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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.