen concentration measurements using Carrier Gas Hot Extraction (CGHE). It was determined whether the strain-induced martensitic transformation of the austenite was present in a DSS 1.4462 (DSS2205) in-service pipe and in samples of freshly charged DSS 1.4462. In comparison to the common electrochemical charging described broadly in the literature, no major direct martensitic phase transformation of the austenite phase under a high-pressure hydrogen environment was observed. As for future experiments, the intention is to analyse the impact of high-pressure gaseous hydrogen on the welded components of this grade, and under mechanical load via the hollow specimen technique.
Fire-induced spalling of normal strength concrete with different types of blended Portland cement
(2024)
The cement industry is looking to reduce its overall CO2 footprint. Greener manufacturing can be achieved by the introduction of more clinker-reduced cements. Concrete exposed to fire tends to show explosive spalling caused by thermomechanical and thermohydraulic processes. It is therefore essential to determine how concretes with clinker-reduced cements behave under fire exposure, especially for concretes containing calcined clays, as these are expected to be the supplementary cementitious material of the future. In this paper, normal strength concretes with four different cements (CEM I, CEM II/A-LL, CEM III/A and CEM II/B-Q) were examined for their fire-induced spalling behaviour. In addition, a mix with PP fibres was investigated for each concrete. The experiments were conducted on ring-restrained cylindrical specimens exposed to the hydrocarbon fire curve. The results showed that the cement type influences spalling behaviour. Samples with CEM I spalled the least, followed by CEM II/A-LL and CEM III/A. Finally, samples with CEM II/B-Q showed the most severe damage. It was found that the spalling behaviour of different concretes correlates with the moisture content before exposure to fire, meaning that higher moisture content leads to higher spalling susceptibility. The use of 2 kg/m³ PP fibres completely inhibited spalling regardless of the cement type used and therefore remains a successful avoidance strategy.
To accelerate the transition to a low-carbon economy while exploiting existing infrastructure, hydrogen can be injected to the natural gas network. However, many technical and regulatory gaps should be closed, and adaptations and investments made to ensure that multi-gas networks across Europe will be able to operate in a reliable and safe way while providing a highly controllable gas quality and required energy demand. The SHIMMER project aims to enable a higher integration and safer hydrogen injection management in multi-gas networks by contributing to the knowledge and better understanding of hydrogen projects, their risks, and opportunities.
Graphene and related 2D materials (GR2Ms) are now entering an exciting phase of commercialization and use in products. Graphene nanoplatelets (GNPs) can be obtained in rather large quantities, but the properties of these industrially produced powders can vary depending on the production method, and even from batch to batch. Understanding and optimizing the surface chemistry of GNPs, modified through chemical functionalization processes is crucial, because it affects their dispersibility in solvents and matrices for the purpose of embedding them into real-world products. Therefore, reliable and repeatable measurements of the surface chemistry of functionalized GNPs are an important issue for suppliers as well as users of these materials. To address these concerns, international documentary ISO standards for measurement methodologies are under development which incorporate protocols that are becoming widely accepted in the community.
Recently, it was shown that pelletizing led to lower average O/C atomic ratios than those measured for powders [1]. In another study, the influence of the morphology on the degree of functionalization was shown [2]. As expected, a higher degree of functionalization was detected for smaller GNPs. The functionalization was located at the outermost surfaces of the GNPs by comparing experiments using photoelectron with soft (Al Kα, 1.486 keV) and hard X-rays (Cr Kα, 5.405 keV). Therefore, it is important for those using GNPs to understand both the physical and chemical properties of these particles, when considering their use in different applications.
The next step for reliable characterization protocols was the realization of an interlaboratory comparison under the auspices of VAMAS (Versailles Project on Advanced Materials and Standards) with 22 participating laboratories from all over the world. Samples of oxygen-, nitrogen-, and fluorine- functionalized GNPs were provided to the participants along with a measurement protocol. Participants were asked to prepare the samples as powders on a tape, powders in a sample holder recess, or as pellets. The lower measured O/C ratio reported for pelletized samples [1] was confirmed. The lowest scattering of the results was observed for the powders measured in the recess (Fig. 1). Furthermore, an influence of the humidity on the results was observed.
Interlaboratory comparisons (ILCs) are an important tool for the validation of characterisation methods, and, herwith, a prerequisite for standardisation. The "Versailles Project on Advanced Materials and Standards" offers a framework for performing such ILCs: (i) TiO2 nanoparticles using ToF-SIMS, and (ii) the chemical composition of functionalized graphene using XPS. The results of both ILCs underline the importance of sample preparation for the measured results.
Wir stellen unseren Ansatz und unsere Methodik zur Simulation von Piping-Erosion vor, welche während des Installationsprozesses von Suction Bucket Fundamenten für Offshore-Windkraftanlagen auftreten kann und ein kritisches Versagen des Installationsprozesses darstellt. Wir zeigen die Ergebnisse mehrere Simulationen und analysieren die hydrodynamischen und Kontaktkräfte, die auf das granulare Medium wirken, sowie die Druckdifferenz der flüssigen Phase. Solche Simulationen können zum besseren Verständnis von Piping-Erosion und letztendlich zu dessen Verhinderung beitragen.