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Noble metal-free nanoparticles (NPs) based on multi-principal element alloys (MPEAs) were synthesized using a one-step pulsed laser ablation in liquids (PLALs) method for the electrochemical reduction of CO2. Laser ablation was performed in pure water or poly-(diallyldimethylammonium chloride) (PDADMAC)-containing an aqueous solution of Al8Cr17Co17Cu8Fe17Ni33 MPEA targets. Transmission electron microscopy (TEM) measurements combined with energy dispersive X-ray (EDX) mapping were used to characterize the structure and composition of the laser-generated MPEA nanoparticles (MPEA-NPs). These results confirmed the presence of a characteristic elemental distribution of a core-shell phase structure as the predominant NP species. The electrocatalytic performance of the laser-generated MPEA-NPs was characterized by linear sweep voltammetry (LSV) demonstrating an enhanced electrocatalytic CO2 activity for PDADMAC-stabilized NPs. The findings of these investigations indicate that MPEAs have great potential to replace conventional, expensive noble metal electrocatalysts.
The production of plastics is rising since they have been invented. Micro, submicro- and nanoplastics are produced intentionally or generated by environmental processes, and constitute ubiquitous contaminants which are ingested orally by consumers. Reported health concerns include intestinal translocation, inflammatory response, oxidative stress and cytotoxicity. Every digestive milieu in the gastrointestinal tract does have an influence on the properties of particles and can cause changes in their effect on biological systems. In this study, we subjected plastic particles of different materials (polylactic acid, polymethylmethacrylate, melamine formaldehyde) and sizes (micro- to nano-range) to a complex artificial digestion model consisting of three intestinal fluid simulants (saliva, gastric and intestinal juice). We monitored the impact of the digestion process on the particles by performing Dynamic Light Scattering, Scanning Electron Microscopy and Asymmetric Flow Field-Flow Fractionation. An in vitro model of the intestinal epithelial barrier was used to monitor cellular effects and translocation behavior of (un)digested particles. In conclusion, artificial digestion decreased cellular interaction and slightly increased transport of all particles across the intestinal barrier. The interaction with organic matter resulted in clear differences in the agglomeration behavior. Moreover, we provide evidence for polymer-, size- and surface-dependent cellular effects of the test particles.
Iron oxide of various structures is frequently used as food colorant (E 172). The spectrum of colors ranges from yellow over orange, red, and brown to black, depending on the chemical structure of the material. E 172 is mostly sold as solid powder. Recent studies have demonstrated the presence of nanoscaled particles in E 172 samples, often to a very high extent. This makes it necessary to investigate the fate of these particles after oral uptake. In this study, 7 differently structured commercially available E 172 food colorants (2 x Yellow FeO(OH), 2 x Red Fe2O3, 1 x Orange Fe2O3 + FeO(OH) and 2 x Black Fe3O4) were investigated for particle dissolution, ion release, cellular uptake, crossing of the intestinal barrier and toxicological impact on intestinal cells. Dissolution was analyzed in water, cell culture medium and artificial digestion fluids. Small-angle X-ray scattering (SAXS) was employed for determination of the specific surface area of the colorants in the digestion fluids. Cellular uptake, transport and toxicological effects were studied using human differentiated Caco-2 cells as an in vitro model of the intestinal barrier. For all materials, a strong interaction with the intestinal cells was observed, albeit there was only a limited dissolution, and no toxic in vitro effects on human cells were recorded.
AbstractHigh-strength aluminum alloys used in aerospace and automotive applications obtain their strength through precipitation hardening. Achieving the desired mechanical properties requires precise control over the nanometer-sized precipitates. However, the microstructure of these alloys changes over time due to aging, leading to a deterioration in strength. Typically, the size, number, and distribution of precipitates for a quantitative assessment of microstructural changes are determined by manual analysis, which is subjective and time-consuming. In our work, we introduce a progressive and automatable approach that enables a more efficient, objective, and reproducible analysis of precipitates. The method involves several sequential steps using an image repository containing dark-field transmission electron microscopy (DF-TEM) images depicting various aging states of an aluminum alloy. During the process, precipitation contours are generated and quantitatively evaluated, and the results are comprehensibly transferred into semantic data structures. The use and deployment of Jupyter Notebooks, along with the beneficial implementation of Semantic Web technologies, significantly enhances the reproducibility and comparability of the findings. This work serves as an exemplar of FAIR image and research data management.
With 2,2-dibutyl-2-stanna-1,3-dithiolane (DSTL) and 2-stanna-1,3-dioxa-4,5,6,7-dibenzoxepane (SnBiPh) as catalysts ring-expansion polymerizations (REP) were performed either in 2 M solution using three different solvents and two different temperatures or in bulk at 140 and 120 ◦C. A kinetically controlled rapid REP up to weight average molecular masses (Mẃs) above 300 000 was followed by a slower degradation of the molecular masses at 140 ◦C, but not at 120 ◦C Furthermore, a low molecular mass cyclic poly(L-lactide) (cPLA) with a Mn around 16 000 was prepared by polymerization in dilute solution and used as starting material for ring-ring equilibration at 140 ◦C in 2 M solutions. Again, a decrease of the molecular mass was detectable, suggesting that the equilibrium Mn is below 5 000. The degradation of the molecular masses via RRE was surprisingly more effective in solid cyclic PLA than in solution, and a specific transesterification mechanism involving loops on the surface of crystallites is proposed. This degradation favored the formation of extended-ring crystallites, which were detectable by a “saw-tooth pattern” in their MALDI mass spectra.
Simulation-Assisted Augmentation of Missing Wedge and Region-of-Interest Computed Tomography Data
(2024)
This study reports a strategy to use sophisticated, realistic X-ray Computed Tomography (CT) simulations to reduce Missing Wedge (MW) and Region-of-Interest (RoI) artifacts in FBP (Filtered Back-Projection) reconstructions. A 3D model of the object is used to simulate the projections that include the missing information inside the MW and outside the RoI. Such information augments the experimental projections, thereby drastically improving the reconstruction results. An X-ray CT dataset of a selected object is modified to mimic various degrees of RoI and MW problems. The results are evaluated in comparison to a standard FBP reconstruction of the complete dataset. In all cases, the reconstruction quality is significantly improved. Small inclusions present in the scanned object are better localized and quantified. The proposed method has the potential to improve the results of any CT reconstruction algorithm.
Alkali-aktivierte Hüttensandbetone – CO2-reduzierte Bindemittel mit hohem Korrosionsschutzpotential
(2023)
Durch den Ersatz von Portlandzement können alkali-aktivierte Bindemittel einen bedeutenden Beitrag zur Verringerung der durch die Zementklinkerherstellung verursachten CO2-Emissionen leisten. Für die Verwendung von alkali-aktivierten Bindemitteln in Stahlbetonkonstruktionen, die Chloriden oder Carbonatisierung ausgesetzt sind, ist die Fähigkeit des Stahls, den passiven Zustand zu erreichen und aufrechtzuerhalten, von großer Bedeutung. Die Prozesse der Deckschichtbildung von Stahl in alkali-aktivierten Materialien unterscheiden sich jedoch zum Teil grundlegend von denen in Portlandzementen. Alkali-aktivierte Hüttensandbetone weisen gute technische Eigenschaften auf, bisher fehlen jedoch grundlegende Kenntnisse bzgl. ihrer schützenden Wirkung bei korrosiven Angriffen. Dies ist vor allem auf ihre sulfidhaltige Porenlösung zurückzuführen, welche die elektrochemischen Eigenschaften der Stahloberfläche beeinflusst und die Verwendung herkömmlicher Bewertungsmaßstäbe erschwert. Es werden erste Ergebnisse eines DFG-Forschungsprojektes vorgestellt, in dem das Passivierungsverhalten von Stahl in alkali-aktivierten Hüttensandmörteln unterschiedlicher Zusammensetzungen sowie in Mörteln auf Basis hüttensandhaltiger Normzemente untersucht wird. Über einen Zeitraum von mindestens 28 Tagen werden an Zylinderprüfkörpern im 3-Elektroden-Aufbau das Ruhepotential sowie die Polarisationswiderstände der Stahlelektroden ermittelt.
Here, we report a comparative study of different sum parameter analysis methods for the extraction of per- and polyfluoroalkyl substances (PFAS) from manufactured consumer products, which can be measured by combustion ion chromatography (CIC). Therefore, a hydrolysis-based extraction method was further developed, which accounts for the addition of hydrolyzable covalently bound polyfluoroalkylated side-chain polymers (SFPs) to the extractable organic fluorine portion of the mass balance proposed as "hydrolyzable organically bound fluorine" (HOF). To test this hypothesis, the method was applied to 39 different consumer products containing fluoropolymers or monomeric PFAS taken from four different categories: outdoor textiles, paper packaging, carpeting, and permanent baking sheets. We also evaluated the method's efficiency by extracting four synthesized fluorotelomer polyacrylate reference compounds. The total fluorine (TF) and extractable organically bound fluorine (EOF) values were measured through CIC using established protocols. The TF values ranged from sub-ppb to %-levels, depending on the compound class. All samples showed results for hydrolyzed organofluorine (HOF) between 0.03 and 76.3 μg/g, while most EOF values were lower (<LOD to 58.1 μg/g). Moreover, the methods were contrasted with the "total hydrolyzable precursor" (THP) assay analyzed using gas-chromatography coupled mass spectrometry (GC-MS), which yielded concentrations of 6:2–10:2 fluorotelomer alcohols (<LOD-568 μg/g) for textile and paper samples. Furthermore, targeted analytical investigation of 25 compounds via liquid chromatography coupled tandem mass spectrometry (LC-MS/MS) was conducted and accounted for significantly lower sum amounts (<LOD-0.98 μg PFAS/g). To estimate the fluorine mass balance of all methods, the fluorine levels of target analytical data were calculated and compared to the sum parameter values and evaluated. Finally, the efficiency of the extraction method was approximated by the recovery analysis of four selected SFP model compounds compared to their TF values, yielding 36.7–74.0% after extraction and 3.8–36.3% after processing the extract for the HOF sum parameter.
Im Jahr 2020 fielen in Deutschland rund 220 Millionen Tonnen mineralische Bau- und Abbruchabfälle an, die als Sekundärrohstoffquelle genutzt werden können. Trotz hoher Recyclingquoten wird ein Teil der mineralischen Bau- und Abbruchabfälle immer noch deponiert oder in Anwendungen mit geringen Qualitätsanforderungen eingesetzt, da ein effektives Recycling dieser heterogenen Abfälle recht kompliziert ist. Bauschutt ist ein heterogener, SiO2-reicher Sekundärrohstoff, der sich aus einem Gemisch verschiedener abgebrochener Baumaterialien wie Ziegel, Betonfertigteile, Leichtbeton, Porenbeton, Kalksandsteine, Natursteine, Gips und Mörtel zusammensetzt. Die genaue Zusammensetzung hängt von der Abbruchstelle, der Vorsortierung und der Wiederaufbereitung in der Recyclinganlage ab. Eine direkte Wiederverwendung als rezyklierte Gesteinskörnung ist aufgrund der uneinheitlichen Zusammensetzung und des bis zu 50 %igen Feinanteils nach der mechanischen Aufbereitung nicht zulässig. Eine Möglichkeit, Mauerwerksschutt effektiv zu recyceln, ist die rohstoffliche Verwertung über ein chemisch-hydrothermales Umwandlungsverfahren, das poröse Granulate erzeugt. Durch die Porenstruktur dieser hydrothermal gehärteten Granulate ergeben sich Anwendungsmöglichkeiten als Filter- oder Wasserspeichermaterial, die über den Bausektor hinausgehen. Diese neuartigen Granulate können leichte Gesteinskörnungen natürlichen Ursprungs (z. B. Lavasand, Bimsstein) oder Körner aus natürlichen Rohstoffen (z. B. Blähton) ersetzen. Die neue Recyclingstrategie spart natürliche Ressourcen. Im Vergleich zur Herstellung von Blähton ist der Energieverbrauch wesentlich geringer. Ziel des Verbundprojektes HYTEGRA war die Entwicklung eines Verfahrens zur Herstellung von leichten Gesteinskörnungen aus SiO2- und CaO-reichen Sekundärrohstoffen. Als Rohstoffe wurden Mauerwerksschutt als SiO2-Quelle und Papierasche aus der energetischen Verwertung von Reststoffen der Altpapierverwertung als CaO-Quelle eingesetzt. Der komplette Prozess von der mechanisch-physikalischen Aufbereitung über die Bildung des Grüngranulats bis zur hydrothermalen Härtung wurde entwickelt und im Labormaßstab getestet. Die Anwendungen des hydrothermal gehärteten Granulats als Wasserspeichermaterial für die innere Nachbehandlung von hochfestem Beton, Pflanzensubstrat und Filtermaterial in Bodenfiltern zur Abwasserreinigung wurden untersucht. Der Beitrag gibt einen Überblick über die wichtigsten Ergebnisse des erfolgreich abgeschlossenen Verbundforschungsprojekts HYTEGRA.
Die Einführung von Wasserstoff als sicherer Energieträger braucht eine robuste Wissensbasis, darauf aufgebaute Werkzeuge zur Auslegung und Sicherheitsbewertung von Wasserstofftechnologien und ein international harmonisiertes Regelwerk. Viele der innovativen Technologien implizieren Wasserstoff bei hohen Drücken und/oder kryogenen Temperaturen, mit denen in verteilten Anwendungen erstmalig private Nutzer in Kontakt kommen. Um überkonservative, teure Sicherheitslösungen zu vermeiden, gleichzeitig aber die Einsetzbarkeit und Sicherheit von Wasserstoffanwendungen zu demonstrieren und die Akzeptanz für die Technologie aufrecht zu halten, muss auch die Sicherheitsforschung mit den Trends der technologischen Entwicklung Schritt halten, oder sie besser noch antizipieren. So beschreibt dieser Überblicksartikel nicht nur den gegenwärtigen Stand der Kenntnisse und Technik bezüglich Wasserstoffsicherheit, sondern auch ihre Weiterentwicklung.
The ISO 3690 standard “Determination of hydrogen content in arc weld metal” requires a thermal activation of the diffusible hydrogen in a piece of weld metal for the subsequent ex situ concentration measurement by carrier gas hot extraction CGHE or thermal desorption spectroscopy (TCD). Laser-induced breakdown spectroscopy (LIBS) offers a time and spatially resolved, almost non-destructive, in situ measurement of hydrogen at surfaces without sample preparation. We measured hydrogen in steels, which were charged either electrochemically or by high-pressure hydrogen gas, and compared the results. Further, the feasibility of quantitative hydrogen line scan measurements with LIBS was demonstrated by measuring hydrogen at water jet cut surfaces. The hydrogen concentrations measured with the help of LIBS were compared with CGHE measurements. It was observed that hydrogen can be reliably measured with LIBS for concentrations larger than 2 wt.-ppm. The maximum hydrogen concentration achieved using electrochemical charging was 85.1 ppm. The results show that LIBS is a promising technique for time- and spatially resolved measurements of hydrogen in steels.
A route to a ZrF4 catalyst active in room temperature Friedel–Crafts and dehydrofluorination reactions was developed via a fluorolytic sol–gel route, which was followed by a postfluorination step using a stream of CHClF2. The behaviour of different Zr(IV) precursors in a sol–gel reaction with anhydrous isopropanol/HF solution was investigated. The subsequent post-fluorination step was optimised in its temperature ramp and confirmed the necessity of a fluorination of the generated xerogels to obtain catalytic activity. The process is discussed in the context of the analysis of the materials using Brunauer–Emmett–Teller analysis (BET), powder X-ray diffraction (XRD), infrared spectroscopy (IR), thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The local structure of the amorphous catalyst was elucidated by extended X-ray absorption fine structure spectroscopy (EXAFS).
The different defect types on SiC samples are measured with various measurement methods including optical and tactile methods. The defect types investigated include particles, carrots and triangles and they are analyzed with imaging ellipsometry, coherent Fourier scatterometry and atomic force microscopy. Each of these methods measures different properties of the defects and they all together contribute to a complete analysis.
Understanding the susceptibility to spalling of concrete members in case of fire is important to evaluate the residual load-bearing capacity. The investigations of the spalling phenomenon of a concrete mixture using real scale members are necessary but expensive to carry out. Reducing the specimen size leads to an increase of boundary effects that can result in a reduced spalling or absence of spalling. In this study, fire tests were carried out on unrestrained, single-sided exposed, cuboid shaped specimens (0.6 m x 0.6 m x 0.29 m) as well as unrestrained and steel ring restrained cylindrical specimens (Ø = 0.47 m, h = 0.29 m), which induce different boundary conditions. These fire tests were carried out on two ordinary concrete mixtures. The two mixtures differ only in the type of aggregates (quartz gravel and basalt grit) and were used to investigate the influence of the thermal expansion of the aggregate on the spalling behaviour of the concrete. The results show a significant increase of
the spalling depth due to the restrained thermal expansion achieved by the applied steel rings. Additionally, the type of aggregate has a direct influence on the spalling behaviour of a concrete mixture. The reduction of the boundary effects by the steel rings recreate the test conditions in the centre of a large concrete member. Thus, this type of specimen is suitable to determine the susceptibility to spalling of a material (screening-tests) as preliminary investigations to full scale fire tests.
The global trend towards decarbonization and the demand for energy security have put hydrogen energy into the spotlight of industry, politics, and societies. Numerous governments worldwide are adopting policies and strategies to facilitate the transition towards hydrogen-based economies. To assess the determinants of such transition, this study presents a comparative analysis of the technological innovation systems (TISs) for hydrogen technologies in Germany and South Korea, both recognized as global frontrunners in advancing and implementing hydrogen-based solutions. By providing a multidimensional assessment of pathways to the hydrogen economy, our analysis introduces two novel and crucial elements to the TIS analysis: (i) We integrate the concept of ‘quality infrastructure’ given the relevance of safety and quality assurance for technology adoption and social acceptance, and (ii) we emphasize the social perspective within the hydrogen TIS. To this end, we conducted 24 semi-structured expert interviews, applying qualitative open coding to analyze the data. Our results indicate that the hydrogen TISs in both countries have undergone significant developments across various dimensions. However, several barriers still hinder the further realization of a hydrogen economy. Based on our findings, we propose policy implications that can facilitate informed policy decisions for a successful hydrogen transition.
Mean-field modeling and phase-field simulation of grain growth under directional driving forces
(2024)
Directional grain growth is a common phenomenon in the synthetic and natural evolution of various polycrystals. It occurs in the presence of an external driving force, such as a temperature gradient, along which grains show a preferred, yet competitive, growth. Novel additive manufacturing processes, with intense, localized energy deposition, are prominent examples of when directional grain growth can occur, beneath the melting pool. In this work, we derive a phenomenological mean-field model and perform 3D phase-field simulations to investigate the directional grain growth and its underlying physical mechanisms. The effect of the intensity of driving force is simulated and systematically analyzed at the evolving growth front as well as various cross-sections perpendicular to the direction of the driving force. We found that although the directional growth significantly deviates from normal grain growth, it is still governed by a power law relation <R> α tⁿ with an exponent n ~ 0.6–0.7. The exponent n exhibits a nontrivial dependence on the magnitude of the directional driving force, such that the lowest growth exponent is observed for intermediate driving forces. We elaborate that this can originate from the fact that the forces at grain boundary junctions evolve out of balance under the influence of the directional driving force. With increasing the driving forces, the growth exponent asymptotically approaches a value of n ≈ 0.63, imposed by the largest possible grain aspect ratio for given grain boundary energies. The current combined mean-field and phase-field framework pave the way for future exploration in broader contexts such as the evolution of complex additively manufactured microstructures.
We demonstrate the determination of anharmonic acoustic phonon properties via second-order Raman scattering exemplarily on copper iodide single crystals. The origin of multi-phonon features from the second-order Raman spectra was assigned by the support of the calculated 2-phonon density of states. In this way, the temperature dependence of acoustic phonons was determined down to 10 K. To determine independently the harmonic contributions of respective acoustic phonons, density functional theory in quasi-harmonic approximation was used. Finally, the anharmonic contributions were determined. The results are in agreement with earlier publications and extend CuI’s determined acoustic phonon properties to lower temperatures with higher accuracy. This approach demonstrates that it is possible to characterize the acoustic anharmonicities via Raman scattering down to zero-temperature renormalization constants of at least 0.1 cm⁻¹.
High-strength steels offer potential for weight optimization due to reduced wall thicknesses in modern constructions. Additive manufacturing processes such as Wire Arc Additive Manufacturing (WAAM) enable the resource-efficient production of structures. In the case of defects occurring in weld seams orWAAM components due to unstable process conditions, the economical solution is local gouging or machining and repair welding. It is important to understand the effects of machining steps on the multiaxial stress state in conjunction with the design-related shrinkage restraints. Research into how welding and slot milling of welds andWAAM structures affects residual stresses is still lacking. For this reason, component-related investigations with high-strength steels with yield strengths ≥790 MPa are carried out in our research. In-situ digital image correlation (DIC) and ex-situ X-ray diffraction (XRD) were used to analyze the stresses and strains induced on specimens during and after milling. The systematic analyses revealed a significant interaction of the stiffness and microstructure of the specimens with the initial residual stresses induced by welding. Subsequent repair welds can result in significantly higher residual stresses.
We present Jobflow, a domain-agnostic Python package for writing computational workflows tailored for high-throughput computing applications. With its simple decorator-based approach, functions and class methods can be transformed into compute jobs that can be stitched together into complex workflows. Jobflow fully supports dynamic workflows where the full acyclic graph of compute jobs is not known until runtime, such as compute jobs that launch
other jobs based on the results of previous steps in the workflow. The results of all Jobflow compute jobs can be easily stored in a variety of filesystem- and cloud-based databases without the data storage process being part of the underlying workflow logic itself. Jobflow has been intentionally designed to be fully independent of the choice of workflow manager used to dispatch the calculations on remote computing resources. At the time of writing, Jobflow
workflows can be executed either locally or across distributed compute environments via an adapter to the FireWorks package, and Jobflow fully supports the integration of additional workflow execution adapters in the future.
The production of plastics is rising since they have been invented. Micro, submicro- and nanoplastics are produced intentionally or generated by environmental processes, and constitute ubiquitous contaminants which are ingested orally by consumers. Reported health concerns include intestinal translocation, inflammatory response, oxidative stress and cytotoxicity. Every digestive milieu in the gastrointestinal tract does have an influence on the properties of particles and can cause changes in their effect on biological systems. In this study, we subjected plastic particles of different materials (polylactic acid, polymethylmethacrylate, melamine formaldehyde) and sizes (micro- to nano-range) to a complex artificial digestion model consisting of three intestinal fluid simulants (saliva, gastric and intestinal juice). We monitored the impact of the digestion process on the particles by performing Dynamic Light Scattering, Scanning Electron Microscopy and Asymmetric Flow Field-Flow Fractionation. An in vitro model of the intestinal epithelial barrier was used to monitor cellular effects and translocation behavior of (un)digested particles. In conclusion, artificial digestion decreased cellular interaction and slightly increased transport of all particles across the intestinal barrier. The interaction with organic matter resulted in clear differences in the agglomeration behavior. Moreover, we provide evidence for polymer-, size- and surface-dependent cellular effects of the test particles.