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Eingeladener Vortrag
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The electrochemical behavior of 4-phenylurazole (Ph-Ur) was studied and the latter was used as a molecular anchor for the electrochemical bioconjugation of tyrosine (Y). Cyclic voltammetry (CV) and controlled potential coulometry (CPC) allowed to generate in situ from phenylurazole the PTAD (4-phenyl-3H-1,2,4-triazole-3,5(4H)-dione) species on demand for tyrosine electrolabeling. To evaluate the performance of tyrosine electrolabeling, coulometric analyses at controlled potentials were performed on solutions of phenylurazole and the phenylurazole-tyrosine mixture in different proportions (2:1, 1:1, and 1:2). The electrolysis of the phenylurazole-tyrosine mixture in the ratio (1:2) produced a charge of 2.07 C, very close to the theoretical value (1.93 C) with high reaction kinetics, a result obtained here for the first time. The products obtained were identified and characterized by liquid chromatography coupled to high-resolution electrospray ionization mass spectrometry (LC-HRMS and LC-HRMMS). Two products were formed from the click reactions, one of which was the majority. Another part of this work was to study the electrochemical degradation of the molecular anchor 4-phenylazole (Ph-Ur). Four stable degradation products of phenylurazole were identified (C7H9N2O, C6H8N, C6H8NO, C14H13N4O2) based on chromatographic profiles and mass spectrometry results. The charge generated during the electrolysis of phenylurazole (two-electron process) (2.85 C) is inconsistent with the theoretical or calculated charge (1.93 C), indicating that secondary/parasitic reactions occurred during the electrolysis of the latter. In conclusion, the electrochemically promoted click phenylurazole-tyrosine reactions give rise to click products with high reaction kinetics and yields in the (1:2) phenylurazole-tyrosine ratios, and the presence of side reactions is likely to affect the yield of the click phenylurazole-tyrosine reaction.
Currently, there is a growing interest in the study of environmental degradation pathways of organic contaminants such as pesticides, with the objective to better understand their potential risk for environmental systems and living organisms. In this context, DFT (conceptual density functional theory) and predictive methods may systematically be used to simplify and accelerate the elucidation of environmental degradation. We report herein the electrochemical behavior/degradation of the carbendazim (CBZ) fungicide widely used to treat cereal and fruit crops. Oxidative degradation of CBZ was studied using an electrochemical flow-through cell directly coupled to a mass spectrometer for rapid identification of CBZ degradation products. The structural elucidation of CBZ oxidation products was based on retention time, accurate mass, isotopic distribution and fragmentation pattern by using LC-HRMS an LC-HRMS2. The most important chemical reactions found to occur in the transformation of CBZ were hydrolysis and hydroxylation. EC-LC-MS and EC-MS analysis has made it possible to highlight the identification of degradation products of CBZ. In addition to previously known transformation products common to those observed during environmental degradation (monocarbomethoxyguanidine, benzimidazole-isocyanate, 2-aminobenzimidazole, hydroxy-2-aminobenzimidazole, hydroxycarbendazim, CBZ-CBZ dimer), two new degradation products were identified in this work: a quinone imine and a nitrenium ion. Electrochemistry mass spectrometry hyphenated techniques represent an accessible, rapid and reliable tool to elucidate the oxidative degradation of CBZ, including reactive degradation products and conjugates.
Data-driven materials design aims to predict and optimize material properties, such as stability and thermal conductivity, which are influenced by vibrational behavior. Approaches like DFT are computationally demanding and have limitations for phonon calculations. Machine learning-driven interatomic potentials (MLIP), like the Gaussian approximation potential (GAP), offer a more efficient alternative.1–8 We developed a Python workflow to automate MLIP generation using the Materials Project database.9 DFT computations, MLIP fitting and benchmark steps are automated.10,11 This approach accelerates phonon calculations and supports testing different data generation strategies and hyperparameters, and further validation12 is planned. Our goal is to provide open-source code and share these potentials.
Resistance to carbonation and chloride migration are critical durability properties in cementitious construction materials. The ingress of CO2 and chlorides can lead to concrete deterioration and reinforcement corrosion, underscoring the importance of ensuring high resistance to these durability-reducing factors. Traditional methods, such as determinating the carbonation coefficient using standard procedures, are time-consuming and resource-intensive. These tests typically require 42 days of preconditioning, followed by 70 days before the final results can be determined using a phenolphthalein test, for a total duration of 112 days. In addition, some test chambers can only accommodate four samples at a time.
In this study, we investigate whether 1H NMR relaxometry can effectively predict not only the carbonation resistance, KAC,3%, but also the chloride migration coefficient, DRCM, and the compressive strength, fc, of concrete, providing a method that could potentially streamline and accelerate the material development process by directing us quickly to potentially well-suited formulations. We performed measurements on non-carbonated fully saturated concrete and mortar samples at 28, 56, and 92 days using the NMR tomograph at BAM (8.9 MHz). Notably, the NMR measurements taken at 28 days showed no significant differences, suggesting that this timeframe is sufficient for meaningful results. The samples analyzed were drill cores, each 70 mm in diameter and approximately 120 mm in height. The NMR features we focused on included the initial amplitude E0, the x and y values of the dominant T2 relaxation time, and the logarithmic mean of the T2 relaxation time distribution. Another key feature was the surface relaxivity, which was determined by comparing the NMR curves with results from mercury intrusion porosimetry. We examined the correlation of these NMR features with the aforementioned durability properties, which were determined in a laboratory on sister samples using standard procedures. No chloride migration tests were performed on the mortar samples, and the carbonation procedure was carried out unter atmospheric conditions.
The preliminary results show that the correlation factors for the NMR features with the carbonation coefficients of concrete were particularly remarkable. The strongest correlations were observed for the dominant relaxation time and the logarithmic mean, with values approaching 1. The preliminary results also indicate that there are high correlations between the compressive strength and amplitude-related features. In contrast, no strong correlations are observed for the DRCM. Although the results related to the mortar samples are still being analyzed, these initial correlations suggest that 1H NMR relaxometry could be a valuable tool for early assessment of material properties. Furthermore, the rapid and non-destructive nature of NMR measurements, requiring only a few minutes per sample, suggests that this technique has the potential to significantly accelerate the process of evaluating durability properties in cementitious materials. This capability also paves the way for the use of NMR features as input for AI-driven predictive models.
In clinical magnetic resonance imaging, non-specific Gd-based contrast agents (GBCAs) are frequently used to improve image quality. However, the interaction of GBCAs with tissue components is not yet fully understood. Many diseases, including inflammation, fibrosis, and tumor invasion, are associated with characteristic changes of the extracellular matrix (ECM). The ECM is a three-dimensional scaffold that embeds the cells of all mammalian tissues. It is composed of structural proteins (e.g., collagen, elastin) and proteoglycans, which consist of glycosaminoglycans (GAGs) covalently bound to a protein core. GAGs are characterized by their ability to form complexes with cations such as lanthanides. Thus, GAGs could be a potential binding partner for GBCAs as a whole or for dechelated Gd. Laser ablation inductively coupled plasma time-of-flight mass spectrometry (LA/ICP-ToF-MS) was used to investigate the uptake and distribution of different GBCAs in spheroids mimicking biological tissue and exhibiting different ECM expressions. Spheroids from Chinese hamster ovary (CHO) cells and GAG-depleted CRL-2242 cells were incubated with gadolinium chloride and various linear and macrocyclic GBCAs. Although all spheroids were exposed to identical Gd concentrations, differences in the amount of Gd taken up were observed. Gadolinium chloride is more strongly absorbed and accumulates mainly in the outer regions of the spheroids. In contrast, after incubation with linear and macrocyclic GBCAs, Gd is detected in the interior of both types of spheroids. Furthermore, differences in the Gd amount were found depending on the GBCA used. However, further studies are needed to elucidate such complex interactions, also using other (bio)analytical techniques.
Optimization Framework for Powder Bed 3D Printed Concrete Structures under Various Constraints
(2024)
The fusion of 3D printing with concrete has transformed large scale construction, accelerating creative design possibilities. In recent years, multiple printing techniques have been developed and are still under investigation. The powder bed technique enables overhang constructions, thereby increasing design flexibility. To maximize the advantages of those printing techniques, a holistic approach is required taking topology optimization through finite element analysis into account. The challenge is to consider a range of constraints, from material to geometrical to manufacturing.
The current research focuses on the development of a holistic approach to large-scale 3D powder bed printed concrete structure optimization, navigating the in-tricacies of constraints, leveraging the advantages of powder-based printers, and integrating essential information from material tests. A workflow starting from geometry input and ending with printing instructions is derived, minimizing user interaction, and offering fast and reliable results for different structures. Starting from a geometric model of the global design with the required load cases, the geometry is optimized with respect to reduce the mass and thus CO2 emissions. Thereby, the topology optimization includes various constraints: stress con-straints (mitigating tension and limit compressive stress using Drucker-Prager based models), geometric constraints (preserving specific surfaces from optimi-zation), and manufacturing constraints (controlling member size and avoiding trapped powder). Different objective functions, like minimizing compliance or mass are considered in this study. The process receives input from upstream ma-terial tests, offering insights into strength, stiffness and possible anisotropy. This integration of material testing enhances the accuracy and reliability of the opti-mization, aligning the design with real-world behavior of 3D printed concrete. An important aspect of the workflow is the segmentation of the optimized global structure into substructures, aligning with the size limitations of the 3D powder-bed printer. As final output of the developed workflow, printer specific fabrica-tion instructions are generated for each substructure. The developed optimization framework is demonstrated in the design of a multiperson shading element.
Over the last 20 years, many researchers, politicians and citizens have become increasingly aware of the growing plastic problem of our time. A lack of recycling concepts and plastic collection points as well as careless dumping lead to accumulation of plastic products in the environment. Natural weathering can cause these plastics to degrade and fractionate, meaning that microplastics (1 1,000 µm, ISO/TR 21960:2020) and nanoplastics (< 1 µm, ISO/TR 21960:2020) of various synthetic polymer materials can now be detected in all parts of the world. Whether microplastics or nanoplastics pose a toxicological hazard is being investigated in a variety of ways. Valid results are still pending. However, the EU precautionary principle applies to micro- and nanoplastics. Monitoring of microplastics is already required in the revision of the Drinking Water and Wastewater Framework Directive.
Reliable monitoring of rivers can be carried out by sampling with sedimentation boxes and microplastic detection by using thermal extraction desorption gas chromatography/mass spectrometry (TED-GC/MS) in routine operation (Figure 1). The river Rhine was sampled for microplastic masses at three different sampling locations over a period of one year and in addition the Danube at randomized sampling locations The TED-GC/MS results showed that various synthetic polymers frequently produced in industry, such as polyethylene, polypropylene or polystyrene as well as the tire compound styrene-butadiene rubber were found. The work not only shows a possible workflow for monitoring concepts, but also provides information on environmentally relevant concentrations of microplastics and tire components in surface waters. This in turn is necessary for ecotoxicological studies.
Der One-Health-Ansatz hat die Gesundheit von Mensch, Tier und Umwelt im Fokus. Dazu ist eine interdisziplinäre Zusammenarbeit von Akteuren aus Human- und Veterinärmedizin sowie den Umweltwissenschaften notwendig. Ein Ineinandergreifen von methodischen Ansätzen und der Analytik wird angestrebt.
Im Zuge der anstehenden Novellierung (2924) der EU-Kommunalabwasserrichtlinie (91/271/EWG) wird die Umsetzung eines One-Health-Ansatzes bereits adressiert. Dazu gehört zum einen der Ausbau und die Prozessüberwachung einer vierten Reinigungsstufe in Klärwerken. Zum anderen ist europaweit die Infrastruktur einer Abwassersurveillance zur Überwachung von Krankheitserregern zu gewährleisten. Dies wird aktuell in Deutschland mit dem Projekt AMELAG ("Abwassermonitoring zur epidemiologischen Lagebewertung") mit zwei Probennahmen pro Woche auf ca. 170 Kläranlagen umgesetzt.
Im Rahmen der weltweiten Corona-Pandemie fordert die EU-Kommission seit März 2021 die systematische Erfassung und Überwachung von SARS-CoV-2 über das Abwasser, welche der Entscheidungsfindung bezüglich bevölkerungsbezogener Maßnahmen dienen soll. Hierbei können Trendanalysen für die epidemiologische Lagebewertung abgeleitet werden, sofern ein großer Anteil des kommunalen Abwassers der Bevölkerung durch das Monitoring abdeckt wird. Die Datenerhebung erfolgt somit unabhängig vom individuellen Test- und Meldeverhalten der Bevölkerung. Eine bedeutende Herausforderung bei der Bestimmung der Gensequenzen mittels polymerase chain reaction (PCR) stellen standortabhängige Faktoren des Einzugsgebietes sowie Schwankungen der Durchflussrate und der Abwasserzusammensetzung dar. Zu den möglichen Ursachen zählen Verdünnungseffekte durch Regen- und Schmelzwasser, Größenunterschiede des kommunalen Entwässerungssystems, Veränderungen der Demografie und Zuflüsse von Indirekteinleitern. Um eine verbesserte Korrelation quantitativ ermittelter Genkopien des SARS-CoV-2 aus der jeweiligen Abwasserprobe mit dem Anteil der infizierten Bevölkerung zu erzeugen, ist eine Normalisierung der PCR Daten vorzunehmen. Neben relativ einfach zu ermittelnden physikalischen Größen, wie der mittleren Durchflussrate oder der Leitfähigkeit, die Aufschlüsse über den Anteil von Fremd- und Regenwasser ermöglichen, können auch anthropogene Marker, wie Spurenstoffe und Surrogatviren im Abwasser, als direkte Indikatoren für menschliche Fäkalien aus dem häuslichen Abwasser dienen.
Im Folgenden soll eine vergleichende Untersuchung von vier Spurenstoffen ‒ Koffein (CAF), Carbamazepin (CBZ), Diclofenac (DCF), Isolithocholsäure (ILA) ‒ sowie einem Surrogatvirus (SV) (Pepper mild mottle virus (PMMoV) oder CrAssphage), die Eignung der jeweiligen Paramater als Normalisierungsfaktoren analysieren. Die Untersuchung fand an 19 Standorten über drei Monate im Rahmen einer Studie aus dem Projekt ESI-CorA statt.
Germany has set itself the task to become a world leader in the field of green hydrogen technologies and is promoting the transition to a hydrogen economy. The H2Mare flagship project is exploring the offshore production of green hydrogen and other power-to-X products. One of the most important goals is the safe and cost-efficient operation of offshore infrastructures, where a service life of at least 25 years is aimed. However, the corrosive environment towards metallic materials presents challenges in marine areas. The atmosphere at one location could be affected by the distance to the sea level and does not have the same corrosivity for all exposed kinds of materials. The creation of an atmosphere corrosion atlas for marine environments by weathering campaigns aims to close this gap. Operators of offshore structures can use the data to estimate the corrosivity of the atmosphere on the construction site. This allows planning to be optimized in terms of platform safety as well as maintenance costs.
Die von der Europäischen Kommission im Jahr 2021 empfohlene, systematische Abwasserüberwachung mittels PCR-Techniken wird als ein wirksames Frühwarnsystem für künftige Pandemien durch Viren und andere Krankheitserreger betrachtet. Ein generelles Problem bei jeder quantitativen Messung von Parametern im Abwasser ist die starke Schwankung des Abwasservolumens und seiner Zusammensetzung im Tages- und Jahreszeitenverlauf. Um die Konzentrationsbestimmungen von Krankheitserregern im Abwasser in Korrelation mit menschlichen Einträgen setzen zu können, könnten sog. "anthropogene Marker" eine herausragende Rolle spielen, deren Eintrag ins Abwasser menschlichen Ursprungs sind. Im Projekt werden mittels ELISA die Konzentrationen ausgewählter anthropogener Marker in deutschlandweit gesammelten Abwasserproben erhoben und analysiert. Die Messergebnisse zeigen eindeutige Standortunterschiede auch in Abhängigkeit der Kläranlagengröße und vorhandener Indirekteinleiter. Die Untersuchungen zeigen, dass nicht alle anthropogene Marker an allen Standorten für eine Normalisierung von PCR-Daten für epidemiologische Untersuchungen verwendbar sind.
ISO 9223 standard for the classification of corrosivity in atmospheres is based on the mass loss of standard samples. We are concerned with the question of which corrosivity categories for Fe-sheets can be found at an offshore wind turbine and where they are comparable with our offshore locations.
The preliminary results indicate that the extreme corrosivity of class CX is only given in splash water-affected exposure, which is not a real atmospheric exposure condition. The results of the exposure at the SP show that the corrosivity category changes into C4, only a few meters above the splash water zone. Compared to the marine environments at Helgoland or OSS-Platform, the corrosivity is higher. The offshore environment is not as corrosive as originally expected, no atmospheric corrosion attack could be determined that would form the corrosivity category C5.
Es wird eine Studie zur Charakterisierung eines anisotropen Stahls vorgestellt, bei der Ultraschalluntersuchungen mit Mikrostrukturanalysen verbunden werden. Das Material weist hohe Festigkeit und Korrosionsbeständigkeit auf, zugleich ist mit anisotropen Eigenschaften die mechanischen und betrieblichen Eigenschaften beeinflussen zu rechnen. Vorläufige Ergebnisse lassen vermuten, dass weitere Untersuchungen notwendig sind, um die Fähigkeiten und Grenzen des Materials genau zu bestimmen. Es wird ein systematischer Ansatz mit Array- Prüfköpfen, Time-of-Flight Diffraction (TOFD) Technik und mikrostrukturellen Untersuchungen angewendet, um die Wechselwirkung zwischen Anisotropie und Mikrostruktur des Stahls zu analysieren. Ultraschallprüfungen mit der TOFD-Technik und in Tauchtechnik liefern Einblicke in das anisotrope Verhalten des Werkstoffes, einschließlich entsprechenden Kornorientierung, Dämpfung und Schallgeschwindigkeitsvariation. Diese Messungen führen in Verbindung mit mikrostrukturellen Analysen zu einem tieferen Verständnis des Materialverhaltens. Unser Hauptziel ist es, ein Framework zu erstellen, welches die Ultraschallantwort anisotroper Materialien mit ihren mikroskopischen Struktureigenschaften verbindet. Die vorgestellte Methodik ermöglicht eine zerstörungsfreie und zügige Bewertung der Materialintegrität, was besonders bei der Anwendung von Hochleistungsmaterialien relevant ist. Durch diesen integrativen Ansatz werden verschiedener Charakterisierungsmethoden kombiniert, um ein umfassenderes Materialverständnis zu erreichen.
Extrusion based 3D concrete printing (3DCP) is a growing technology because of its high potential for automating construction and the new possibilities of de-sign. In conventional construction methods, a sample is taken to be representative for one material batch. However, in 3DCP continuous mixing is used which re-sults in variations during the mixing process. Therefore, one sample is not repre-sentative for the entire structure. This leads to the necessity of continuous and re-al-time process monitoring.
At the Bundesanstalt für Materialforschung und -prüfung (BAM), Berlin, a test rig is developed to allow for comprehensive monitoring of the printing process. For this purpose, sensors for torque, temperature, pressure and moisture are in-stalled into the pipe. A laser scanner is installed at the nozzle to acquire infor-mation about the geometry of the extruded material.
This study focuses on the variations of pressure and temperature which are caused by changes in the material due to the ongoing mixing process. Preliminary results indicate that changes in the material properties cause changes in the sensor signals as well. These changes can be observed in various sensors with a delay, caused by material which is carried downstream. In the following, the data is ana-lysed to investigate if the changing material and the so caused change in pressure can be used to calculate volume flow.
Interaction of electromagnetic waves, such as electron beams or light, with conductive material can lead to localized surface plasmon resonances (LSPRs) where the incoming energy can be deposited in a collective excitation of electrons of the conduction band, which in turn can result in coherent localized plasmon oscillations. LSPR in metallic nanostructures, such as nanoparticles (NPs), which are sensitive to geometry, material composition and environment, are currently utilized in a wide range of applications, such as surface-enhanced Raman spectroscopy, plasmonic wave guides, improved solar cells, on-chip particle accelerators and nanoantennas. A host of studies that focus on plasmonic NPs ranging from single NPs with several shapes (cubic, spherical, tetrahedral) over 1D assemblies of NPs such as chains, to ordered 2D assemblies of NPs show an increase of the complexity regarding the hybridization behavior of LSPRs eventually lead to delocalized Surface Plasmons. Furthermore, Anderson predicted in 1977 the absence of diffusion or delocalization of waves in disordered systems, which has been discussed as the underlying mechanism for LSPRs localization in disordered metallic thin films and ultrathin 2D networks. Our aim is to further develop these studies on the surface plasmon localization in disordered structures by (1) developing a novel NPs assembly fabrication method that allows fabricating disordered assemblies of NPs of a wide range of NPs sizes, and (2) probing the LSPR with high-resolution electron energy-loss spectroscopy (EELS). Moreover, the dominant dipolar interaction between the NPs, also facilitates an efficient numerical modeling of these systems, which in comparison with the experiments allows for an in-depth study of the impact of various geometric parameters as well as retardation and life-time damping on the observed localization behavior.
To synthesize 2D disordered assemblies of gold NPs on a TEM transparent silicon oxide substrate, a new synthesis routine was developed. This procedure is based on sublimation and redeposition of a gold microparticle precursor induced by an electron beam in a scanning electron microscope (SEM) operated at 30 kV. To characterize the assembly of synthesized NPs in terms of size, shape and spreading over the substrate, TEM measurements were conducted subsequently. To study LSPRs experimentally, EELS in scanning transmission electron microscopy (STEM) mode was carried out. The numerical modelling of LSPRs was performed using a self-consistent dipole model.
The synthesized 2D disordered gold NPs assemblies exhibit a gradient in the NPs mean size, which ranges from 100 nm close to the precursor location down to 2 nm at a distance of more than 20 µm from the precursor location. Additionally, the interparticle distance between the gold NPs increases with increasing distance to the precursor location.
The experimental investigation as well as the numerical simulation of the LSPRs demonstrate a localization behavior that decreases toward larger energies, which is driven by the disorder of the NPs assembly (mainly the random particle distance). That localization behavior stays in contrast to what was found in ultrathin 2D gold networks showing increasing of localization towards higher LSPRs energies. By varying the geometric parameters of the NPs assembly in the simulation, we could identify the NPs thickness as the parameter, that determines the energy-dependence of the localization. Specifically, a critical thickness of approx. 10 nm separates the two localization regimes, which correlates to the energy of the dipole mode resonance crucially depending on the thickness of the NPs.
2D disordered assemblies of gold NPs of a wide range of NPs sizes and distances can be synthesized directly on thin substrates facilitating structural characterization and EELS measurements in a TEM. It could be shown that such assemblies exhibit LSPRs with a localization behavior that may be tuned by the NPs sizes (including thickness) and interparticle distances. The proposed synthesis of random NPs assemblies opens new avenues for fundamental studies on Anderson localization in disordered plasmonic structures as well as its applications such as surface-enhanced Raman spectroscopy where localization behavior must be tuned to specific wave lengths.
Sub-4 nm particles from FFF-3D printing measured with the TSI 1 nm CPC and the Airmodus A11 nCNC
(2024)
Concerns have been raised as Fused Filament Fabrication (FFF) desktop 3D printer emits harmful ultrafine particles (dP < 100 nm) during operation in indoor spaces. However, the vast majority of previous emission studies have neglected the possible occurrence of sub-4 nm particles by using conventional condensation particle counter (CPC) for detection. Thus, the total particle emission could be systematically underestimated. This study has compared two diethylene glycol (DEG) based instruments to evaluate their suitability for measuring organic FFF particles in the sub-4 nm size range either as particle counter or as a particle size spectrometer.
This study introduces an innovative method for efficiently determining the creep properties of high-temperature materials through high-throughput testing, employing digital image correlation [1,2]. The focus is on the AlCoCrFeNiTi alloy [3-5], synthesized by directional solidification, known for its exceptional strength and unique properties. Experimental investigations, including compression, and bending creep tests, were conducted at 750°C.
Capitalizing on the inhomogeneous stress and strain distribution within a cantilever subjected to bending, we leverage this characteristic to extract multiple creep curves from a single test. Stresses at key points were determined using existing analytical solutions [5,6]. Uniaxial tests spanning 300 to 500 MPa initial stress were complemented by bending tests designed to induce similar stress levels. A detailed comparison between bending and uniaxial creep is presented, including the results of verification studies on additional alloys.
This methodology not only expedites testing but also minimizes material usage, energy consumption, and manual labour. This research showcases a reliable and time-efficient approach to exploring the creep behavior of high-temperature materials. The technique is particularly advantageous for characterizing precious alloys with limited dimensions. Microstructural heterogeneity may exist in specimens tested under bending load, however, it can still be correlated to the mechanical properties with modern high-resolution characterization methods. Stress and resulting strain can be directly compared in a single specimen, ensuring uniform manufacturing, and heating history. This method eliminates the possible errors due to testing with different rigs, which could impair the accuracy of studies based on individual tests.
Mit der zunehmenden Relevanz der additiven Fertigung in Fertigungsbereiche mit hohen Anforderungen an Bauteilqualität, wird eine gute Prozessüberwachung unausweichlich. Eine Methode, die bereits gute Korrelation mit Bauteilfehlern gezeigt hat, ist die Temperaturüberwachung mithilfe von thermografischen Methoden. Allerdings unterliegt die Bestimmung der Realtemperaturen vielen unterschiedlichen Problemen. Ein Ansatz mit den Herausforderungen umzugehen, stellt der multispektrale Ansatz dar, der im Projekt QT-LPA untersucht und hier vorgestellt wird.
Black fungi belong to different classes of Ascomycota but evolved similar morpho-physiological adaptations such as yeast-like growth and constitutive melanin formation to colonize extreme competition-free environments. They are ubiquitously found on air-exposed surfaces, from ancient marble monuments to modern solar panels. The rock inhabitant Knufia petricola was chosen to become a model for these extremotolerant black fungi. Plasmid-based and ribonucleoprotein-based CRISPR/Cas9 techniques were introduced to precisely introduce one to multiple double strand breaks into the DNA to modify, replace or add sequences to the genome either using the available selection marker systems (hygR, natR, genR, baR, suR) or by marker-free approaches. Multiplexing is very efficient, allowing for four or more simultaneous genome editing events. The newly generated cloning vectors containing the Tet on construct for doxycycline-controlled gene expression, and the validated sites in the K. petricola genome for color-selectable (pks1, phs1, ade2) or neutral insertion (igr1 to 5) of expression constructs complete the reverse genetics toolbox. One or multiple endogenous or heterologous genes can be expressed on demand from different genomic loci or from a single construct by using 2A self-cleaving peptides. We thus can express genes from synthetic clusters in a non-pigmented background (Δpks1/Δphs1). The fact that K. petricola only produces few secondary metabolites (DHN melanin, carotenoids, mycosporines and a siderophore) and plant cell-wall degrading enzymes but is capable to take the burden of acetyl-CoA-consuming metabolism and protein secretion renders K. petricola a promising host for the expression of heterologous genes encoding high-end secondary metabolites and enzymes.
In times of digital data processing and sharing, a central challenge for the Materials Science and Engineering (MSE) community is the complete digital representation of materials, including their relevant processing and microstructure details and the resulting properties. This digital representation, supported by digital infrastructures, enables entirely new qualities of collaborative work and is central to how we will conduct MSE research and develop products in the future. The main challenges are the composition, shaping, and description of the data so that it can be easily interpreted, trusted, and re-used. This presentation introduces our current effort to develop a best practice framework for generating and distributing creep reference datasets for Ni-based superalloys, which builds on previous approaches. Researchers can use such datasets to compare their own experimental or simulation results, used, for instance, to perform simulation-based alloy design and optimization or in the verification of the own testing equipment. The concept includes building an easily accessible digital infrastructure to annotate and discover the datasets and the integration of an ontology that aligns with the necessary metadata schema. With the help of an ontology, the reference dataset for creep can be semantically described, thus enabling the digital representation and reusage of shared concepts from domain experts and the community. To achieve this, it is necessary to establish a defined vocabulary with corresponding relations and annotations. The interplay between a digital infrastructure, the agreement on the necessary metadata and related metadata schema, and an underlying ontology will ensure that data and results can be easily shared, taken up, and re-used, thus fulfilling the FAIR principles (Findable, Accessible, Interoperable, Reusable). Furthermore, we aim to develop a widely accepted definition of reference data and data quality levels and to reach a self-supported community process. We intend to motivate the discussion about reference material datasets, necessary metadata, and future collaborations within the creep community.
The recently certified reference material (CRM) BAM-N012 as cubical iron oxide FeOx nanoparticles (NPs) of 8 nm area equivalent square edge length (ESL) and the RM candidate BAM-N013 as nearly spherical NPs of 22 nm size were analyzed in detail by electron microscopy (EM).
For the metrological characterization with SEM, STEM in SEM and TEM, the understanding of the imaging contrasts and sensitivities, and the correct interpretation of the (art)effects which are inherent to each detection mode is necessary.
The same sample areas with NPs deposited on a TEM grid were analyzed by two SEM acquisition modes, i. e. SE InLens and STEM in SEM using a dedicated transmission sample holder, and further, correlatively, analyzed with TEM.
With increasing kV, SE InLens shows increasing particle size (unless overcharging at the particle boundaries is filtered), as a known effect. For STEM-in-SEM the particle size decreases significantly and individual particles are identified easier (at 2 kV only a few single particles can be detected automatically).
❑ Documentation of the sample preparation and measurement conditions (including optimization process) is important for reproducibility.
❑ Plasma cleaning, analysis in the transmission mode at SEM is recommended for FeOx NPs.
❑ Selection of the threshold algorithm can significantly alter the reported ECD.
The residual post-fire mechanical properties of fiber-reinforced epoxy (EP) composites are influenced by their fire residues after burning. This study uses intumescent/low-melting glass flame retardants (FRs) to tailor fire residues in epoxy resin. Processibility of prepregs, and their quality are analysed for transfer of the flame-retardant epoxy resins to layered glass-fiber reinforced composites (GFRCs). Minimal effects were found on the pre-fire flexural strengths of the composites due to low loading of the FRs. However, when transferred to GFRCS, the fire residues diminish significantly. Process, testing, and material adaptations are required to improve theoretical and experimental estimations of the post-fire mechanics of the composites.
Bei der Versorgung von Zähnen mit dentalen Kronenrestaurationen entsteht ein Kronen-Zement-Zahn-Komplex (KZZK). Dentale Werkstoffe überzeugen mit besten Materialeigenschaften, aber wie funktionieren sie im Verbund? Unsere zentrale Annahme lautet, dass die Alterung des KZZK eine zentrale Rolle bei Misserfolgen spielt. Präsentiert werden die Methodik und Bilder der ersten Arbeitsphase.
As the first commercial sodium-ion-batteries (SIBs) are available for purchase, it is possible to investigate material composition. Gaining an insight into the material composition of these SIBs is of interest not only for the classification of possible safety risks and hazards, but also in regards to recycling. Herein we report the preliminary investigations of the chemical and structural composition of first commercial SIB-cells. Two different SIB-cells with different specification were compared regarding electrode size, thickness and further parameters. Furthermore, the composition of the active materials and electrolyte was investigated and compared.
An understanding of Hydrogen-Oxygen/Air-Diluents gas mixtures combustion characteristics and their accurate prediction is crucial for ensuring the safety of hydrogen-related applications, reducing accidents risk, and protecting lives and property. Hydrogen detonation propagations are characterized by the detonation cell size, used to quantitatively predict for a mixture to detonate including, among others, the initiation energy, critical and minimum tube diameters. For the prediction of explosion limits, detonation run-up-distances and cell sizes, various empirical, semi-empirical and numerical models can be found in literature. These models are usually limited to a narrow range of explosion process or geometrical experimental parameters. Moreover, based on the limited availability of the detonation cell widths measurements, current estimation models are seemingly inaccurate. Machine learning models can be utilized to make justifiable prediction on the detonation cell sizes of hydrogen-air mixtures and other gaseous explosive mixtures cell sizes, explosion limits or run-up distance to detonation based on the mixture type, temperature, pressure, equivalence ratios as well as on geometrical parameters with consideration of highly diverse experimental data measurements uncertainties. Therefore, an up-to date database for explosion characteristics will be established and machine learning models will be developed, trained, tested, and validated using experimental data to predict explosion characteristics of hydrogen mixtures. The models predicted results will be validated against existing models. It will be tested whether machine learning models are able to predict the explosion characteristics of hydrogen mixtures with better accuracy and more comprehensively than conventional empirical and numerical models to be found in literature.
Non-equilibrium microstructure evolution in additive manufacturing (AM) is a major barrier for establishing a safe and sustainable application of AM in industrial processes. The constant heat source in the AM continuously affects the just-solidified grains beneath the melting pool, leading to directional grain growth (DGG). While real-time measurements of the non-equilibrium microstructure evolution is challenging, here developing a computational framework to systematically explore DGG becomes imperative.
We have advanced a comprehensive approach, integrating mean-field modeling and phase-field simulations, to elucidate the dynamics of DGG under an external driving force. Our simulations unveil a steady-state power-law grain growth kinetics during DGG, characterized by the interplay between curvature-driven dynamics at grain boundary junctions and directional driving forces.
The use of proton-transfer-reaction mass spectrometry (PTR-MS) for the determination of formaldehyde, ammonia and volatile sulfur organic compounds is described and suggestions are made for the application of stationary PTR-MS in a test laboratory. One advantage of PTR-MS compared to TD-GC-MS (thermal desorption gas chromatography mass spectrome-try) is the faster online measurement. Another advantage is the simultaneous determination of formaldehyde, ammonia, very volatile organic compounds (VVOC) and volatile organic com-pounds (VOC) which normally needs four different kinds of sampling. Coupling the PTR-MS with (multiple) air sample canisters or (multiple) emission test chambers would enable a quick analysis of indoor air and material emissions.
The development of a robust hydrogen infrastructure poses challenges to materials exposed to high pressurized hydrogen environments. Polymeric materials, which are expected to perform as seals, gaskets, O-rings, hoses among other applications face high risk of damage due to rapid gas decompression (RGD) which might cause operational safety issues. In this study, we intend to assess the effects of a high pressurized hydrogen environment on carbon black filled (CB) elastomers. The materials were exposed to 100 MPa hydrogen atmosphere at room temperature and at 85°C. Ex-situ characterization was performed during the first 30 minutes after decompression and repeated two days after the exposure when total gas desorption has taken place. The physical and mechanical characteristics of the materials were determined by means of density and volume change, hardness and tensile tests, and dynamic mechanical analysis.
Early detection of fatigue cracks and accurate measurements of the crack growth play an important role in the maintenance and repair strategies of steel and composite structures exposed to cyclic loads during their service life. Commonly used non-destructive techniques such as strain gauges, clip gauges, ultrasound, etc. used for detection and monitoring of fatigue damage are contact-based and perform local measurements. In addition, complex full-field techniques are commonly investigated, such as digital image correlation (DIC) and infrared thermography (IRT). In this work, a specific implementation of IRT, called lock-in IRT, is implemented for fatigue damage detection. This technique evaluates the thermal stress response of test specimens, specifically focusing or “locking-in” on the frequency of applied cyclic loads. Three different test scenarios are presented.
First, a section of a wind turbine rotor blade made of a glass fibre reinforced plastic (GFRP) shell structure under cyclic load was examined with Lock-In IRT along with DIC. The primary advantage of Lock-In IRT in this test setup was that it required no sample preparation, as compared to the painting and speckle pattern required for DIC. In the frequency domain, specifically the frequency of applied cyclic load, it was possible to extract local directional inhomogeneous loading within the shell structure due to progressive damage, confirmed with the deformation obtained from DIC results.
Second, thick welded specimens made of structural steel S355 were subjected to multiple NDT methods such as strain gauges, crack luminescence penetration (developed specifically at BAM), ultrasound, and IRT, with the aim of investigating the ability of each technique to detect fatigue damage initiation as early as possible in the total fatigue life of the specimen. Amongst the range of implemented techniques, Lock-In IRT provided the first indication of fatigue crack initiation at the weld toe of the specimens. This was validated with the other techniques as well as fractography.
Third, steel S355 specimens used to manufacture offshore wind turbine monopiles were tested. The specimens were extracted from a plate that was submerged in a marine environment, resulting in a corroded surface with corrosion pits. These specimens were subjected to cyclic tensile loads without removing the corrosion pits. The fatigue tests were monitored using IRT in a special full-field capturing setup that enables both sides of the specimen to be examined with one IRT camera. This allowed the entire pitted surface to be monitored for fatigue damage initiation at the same time. With the implementation of Lock In IRT, the surface stress distribution could be captured (the stress concentration at the pits), and fatigue crack initiation could be detected and linked with specific corrosion pits.
Since the original report in 2004 by Novoselov and Geim, Graphene gained incredible attention due to its fascinating properties. In the past 20 years, the synthesis and functionalization of graphene has evolved significantly[3]. Different synthesis techniques were developed which led to other graphenerelated materials such as graphene oxide (GO) or elemental-doped graphene. Further chemical functionalization can enhance but also alter or reduce specific properties of the graphene. To reveal the nature of these materials a proper physico‑chemical characterization with different analytical techniques is crucial.
Single-layer GO flakes kindly provided by Graphenea (Spain) were prepared for systematic image analysis. These flakes were disposed on an alignment-marked SiO2 substrate and correlatively imaged by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy. The high lateral resolution and/ or extreme surface sensitivity of the mentioned
techniques is necessary to explore monolayers. The ToF-SIMS images match well with the SEM and AFM images and provide information about the chemistry. With 2D Raman spectroscopy it is possible to differentiate between the number of stacked single-layer flakes. This is visualized in a 3D image (Figure b). Well-defined GO flakes could be used as a reference material for imaging of graphene-like structures but also of other types of 2D materials.
In addition to these monolayer GO flakes, commercial graphene-containing inks (Haydale) with a more complex morphology were also correlatively imaged. ToF-SIMS and SEM images were merged to identify the origin of different chemical fragments. The findings correlate closely with the expectation that the specific functionalizations (with fluorine and nitrogen as marker elements) are present only on the graphene flakes as presumed from the SEM images. Energy-dispersive X-ray spectroscopy (EDX) supports these results, yet with a much lower sensitivity compared to ToF-SIMS.
Since the original report in 2004 by Novoselov and Geim, Graphene gained incredible attention due to its fascinating properties. In the past 20 years, the synthesis and functionalization of graphene has evolved significantly[3]. Different synthesis techniques were developed which led to other graphenerelated materials such as graphene oxide (GO) or elemental-doped graphene. Further chemical functionalization can enhance but also alter or reduce specific properties of the graphene. To reveal the nature of these materials a proper physico‑chemical characterization with different analytical techniques is crucial.
Single-layer GO flakes kindly provided by Graphenea (Spain) were prepared for systematic image analysis. These flakes were disposed on an alignment-marked SiO2 substrate and correlatively imaged by scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and Raman spectroscopy. The high lateral resolution and/ or extreme surface sensitivity of the mentioned
techniques is necessary to explore monolayers. The ToF-SIMS images match well with the SEM and AFM images and provide information about the chemistry. With 2D Raman spectroscopy it is possible to differentiate between the number of stacked single-layer flakes. This is visualized in a 3D image (Figure b). Well-defined GO flakes could be used as a reference material for imaging of graphene-like structures but also of other types of 2D materials.
In addition to these monolayer GO flakes, commercial graphene-containing inks (Haydale) with a more complex morphology were also correlatively imaged. ToF-SIMS and SEM images were merged to identify the origin of different chemical fragments. The findings correlate closely with the expectation that the specific functionalizations (with fluorine and nitrogen as marker elements) are present only on the graphene flakes as presumed from the SEM images. Energy-dispersive X-ray spectroscopy (EDX) supports these results, yet with a much lower sensitivity compared to ToF-SIMS.
Das EU-finanzierte Projekt REINCARNATE, im Rahmen des Horizont Europa Programms, setzt neue Maßstäbe in der Kreislaufwirtschaft des Bauwesens durch den Einsatz fortschrittlicher Bauwerksdiagnose-Tools. Diese Werkzeuge, insbesondere die Zerstörungsfreie Prüfung (ZfP), spielen eine zentrale Rolle bei der Förderung der Zirkularität in der Baubranche. Die ZfP ermöglicht es, die Qualität und Eignung von Baumaterialien präzise zu bestimmen, ohne diese zu beschädigen. Dies ist entscheidend für die Wiederverwendung und das Recycling von Baustoffen und trägt wesentlich zur Reduzierung des Bauabfalls bei. Durch die Integration dieser Technologie in die Planungs- und Entwurfsphase können Architekten und Ingenieure aktiv einen nachhaltigeren Bauprozess fördern. REINCARNATE verbindet diese Diagnosemethoden mit digitalen Innovationen wie der Technologie des digitalen Zwillings und KI-gesteuerten Lösungen. Diese Kombination ermöglicht eine noch genauere und effizientere Bewertung und Nutzung von Baustoffen, was die Wiederverwendbarkeit und das Recycling verbessert. Im Rahmen des Projekts werden elf Demonstrationsprojekte in ganz Europa umgesetzt, die die praktische Anwendung dieser Technologien zeigen. Diese Projekte demonstrieren, wie ZfP und digitale Werkzeuge zusammenwirken, um Materialien, die traditionell als Abfall angesehen werden, in wertvolle Ressourcen umzuwandeln. Das Ziel von REINCARNATE ist eine 80-prozentige Verringerung der Bauabfälle und eine 70-prozentige Reduzierung des CO2-Fußabdrucks. Mit diesem Beitrag demonstrieren wir eine klare, umsetzbare Anleitung für die Bauindustrie, wie Innovationen in die Praxis umgesetzt werden können. Wir präsentieren greifbare Strategien zur Implementierung nachhaltiger, zirkulärer Praktiken im Bauwesen und markiert einen Wendepunkt in Richtung einer nachhaltigeren Bauindustrie.
Hybrid additive manufacturing is becoming increasingly important in the field of additive manufacturing. Hybrid approaches combine at least two different manufacturing processes. The focus of this work is the build-up of geometries onto conventionally manufactured parts using laser-based powder bed fusion of metals (PBF-LB/M). The hybrid build-up requires a precise position detection system inside the PBF-LB/M machines to determine the exact position of the existing component. For this purpose, high-resolution camera systems can be utilized. However, the use of a camera system is associated with several challenges. The captured images are subject to various distortions of the optical path. Due to these distortions, it is not possible to use the images for measurements and, therefore, it is not possible to calculate the positions of objects. In this study a homography matrix is calculated to correct keystone distortion in the images. Different calibration patterns have been tested for the calculation of the homography matrix. The influence of the number of calibration points on the precision of position detection of objects is determined. Furthermore, the influence of an additional camera calibration by using ChArUco boards is evaluated. The result is a camera calibration workflow with associated calibration pattern for a precise position detection of parts inside PBF-LB/M machines allowing a hybrid build-up with minimum physical offset between base component and build-up.
In der automatisierten Ultraschallprüfung von Komponenten mit komplexen Oberflächengeometrien werden zur Führung des Prüfkopfes zunehmend 6-Achsen-Roboter erprobt. Diese stellen die notwendige Automatisierbarkeit und Flexibilität bereit, um die lokal senkrechte Einschallung sicherzustellen. Durch den Einsatz von linearen Arrays und bildgebenden Verfahren können die Bilder oder die daraus extrahierten Merkmale zu einer Rekonstruktion in 3D zusammengesetzt werden. Die Anforderungen an die Prüfbahnen für die bildgebende Array-Ultraschallprüfung gehen dabei über konventionellen Bahnplanungsprogramme hinaus. Es wird ein Prozess vorgestellt, der Roboterbahnen auf der Grundlage des 3D-Modells von Körpern mit doppelt gekrümmter Oberfläche unter Berücksichtigung der Prüfparameter erzeugt. Hierbei wird zum einen die senkrechte Prüfkopfstellung und zum anderen eine optimale Abdeckung der Oberfläche realisiert. Dabei wird die lokale Oberflächengeometrie beachtet, da diese das Reflexionsverhalten beeinflusst und sich daher auf die optimale Verteilung und Orientierung der Prüfpositionen auswirkt. Damit einhergehend erfolgt eine Ablösung von konventionellen Konzepten, die auf linearen Prüfbahnen basieren, welches spannende neue Prüfstrategien eröffnet.
The stress–strain behavior of certain ceramics, such as aluminum titanate (AT, Al2TiO5), has features that are unusual for brittle material. In particular, a substantial nonlinearity under uniaxial tension, and load–unload hysteresis caused by the increase of the incremental stiffness at the beginning of unloading. These features are observed experimentally and attributed to microcracking. In this study, we investigate the mechanical response of an AT material at room and high temperature. Microstructure and microcracking are analyzed by means of electron microscopy, and both synchrotron micro computed tomography (µCT) and refraction radiography (SXRR). Synchrotron refraction radiography is combined with in-situ heating at high-temperatures (up to 1400°C) to be able to monitor the relative closure of microcracks as a function of increasing/decreasing temperatures.
ACCORDs is an Horizon Europe project working in the development of an imaging-based characterization framework (ACCORDs framework) for the holistic correlative assessment of Graphene Family Materials (GFMs) as a representative of 2D nanomaterials (NMs) to assess and predict 2D NMs health and environmental risks. The ACCORDs framework will operationalise safe and sustainable by design (SSbD) strategies proposed in past or ongoing H2020 projects or within OECD by correlating low-, medium-, and high-resolution physico-chemical-biological imaging-based methods with non-imaging methods in a tiered approach. ACCORDs will deliver the ACCORDs framework and user guidance, new imaging-based characterisation methods, reference in vitro tests, new reference 2D NMs for different matrices, a new minimum information reporting guideline for FAIR data sharing and reuse of images as well as an atlas with reference images for diagnostics of compromised safety of GFMs/GFM products. The new guidelines and standard proposals will be submitted to standardisation bodies to allow creation of regulatory ready products. The novelty of ACCORDs is in translating the principles of medical imaging-based diagnostics to 2D material hazard diagnostics. ACCORDs will accelerate industrial sectors in the area of aviation, marine construction, drone production, flexible electronics, photovoltaics, photocatalytics and print inks-based sensors. The value ACCORDs proposes to the graphene industry are practical, easy, imaging-based tools for GFM quality monitoring next to the production line with a possibility to be correlated with advanced highresolution imaging characterization methods in case hazard i.e. deviation from controls (benchmark values) are diagnosed. The ACCORDs framework and tools will contribute to the European Green Deal by addressing the topic: “Graphene: Europe in the lead” and to a new European strategy on standardization, released on 2nd February, 2022.
A new hydrogen-based test rig is being developed for a feasibility study on the use of hydrogen as an energy source for thermal testing in accordance with the IAEA SSR-6 guidelines for transport packages containing radioactive materials.
The test rig will be capable of combusting hydrogen for a wide range of different burner geometries, mass flows and if necessary hydrogen blends. As this type of fire test according to the IAEA boundary conditions (SSR-6 & SSG-26) does not yet exist, a large number of preliminary investigations, safety assessments and calculations must be carried out in order to develop a viable concept for hydrogen fires.
A new hydrogen-based test rig is being developed for a feasibility study on the use of hydrogen as an energy source for thermal testing in accordance with the IAEA SSR-6 guidelines for transport packages containing radioactive materials.
The test rig will be capable of combusting hydrogen for a wide range of different burner geometries, mass flows and if necessary hydrogen blends. As this type of fire test according to the IAEA boundary conditions (SSR-6 & SSG-26) does not yet exist, a large number of preliminary investigations, safety assessments and calculations must be carried out in order to develop a viable concept for hydrogen fires.
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.
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.
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.
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.
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.
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.
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.
Hydrogen gas plays a key role in the European energy transition strategy. When transmitting and storing compressed hydrogen gas, safety is one of the most important conditions. With increasing hydrogen pressure and temperature, more hydrogen is absorbed by the steel components, such as pipelines or valves, and may lead to embrittlement. Although, a deep understanding of microstructure on the hydrogen solubility in steels is missing. Classical Sieverts’ law is only valid at high temperatures and low gas pressures. For that purpose, new theory is presented, which explains the role of microstructure on hydrogen solubility. Hydrogen trapping at microstructural defects is a thermally activated mechanism and causes an increase of the hydrogen solubility with decreasing temperatures. This mechanism has to be considered in cryogenic applications, such liquid or compressed hydrogen storage.
The hollow specimen technique is a simple and economical method
that has the potential to overcome the limitations and complement
the current techniques for qualifying metallic materials under highpressure
hydrogen gas.
In this technique, an axial hole is manufactured in a tensile
specimen, which is then filled with hydrogen gas, sealed, and
placed in a standard testing machine. This method requires
significantly lower amounts of hydrogen, resulting in fewer safety
measures and does not require complex equipment or a specialised
laboratory, unlike the conventional autoclave technique.
Initial studies have demonstrated the feasibility of assessing
hydrogen effects in metallic materials using the hollow specimen
technique. This led to the establishment of the committee ISO/TC
164/SC 1/WG 9 to standardise the method, however, there are still
open questions that currently prevent the technique from being
standardised for hydrogen testing. These open questions are being
addressed in the H2HohlZug project, which is presented in this
contribution.