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Paper des Monats
- ja (71)
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.
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.
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.
Reliable measurement of the size of polydisperse, complex-shaped commercial nanopowders is a difficult but necessary task, e.g., for regulatory requirements and toxicity risk assessment. Suitable methods exist for the accurate characterization of the size of non-aggregated, stabilized, spherical and monodisperse nanoparticles. In contrast, industrial nanoscale powders usually require dedicated sample preparation procedures developed for the analysis method of choice. These nano-powders tend to agglomerate and/or aggregate, a behavior which in combination with an innate broad particle size distribution and irregular shape often significantly alters the achievable accuracy of the measured size parameters. The present study systematically tests two commercially available nanoscale powders using different sample preparation methods for correlative analysis by scanning electron microscopy, dynamic light scattering, Brunauer–Emmet–Teller method and differential mobility analysis. One focus was set on the sample preparation by embedding nanoparticles in carbon-based hot-mounting resin. Literature on this topic is scarce and the accuracy of the data extracted from cross sections of these particles is unclearly stated. In this paper systematic simulations on the deviation of the size parameters of well-defined series of nanoparticles with different shapes from the nominal value were carried out and the contributing factors are discussed.
Knowledge representation in the Materials Science and Engineering (MSE) domain is a vast and multi-faceted challenge: Overlap, ambiguity, and inconsistency in terminology are common. Invariant (consistent) and variant (context-specific) knowledge are difficult to align cross-domain. Generic top-level semantic terminology often is too abstract, while MSE domain terminology often is too specific. In this paper, an approach how to maintain a comprehensive MSE-centric terminology composing a mid-level ontology–the Platform MaterialDigital Core Ontology (PMDco)–via MSE community-based curation procedures is presented. The illustrated findings show how the PMDco bridges semantic gaps between high-level, MSE-specific, and other science domain semantics. Additionally, it demonstrates how the PMDco lowers development and integration thresholds. Moreover, the research highlights how to fuel it with real-world data sources ranging from manually conducted experiments and simulations with continuously automated industrial applications.
The usefulness of seven different Tin catalysts, Bismuth subsalicylate and Titan tetra(ethoxide) for the polycondensation of ethyl L-lactate (ELA) was examined at 150 °C/6 d. Dibutyltin bis(phenoxides) proved to be particularly effective. Despite the low reactivity of ELA, weight average molecular masses (Mw) up to 12 500 were found along with partial crystallization. Furthermore, polylactides (PLAs) of similar molecular masses were prepared via ELA-initiated ROPs of L-lactide by means of the four most effective polycondensation catalysts. The crystalline linear PLAs were annealed at 140 or 160 °C in the presence of these catalysts. The consequences of the transesterification reactions in the solid PLAs were studied by means of matrix-assisted laser desorption/ionization (MALDI TOF) mass spectrometry, gel permeation chromatography (GPC) and small-angle X-ray scattering (SAXS). The results indicate that polycondensation and formation of cycles proceed in the solid state via formation of loops on the surface of the crystallites. In summary, five different transesterification reactions are required to explain all results.
Pressure-sensitive adhesive tapes are used in several industrial applications such as con-struction, railway vehicles and the automotive sector,where the burning behavior is ofcrucial importance. Flame retarded adhesivetapes are developed and provided, however,often without considering the interaction of adhesive tapes and the bonded materialsduring burning nor the contribution of the tapes to fire protection goal of the bondedcomponents in distinct fire tests. This publication delivers an empirical comprehensiveknowledge how adhesive tapes and their flame retardancy effect the burning behaviorof bonded materials. With a special focus on the interaction between the single compo-nents, one flame retarded tape and one tapewithout flame retardant are examined inscenarios of emerging and developing fires, along with their bonds with the commonmaterials wood, zinc-plated steel, mineral wool, polycarbonate, and polymethylmethacry-late. The flame retardant significantly improved the flame retardancy of the tape as afree-standing object and yielded a V-2 rating in UL 94 vertical test and raised the OxygenIndex by 5 vol.%. In bonds, or rather laminates, the investigations prove that the choiceof carrier and substrates are the factors with the greatest impact on the fire propertiesand can change the peak of heat release rate and the maximum average rate of heatemission up to 25%. This research yielded a good empirical overall understanding of thefire behavior of adhesive tapes and bonded materials. Thus, it serves as a guide for tapemanufacturers and applicants to develop tapes and bonds more substrate specific.
A systematic study on a face‐centered cubic‐based compositionally complex alloy system Al–Co–Cr–Cu–Fe–Ni in its single‐phase state is carried out, where a mother senary compound Al₈Co₁₇Cr₁₇Cu₈Fe₁₇Ni₃₃ and five of its suballoys, obtained by removing one element at a time, are investigated and exhaustively analyzed determining the contribution of each alloying element in the solid solution. The senary and the quinaries are compared using experimental techniques including X‐ray absorption spectroscopy, X‐ray diffraction, transmission electron microscopy, and first principles hybrid Monte Carlo/molecular dynamics simulations. Chemical short‐range order and bond length distances have been determined both at the experimental and computational level. Electronic structure and local atomic distortions up to 5.2 Å have been correlated to the microhardness values. A linear regression model connecting hardness with local lattice distortions is presented.
In this work, the thermal properties of ternary Li₃ₓCo₇₋₄ₓSb₂₊ₓO₁₂ solid solutions are studied for different concentrations in the range 0 ≤ x ≤ 0.7. Samples are elaborated at four different sintering temperatures: 1100, 1150, 1200 and 1250 °C. The effect of increasing the content of Li⁺ and Sb⁵⁺, accompanied by the reduction of Co²⁺, on the thermal properties is studied. It is shown that a thermal diffusivity gap, which is more pronounced for low values of x, can be triggered at a certain threshold sintering temperature (around 1150 °C in this study). This effect is explained by the increase of contact area between adjacent grains. Nevertheless, this effect is found to be less pronounced in the thermal conductivity. Moreover, a new framework for heat diffusion in solids is presented that establishes that both the heat flux and the thermal energy (or heat) satisfy a diffusion equation and therefore highlights the importance of thermal diffusivity in transient heat conduction phenomena.
AbstractLithium‐ion cells connected in series are prone to an electrical safety risk called overdischarge. This paper presents a comprehensive investigation of the overdischarge phenomenon in lithium‐ion cells using operando nondestructive imaging. The study focuses on understanding the behavior of copper dissolution and deposition during overdischarge, which can lead to irreversible capacity loss and internal short‐circuits. By utilizing synchrotron X‐ray computed tomography (SXCT), the concentration of dissolved and deposited copper per surface area is quantified as a function of depth of discharge, confirming previous findings. The results also highlight for the first time a nonuniform distribution pattern for copper deposition on the cathode. This research provides insights for safer battery cell design.
Future lunar exploration will be based on in-situ resource utilization (ISRU) techniques. The most abundant raw material on the Moon is lunar regolith, which, however, is very scarce on Earth, making the study of simulants a necessity. The objective of this study is to characterize and investigate the sintering behavior of EAC-1A lunar regolith simulant. The characterization of the simulant included the determination of the phase assemblage, characteristic temperatures determination and water content analysis. The results are discussed in the context of sintering experiments of EAC-1A simulant, which showed that the material can be sintered to a relative density close to 90%, but only within a very narrow range of temperatures (20–30 °C). Sintering experiments were performed for sieved and unsieved, as well as for dried and non-dried specimens of EAC-1A. In addition, an analysis of the densification and mechanical properties of the sintered specimens was done. The sintering experiments at different temperatures showed that the finest fraction of sieved simulant can reach a higher maximum sintering temperature, and consequently a higher densification and biaxial strength. The non-dried powder exhibited higher densification and biaxial strength after sintering compared to the dried specimen. This difference was explained with a higher green density of the non-dried powder during pressing, rather than due to an actual influence on the sintering mechanism. Nevertheless, drying the powder prior to sintering is important to avoid the overestimation of the strength of specimens to be fabricated on the Moon.
Laser powder bed fusion of metallic components (PBF-LB/M) is gaining acceptance in industry. However, the high costs and lengthy qualification processes required for printed components create the need for more effective in-situ monitoring and testing methods. This article proposes multispectral Optical Tomography (OT) as a new approach for monitoring the PBF-LB/M process. Compared to other methods, OT is a low-cost process monitoring method that uses long-time exposure imaging to observe the build process. However, it lacks time resolution compared to expensive thermographic sensor systems. Monochromatic OT (1C-OT) is already commercially available and observes the building process layer-wise using a single wavelength window in the NIR range. Multispectral OT (nC-OT) utilizes a similar setup but can measure multiple wavelength ranges per location simultaneously. By comparing the classical 1C-OT and nC-OT approaches, this article examines the advantages of nC-OT (two channel OT and RGB-OT) in reducing the false positive rate for process deviations and approximating maximum temperatures for a better comparison between different build processes and materials. This could ultimately reduce costs and time for part qualification. The main goal of this contribution is to assess the advantages of nC-OT compared to 1C-OT for in-situ process monitoring of PBF-LB/M.
The Large Aperture Ultrasound System (LAUS) developed at BAM is known for its ability to penetrate thick objects, especially concrete structures commonly used in nuclear waste storage and other applications in civil engineering. Although the current system effectively penetrates up to ~9 m, further optimization is imperative to enhance the safety and integrity of disposal structures for radioactive or toxic waste. This study focuses on enhancing the system’s efficiency by optimizing the transducer spacing, ensuring that resolution is not compromised. An array of twelve horizontal shear wave transducers was used to find a balance between penetration depth and resolution. Systematic adjustments of the spacing between transmitter and receiver units were undertaken based on target depth ranges of known reflectors at depth ranges from 5 m to 10 m. The trade-offs between resolution and artifact generation were meticulously assessed. This comprehensive study employs a dual approach using both simulations and measurements to investigate the performance of transducer units spaced at 10 cm, 20 cm, 30 cm, and 40 cm. We found that for depths up to 5 m, a spacing of 10 cm for LAUS transducer units provided the best resolution as confirmed by both simulations and measurements. This optimal distance is particularly effective in achieving clear reflections and a satisfactory signal-to-noise ratio (SNR) in imaging scenarios with materials such as thick concrete structures. However, when targeting depths greater than 10 m, we recommend increasing the distance between the transducers to 20 cm. This increased spacing improves the SNR in comparison to other spacings, as seen in the simulation of a 10 m deep backwall. Our results emphasize the critical role of transducer spacing in achieving the desired SNR and resolution, especially in the context of depth imaging requirements for LAUS applications. In addition to the transducer spacing, different distances between individual sets of measurement positions were tested. Overall, keeping the minimal possible distance between measurement position offsets provides the best imaging results at greater depths. The proposed optimizations for the LAUS in this study are primarily relevant to applications on massive nuclear structures for nuclear waste management. This research highlights the need for better LAUS efficiency in applications such as sealing structures, laying the foundation for future technological advances in this field.
Offshore wind turbines continuously increase in size and weight and demand adequate offshore foundations concepts like monopiles, tripods, or jackets. These components are typically constructed using submerged arc welding (SAW) with high-strength thick steel plates like the S420ML. During welding, the occurrence of delayed hydrogen-assisted cracking (HAC) must be anticipated. HAC is a critical combination of the local hydrogen concentration within a susceptible microstructure under certain mechanical load, i.e., the occurring (welding) residual stresses. The welding sequence of the thick-walled plates complicates the residual stress distribution due to the necessary repeated thermal cycling, i.e., welding seam/layer deposition to fill the joint. For that purpose, SAW with two-wire-technique was used to weld a specially designed and prototype-like mock-up of a real component with a thickness of 50 mm, filled with over 20 passes and a seam length of 1000 mm. Additional welded stiffeners simulated the effect of a high restraint, to achieve critical HAC conditions. The necessity of a minimum waiting time (MWT) before the NDT can be conducted (to exclude HAC) was critically verified by the application of ultrasonic testing of the welded joint at different time-steps of the NDT of up to 48 h after the completion welding. The residual stresses were determined by a robot XRD goniometer. Tensile residual stresses up to the yield limit are found both in the weld metal and in the heat-affected zone. Numerical modeling allowed the qualitative estimation of the hydrogen diffusion in the weld. No noticeable HAC occurrence was identified and confirms the high cracking resistance of the investigated material. Finally, the applicability of the MWT concept should be critically discussed.
A novel DAS setup based on geometric phases in coherent heterodyne detection is applied for the first time to the characterisation of the Earth’s subsurface. In addition, an optimisation of the proposed setup in terms of its spatial resolution is also presented for the first time. The surface waves are generated by strong blasts of 25 kg of explosives at a dedicated test site. A 10 km dark fiber link in the vicinity of the test site connected to the test setup records the resulting strain signals. The spike-free and low-noise strain data thus obtained minimize post-processing requirements, making the setup a candidate for real-time seismic monitoring. An analysis of the dispersion characteristics of the generated surface waves is performed using a recently reported optimised seismic interferometric technique. Based on the dispersion characteristics, the shear wave velocities of the surface waves as a function of the depth profile of the Earth’s crust are determined using an optimised evolutionary algorithm.
The statistical tool eCerto was developed for the evaluation of measurement data to assign property values and associated uncertainties of reference materials. The analysis is based on collaborative studies of expert laboratories and was implemented using the R software environment. Emphasis was put on comparability of eCerto with SoftCRM, a statistical tool based on the certification strategy of the former Community Bureau of Reference. Additionally, special attention was directed towards easy usability from data collection through processing, archiving, and reporting. While the effects of outlier removal can be flexibly explored, eCerto always retains the original data set and any manipulation such as outlier removal is (graphically and tabularly) documented adequately in the report. As a major reference materials producer, the Bundesanstalt für Materialforschung und -prüfung (BAM) developed and will maintain a tool to meet the needs of modern data processing, documentation requirements, and emerging fields of RM activity. The main features of eCerto are discussed using previously certified reference materials.
The ultrasonic echo technique is widely used in non-destructive testing (NDT) of concrete objects for thickness measurements, geometry determinations and localization of built-in components. To improve ultrasonic imaging of complex concrete structures, we transferred a seismic imaging technique, the Reverse Time Migration (RTM), to NDT in civil engineering. RTM, in contrast to the conventionally used synthetic aperture focusing technique (SAFT) algorithms, considers all wavefield types and thus, can handle complex wave propagations in any direction with no limit on velocity variations and reflector dip. In this paper, we focused on the development, application and evaluation of a two-dimensional elastic RTM algorithm considering horizontally polarized shear (SH) waves only. We applied the elastic SH RTM routine to synthetic ultrasonic echo SH-wave data generated with a concrete model incorporating several steps and circular cavities. As these features can often be found in real-world NDT use cases, their imaging is extremely important. By using elastic SH RTM, we were able to clearly reproduce almost all reflectors inside the concrete model including the vertical step edges and the cross sections of the cavities.We were also capable to show that more features could be mapped compared to SAFT, and that imaging of complex reflectors could be sharpened compared to elastic P-SV (compressional-vertically polarized shear) RTM. Our promising results illustrate that elastic SH RTM has the potential to significantly enhance the reconstruction of challenging concrete structures, representing an important step forward for precise, high-quality ultrasonic NDT in civil engineering.
The long-term leaching behavior of incineration bottom ash (IBA) was studied with large-scale samples from two German waste incinerators with grate technology. The observation period was up to 281 days. The aging processes proceeded faster in the outdoor storage of the samples. The dominant factor in the leaching behavior is the pH, which starts at values above 12 and decreases to values below 10 (outdoors, <11 indoors). Most heavy metals exhibit minimum solubility in this pH range. The solubility of Sb depends on the prevailing Ca concentration, due to the formation of low-soluble Ca antimonate. The very low sulfate concentrations observed in the leaching tests with fresh IBA could be explained by the presence of ettringite. In the course of the aging reaction, ettringite is transformed into gypsum. The results from batch tests were compared with those from column tests, showing reasonable agreement. Leaching dynamics can be better followed with column tests. All results confirm that the use of IBA is possible under German law.
Protein modifications such as oligomerization and tyrosine nitration alter the immune response to allergens and may contribute to the increasing prevalence of allergic diseases. In this mini-review, we summarize and discuss relevant findings for the major birch and grass pollen allergens Bet v 1 and Phl p 5 modified with tetranitromethane (laboratory studies), peroxynitrite (physiological processes), and ozone and nitrogen dioxide environmental conditions). We focus on tyrosine nitration and the formation of protein dimers and higher oligomers via dityrosine cross-linking and the immunological effects studied.
The digitalization of quality control processes and the underlying data infrastructures for safety relevant components, such as hydrogen pressure vessels, plays a significant role in the transition towards Industry 4.0. In the current safety regulations for hydrogen pressure vessels, there is no established concept for structural health monitoring. The development of a reliable structural health monitoring methodology for monitoring the structural integrity of pressure vessels enables a fast-forward transition from personnel- and costintensive recurring inspections, a.k.a. periodic maintenance, to predictive maintenance. In the work presented; we investigated the application of ultrasonic guided wave propagation to monitor and assess the condition of Type IV composite overwrapped pressure vessel (COPV). A sensor network of fifteen piezo-electric wafers is placed on the carbon fibre reinforced composite cylinder. Five different artificial damage configurations are created by gluing two different weight blocks on three different locations. The database containing measured guided wave data sets is enriched by two different boundary conditions. We utilized an open-source software, openBIS labnotebook, to store and analyse experimental datasets. The guided wave ultrasonic signals were investigated and analysed by using commonly used ultrasonic features (e.g., amplitude, frequency, time of flight) as well as non-traditional time-series features (kurtosis, skewness, variance). The features were used to calculate damage index and the detection performance for the results has been evaluated. The results suggest that both traditional and non-traditional features assume significant importance in artificial damage detection. The future works will additionally involve the impacts of operational conditions, such as periodic pressure variations temperature loadings as well as material degradations.
The application of composite overwrapped pressure vessels (COPV) to store hydrogen and other compressed gases, especially when operating at high pressures, imposed the need for an innovative and reliable approach to ensure the safe operation of the system. Continuous structural health monitoring (SHM) based on ultrasonic guided waves (GWs) is a promising approach due to the ability of the wave to propagate for long distances and go around complex structures, moreover the high sensitivity to various failure modes such as delamination, matrix cracking and debonding. In this study, we scrutinize the behavior of (GWs) within the COPV using a network of PZT elements that are used for excitation and sensing. A laser doppler vibrometer (LDV) was also used to scan the surface of the vessel in various directions. L(0,1) and L(0,2) were observed in the captured signal. The L(0, 2) appeared to be a dominant mode in the COPV and was capable of propagating along the entire length and maintaining a good signal-to-noise ratio. The L(0,2) mode maintained the same phase velocity when it is captured at various excitation angles (0, 45, and 90 degrees). The reduced effect of the orthotropy of the materials on the propagating waves is an important result as it will reduce the complexity in data processing when performing damage identification.
(1) Background: The desire to avoid autograft harvesting in implant dentistry has prompted an ever-increasing quest for bioceramic bone substitutes, which stimulate osteogenesis while resorbing in a timely fashion. Consequently, a highly bioactive silicon containing calcium alkali orthophosphate (Si-CAP) material was created, which previously was shown to induce greater bone cell maturation and bone neo-formation than β-tricalcium phosphate (β-TCP) in vivo as well as in vitro. Our study tested the hypothesis that the enhanced effect on bone cell function in vitro and in sheep in vivo would lead to more copious bone neoformation in patients following sinus floor augmentation (SFA) employing Si-CAP when compared to β-TCP. (2) Methods: The effects of Si-CAP on osteogenesis and Si-CAP resorbability were evaluated in biopsies harvested from 38 patients six months after SFA in comparison to β-TCP employing undecalcified histology, histomorphometry, and immunohistochemical analysis of osteogenic marker expression. (3) Results: Si-CAP as well as β-TCP supported matrix mineralization and bone formation. Apically furthest away from the original bone tissue, Si-CAP induced significantly higher bone formation, bone-bonding (bone-bioceramic contact), and granule resorption than β-TCP. This was in conjunction with a higher expression of osteogenic markers. (4) Conclusions: Si-CAP induced higher and more advanced bone formation and resorbability than β-TCP, while β-TCP’s remarkable osteoconductivity has been widely demonstrated. Hence, Si-CAP constitutes a well-suited bioactive graft choice for SFA in the clinical arena.
It is shown that preconditioning of experimental X‐ray computed tomography (XCT) data is critical to achieve high‐precision segmentation scores. The challenging experimental XCT datasets and deep convolutional neural networks (DCNNs) are used that are trained with low‐resemblance synthetic XCT data. The material used is a 6‐phase Al–Si metal matrix composite‐reinforced with ceramic fibers and particles. To achieve generalization, in our past studies, specific data augmentation techniques were proposed for the synthetic XCT training data. In addition, two toolsets are devised: (1) special 3D DCNN architecture (3D Triple_UNet), slicing the experimental XCT data from multiple views (MultiView Forwarding), the i.S.Sy.Da.T.A. iterative segmentation algorithm, and (2) nonlocal means (NLM) conditioning (filtering) for the experimental XCT data. This results in good segmentation Dice scores across all phases compared to more standard approaches (i.e., standard UNet architecture, single view slicing, standard single training, and NLM conditioning). Herein, the NLM filter is replaced with the deep conditioning framework BAM SynthCOND introduced in a previous publication, which can be trained with synthetic XCT data. This leads to a significant segmentation precision increase for all phases. The proposed methods are potentially applicable to other materials and imaging techniques.
The applications of composite overwrapped pressure vessels (COPVs) in extreme conditions, such as storing hydrogen gases at very high pressure, impose new requirements related to the system's integrity and safety. The development of a structural health monitoring (SHM) system that allows for continuous monitoring of the COPVs provides rich information about the structural integrity of the component. Furthermore, the collected data can be used for different purposes such as increasing the periodic inspection intervals, providing a remaining lifetime prognosis, and also ensuring optimal operating conditions. Ultimately this information can be complementary to the development of the envisioned digital twin of the monitored COPVs. Guided waves (GWs) are preferred to be used in continuous SHM given their ability to travel in complex structures for long distances. However, obtained GW signals are complex and require advanced processing techniques. Machine learning (ML) is increasingly utilized as the main part of the processing pipeline to automatically detect anomalies in the system's integrity. Hence, in this study, we are scrutinizing the potential of using ML to provide continuous monitoring of COPVs based on ultrasonic GW data. Data is collected from a network of sensors consisting of fifteen Piezoelectric (PZT) wafers that were surface mounted on the COPV. Two ML algorithms are used in the automated evaluation procedure (i) a long short-term memory (LSTM) autoencoder for anomaly detection (defects/impact), and (ii) a convolutional neural network (CNN) model for feature extraction and classification of the artificial damage sizes and locations. Additional data augmentation steps are introduced such as modification and addition of random noise to original signals to enhance the model's robustness to uncertainties. Overall, it was shown that the ML algorithms used were able to detect and classify the simulated damage with high accuracy.
We report the selective ring opening copolymerisation (ROCOP) of
oxetane and phthalic thioanhydride by a heterobimetallic Cr(III)K
catalyst precisely yielding semi-crystalline alternating poly(esteralt-
thioesters) which show improved degradability due to the
thioester links in the polymer backbone.
LIBS‐ConSort: Development of a sensor‐based sorting method for construction and demolition waste
(2023)
AbstractA joint project of partners from industry and research institutions approaches the challenge of construction and demolition waste (CDW) sorting by investigating and testing the combination of laser‐induced breakdown spectroscopy (LIBS) with near‐infrared (NIR) spectroscopy and visual imaging. Joint processing of information (data fusion) is expected to significantly improve the sorting quality of various materials like concrete, main masonry building materials, organic components, etc., and may enable the detection and separation of impurities such as SO3‐cotaining building materials (gypsum, aerated concrete, etc.)Focusing on Berlin as an example, the entire value chain will be analyzed to minimize economic / technological barriers and obstacles at the cluster level and to sustainably increase recovery and recycling rates.The objective of this paper is to present current progress and results of the test stand development combining LIBS with NIR spectroscopy and visual imaging. In the future, this laboratory prototype will serve as a fully automated measurement setup to allow real‐time classification of CDW on a conveyor belt.
Steelmaking slag is a by-product of steel production, of which 4.5 Mt were produced in 2020 in Germany alone. It is mainly used in road construction, earthwork and hydraulic engineering. A smaller part is returned to the metallurgical cycle, used as fertiliser or landfilled.
With this use, iron oxides still contained in steelmaking slag are lost. In addition, the possibility of producing higher-grade products from steelmaking slag is foregone. In recent decades, many researchers have investigated the production of Portland cement clinker and crude iron from basic oxygen furnace slags (BOFS) via a reductive treatment. Carbothermal treatment of liquid BOFS causes a reduction of iron oxides to metallic iron, which separates from the mineral phase due to its higher density. Simultaneously, the chemical composition of the reduced slag is adapted to that of Portland cement clinker.
In this study, German BOFS was reduced in a small-scale electric arc furnace using petrol coke as a reducing agent. The resulting low-iron mineral product has a similar chemical composition to Portland cement clinker and was rich in the tricalcium silicate solid solution alite (Ca3SiO5). Based on its chemical and mineralogical composition, similar to that of Portland cement clinker, the reduced BOFS has the potential to react comparably. In our study, the reduced BOFS produced less hydration heat than OPC, and its hydraulic reaction was delayed. However, adding gypsum has shown to accelerate the hydration rate of the reduced BOFS compared to that known from the calcium silicates of Portland cement clinker.
Further research to improve the hydraulic properties of the reduced slag is essential. If successful, producing a hydraulic binder and crude iron from BOFS has economic and ecological benefits for both the cement and steel industries.
Trace element (TE) analysis of pyrite via LA-ICP-MS can be used to reconstruct the conditions of pyrite formation in complex mineral systems. The Carpentaria province in northern Australia is host to some of the world’s highest value Zn-Pb (+Ag, Cu) deposits. The genesis of many of these deposits is controversial, with competing models of single-vs. multi-stage ore formation. In this study, LA-ICP-MS data of paragenetically constrained pyrite from the George Fisher Zn-Pb-Ag deposit has been analysed to investigate the chemistry of different stages of ore formation. Pyrite from correlative unmineralized host rocks has also been analysed to investigate evidence of distal hydrothermal anomalism. All LA-ICP-MS data have been statistically evaluated (principal component analysis) and interpreted together with whole rock lithogeochemical data of the same samples. Pre-ore diagenetic pyrite is compositionally similar to other Proterozoic diagenetic pyrite, with some evidence of minor hydrothermal anomalism that with further analysis could help define distal alteration. Pyrite from the different ore stages are compositionally distinct, consistent with a multi-stage system. Ore stage 1 pyrite exceeds background contents of Co, Cu, Zn, As, Ag, Sb, Tl, and Pb and has elevated Co/Ni ratios, whereas only Ni and Co are above background abundances in ore stage 2 and 3 pyrite, of which only ore stage 3 pyrite has high Co/Ni ratios. Ore stage 1 pyrite has a similar composition to hydrothermal pyrite in the undeformed northern Carpentaria CD-type deposits and was likely syn-diagenesis. Ore stage 2 was syn-deformation, and resulted in replacement and recrystallization of pre-existing pyrite, and the expulsion of incompatible TEs. Ore stage 3 formed via a later Cu-Zn-Pb mineralizing event that resulted in a new geochemically distinct generation of Co-rich pyrite. Overall, this study demonstrates the value of paragenetically-constrained pyrite TE data for refining genetic models in complex sediment hosted mineral systems.
Molten sulfur is found in various subaerial volcanoes. However, limited records of the pools and flows of molten sulfur have been reported: therefore, questions remain regarding the physicochemical processes behind this phenomenon. A suite of new sulfur flows, some of which active, was identified at the Lastarria volcano (northern Chile) and studied using satellite imagery, in situ probing, and temperature and video recording. This finding provides a unique opportunity to better understand the emplacement mechanisms and mineral and chemical compositions of molten sulfur, in addition to gaining insight into its origin. Molten sulfur presented temperatures of 124–158°C, with the most prolonged sulfur flow reaching 12 m from the source. Photogrammetric tools permitted the identification of levees and channel structures, with an estimated average flow speed of 0.069 m/s. Field measurements yielded a total volume of 1.45 ± 0.29 m3 of sulfur (equivalent to ∼2.07 tons) mobilized during the January 2019 event for at least 408 min. Solidified sulfur was composed of native sulfur with minor galena and arsenic- and iodine-bearing minerals. Trace element analysis indicated substantial enrichment of Bi, Sb, Sn, Cd, as well as a very high concentration of As (&gt;40.000 ppm). The January 2019 molten sulfur manifestations in Lastarria appear to be more enriched in As compared to the worldwide known volcanoes with molten sulfur records, such as the Shiretoko-Iozan and Poás volcanoes. Furthermore, their rheological properties suggest that the “time of activity” in events such as this could be underestimated as flows in Lastarria have moved significantly slower than previously thought. The origin of molten sulfur is ascribed to the favorable S-rich chemistry of fumarolic gases and changes in host rock permeability (fracture opening). Molten sulfur in Lastarria correlates with a peak in activity characterized by high emissions of SO2 and other acid species, such as HF and HCl, in addition to ground deformation. Consequently, molten sulfur was framed within a period of volcanic unrest in Lastarria, triggered by changes in the magmatic-hydrothermal system. The appearance of molten sulfur is related to physicochemical perturbations inside the volcanic system and is perhaps a precursor of eruptive activity, as observed in the Poás and Turrialba volcanoes.
Synthesis of Li ion battery materials via ball milling has been a huge area of growth, leading to new high-capacity electrode materials, such as a number of promising disordered rocksalt (DRS) phases. In prior work, it was generally assumed that the synthesis was facilitated simply by local heating effects during the milling process. In this work, we show that ball milling Li2MoO4 leads to a phase transformation to the high pressure spinel polymorph and we report electrochemical data for this phase. This observation of the formation of a high pressure polymorph shows that local heating effects alone cannot explain the phase transformation observed (phenakite to spinel) and so indicates the importance of other effects. In particular, we propose that when the milling balls collide with the material, the resulting shockwaves exert a localised pressure effect, in addition to local heating. To provide further support for this, we additionally report ball milling results for a number of case studies (Li2MnO3, Li2SnO3, Nb2O5) which reinforces the conclusion that local heating alone cannot explain the phase transformations observed. The work presented thus provides greater fundamental understanding of milling as a synthetic pathway and suggests potential strategies to prepare such samples without milling (e.g., doping to create internal chemical pressure). In addition, we suggest that further research is needed into the effect of the use of milling as a route to smaller particles, since we believe that such milling may also be affecting the surface structure of the particles through the influence of the shockwaves generated.
This data article introduces a dataset comprising 1630 alkali-activated concrete (AAC) mixes, compiled from 106 literature sources. The dataset underwent extensive curation to address feature redundancy, transcription errors, and duplicate data, yielding refined data ready for further data-driven science in the field of AAC, where this effort constitutes a novelty. The carbon footprint associated with each material used in the AAC mixes, as well as the corresponding CO2 footprint of every mix, were approximated using two published articles. Serving as a foundation for future expansions and rigorous data applications, this dataset enables the characterization of AAC properties through machine learning algorithms or as a benchmark for performance comparison among different formulations. In summary, the dataset provides a resource for researchers focusing on AAC and related materials and offers insights into the environmental benefits of substituting traditional Portland concrete with AAC.
In recent decades, the number of components in concrete has grown, particularly in formulations aimed at reducing carbon footprints. Innovations include diverse binders, supplementary cementitious materials, activators, concrete admixtures, and recycled aggregates. These developments target not only the enhancement of material properties but also the mitigation of the ecological and economic impacts of concrete — the most extensively used material by humankind. However, these advancements also introduce a greater variability in the composition of raw materials. The material’s behavior is significantly influenced by its nanoscale properties, which can pose challenges in accurate characterization. Consequently, there’s an increasing need for experimental tuning of formulations. This is accompanied by a more inconsistent composition of raw materials, which makes an experimental tuning of formulations more and more necessary. However, the increased complexity in composition presents a challenge in finding the ideal formulation through trial and error. Inverse design (ID) techniques offer a solution to this challenge by allowing for a comprehensive search of the entire design space to create new and improved concrete formulations. In this publication, we introduce the concept of ID and demonstrate how our open-source app “SLAMD” provides all necessary steps of the workflow to adapt it in the laboratory, lowering the application barriers. The intelligent screening process, guided by a predictive model, leads to a more efficient and effective data-driven material design process resulting in reduced carbon footprint and improved material quality while considering socio-economic factors in the materials design.
Large-language models (LLMs) such as GPT-4 caught the interest of many scientists. Recent studies suggested that these models could be useful in chemistry and materials science. To explore these possibilities, we organized a hackathon. This article chronicles the projects built as part of this hackathon. Participants employed LLMs for various applications, including predicting properties of molecules and materials, designing novel interfaces for tools, extracting knowledge from unstructured data, and developing new educational applications. The diverse topics and the fact that working prototypes could be generated in less than two days highlight that LLMs will profoundly impact the future of our fields. The rich collection of ideas and projects also indicates that the applications of LLMs are not limited to materials science and chemistry but offer potential benefits to a wide range of scientific disciplines.
Titanium and its alloys are known to allow the straightforward laser-based manufacturing of ordered surface nanostructures, so-called high spatial frequency laser-induced periodic surface structures (HSFL). These structures exhibit sub-100 nm spatial periods – far below the optical diffraction limit. The resulting surface functionalities are usually enabled by both, topographic and chemical alterations of the nanostructured surfaces. For exploring these effects, multi-method characterizations were performed here for HSFL processed on Ti–6Al–4V alloy upon irradiation with near-infrared ps-laser pulses (1030 nm, ≈1 ps pulse duration, 1–400 kHz) under different laser scan processing conditions, i.e., by systematically varying the pulse repetition frequency and the number of laser irradiation passes. The sample characterization involved morphological and topographical investigations by scanning electron microscopy (SEM), atomic force microscopy (AFM), tactile stylus profilometry, as well as near-surface chemical analyses hard X-ray photoelectron spectroscopy (HAXPES) and depth-profiling time-of-flight secondary ion mass spectrometry (ToF-SIMS). This provides a quantification of the laser ablation depth, the geometrical HSFL characteristics and enables new insights into the depth extent and the nature of the non-ablative laser-induced near-surface oxidation accompanying these nanostructures. This allows to answer the questions how the processing of HSFL can be industrially scaled up, and whether the latter is limited by heat-accumulation effects.
Although the use of noble metal catalysts can increase the efficiency of hydrogen evolution reaction, the process is still limited by the characteristics of the metal-hydrogen (M−H) bond, which can be too strong or too weak, depending on the metal employed. Studies revealed that the hydrogen affinity for the metal surface (i.e. H absorption/desorption) is regulated also by the potential at the metal nanoparticles. Through controlled periodic illumination (CPI) of a series of metal/TiO2 suspensions, here we demonstrated that an increase of the HER efficiency is possible for those photodeposited metals which have a Tafel slope below 125 mV. Two possible explanations are here reported, in both of them the M−H interaction and the metal covering level play a prominent role, which also depend on the prevailing HER mechanism (Volmer-Heyrovsky or Volmer-Tafel).
Even after autoclaving for 2 weeks in the temperature range of 120 to 200 °C, CEM I paste with a water-to-cement ratio of 0.5 still contains some low-crystalline C-S-H. The conversion of low-crystalline C-S-H to crystalline is faster with increasing temperature. The observed low-crystalline and crystalline C-S-H phases (reinhardbraunsite, jaffeite) indicate that the sampleshave not reached equilibrium yet under these experimental conditions. However, there is a good agreement between experiment and thermodynamic modelling for the other solids indicating that the used datasets are suitable for this application.
AbstractIn this study, we present a screening method based on molecular absorption spectrometry to study PFAS uptake and fate in plants. To evaluate the suitability of this method we analyzed plant extracts with molecular absorption spectrometry (MAS) as well as liquid chromatography–tandem mass spectrometry (LC–MS/MS) for mass balance studies (w(F)). French bean plants (Phaseolus vulgaris) were grown on soil spiked using eight PFAS substances that vary in chain length and functional group composition. Specifically, these include three short-chained (C4–C5), five long-chained (C7–C10) carboxylic acids, one sulfonic acid and one sulfonic amide moieties. To investigate substance-specific PFAS uptake systematically, PFAS were spiked as single substance spike. Additionally, we studied one mixture of the investigated substances in equal proportions regarding w(F) and four PFAS mixtures of unknown composition. After 6 weeks, the plants were separated into four compartments. We analyzed the four compartments as well as the soil for extractable organically bound fluorine (EOF) by high resolution-continuum source-graphite furnace-molecular absorption spectrometry (HR-CS-GFMAS) as well as for sum of ten target-PFAS by LC–MS/MS. All three short-chained PFAS perfluorobutanoic acid (PFBA), perfluorobutanoic sulfonic acid (PFBS) and perfluoropentanoic acid (PFPeA) were determined in high concentrations mainly in the fruits of the investigated plants while long-chained PFAS perfluorononanoic acid (PFNA) and perfluorodecanoic acid (PFDA) were mainly determined in roots. PFBS was determined in remarkably high concentrations in leaves compartment by both quantification methods. Overall, comprehensive results of single substance spikes were in good agreement for both methods except for a few cases. Hence, two phenomena were identified: for mixed PFAS spikes of unknown composition huge differences between EOF and sum of target PFAS were observed with systematically higher EOF values. Overall, both methods indicate comparable results with MS being more reliable for known PFAS contamination and MAS being more valuable to identify PFAS exposure of unknown composition.
Graphical Abstract
The degradation of a single-site atomically dispersed, model Fe–N–C powder catalyst with high activity is investigated using cryo-Mössbauer spectroscopy. The results indicate a degradation initiated by an Fe2+ to Fe3+ oxidation due to coordination of oxygen to tetrapyrrolic Fe–N4 sites at atmospheric conditions (change between characteristic doublets) before iron(III) oxide is formed (sextet). Thermal reactivation can be used to restore substantial catalytic activity of aged Fe–N–C powders.
The lack of traceability to meter of X-ray Computed Tomography (CT) measurements still hinders a more extensive acceptance of CT in coordinate metrology and industry. To ensure traceable, reliable, and accurate measurements, the determination of the task-specific measurement uncertainty is necessary. The German guideline VDI/VDE 2630 part 2.1 describes a procedure to determine the measurement uncertainty for CT experimentally by conducting several repeated measurements with a calibrated test specimen. However, this experimental procedure is cost and effort intensive. Therefore, the simulation of dimensional measurement tasks conducted with X-ray computed tomography can close these drawbacks. Additionally, recent developments towards a resource and cost-efficient production (“smart factory”) motivate the need for a corresponding numerical model of a CT system (“digital twin”) as well. As there is no standardized procedure to determine the measurement uncertainty of a CT system by simulation at the moment, the project series CTSimU was initiated, aiming at this gap. Concretely, the goal is the development of a procedure to determine the measurement uncertainty numerically by radiographic simulation. The first project (2019-2022), "Radiographic Computed Tomography Simulation for Measurement Uncertainty Evaluation - CTSimU" developed a framework to qualify a radiographic simulation software concerning the correct simulation of physical laws and functionalities. The most important outcome was a draft for a new guideline VDI/VDE 2630 part 2.2, which is currently under discussion in the VDI/VDE committee. The follow-up project CTSimU2 "Realistic Simulation of real CT systems with a basic-qualified Simulation Software" will deal with building and characterizing a digital replica of a specific real-world CT system. The two main targets of this project will be a toolbox including methods and procedures to configure a realistic CT system simulation and to develop tests to check if this replica is sufficient enough. The result will be a draft for a follow-up VDI/VDE guideline proposing standardized procedures to determine a CT system's corresponding characteristics and test the simulation (copy) of a real-world CT system which we call a "digital twin".
We show that mechanochemically driven polymorphic transformations can require extremely long induction periods, which can be tuned from hours to days by changing ball milling energy. The robust design and interpretation of ball milling experiments must account for this unexpected kinetics that arises from energetic phenomena unique to the solid state. Detailed thermal analysis, combined with DFT simulations, indicates that these marked induction periods are associated with processes of mechanical activation. Correspondingly, we show that the pre‐activation of reagents can also lead to marked changes in the length of induction periods. Our findings demonstrate a new dimension for exerting control over polymorphic transformations in organic crystals. We expect mechanical activation to have a much broader implication across organic solid‐state mechanochemistry.
Due to their favorable properties and high porosity, zeolitic imidazolate frameworks (ZIFs) have recently received much limelight for key technologies such as energy storage, optoelectronics, sensorics, and catalysis. Despite widespread interest in these materials, fundamental questions regarding the zinc coordination environment remain poorly understood. By focusing on zinc(II)2-methylimidazolate (ZIF-8) and its tetrahedrally coordinated analogues with Br-, Cl-, and H-substitution in the 2-ring position, we aim to clarify how variations in the local environment of Zn impact the charge distribution and the electronic properties of these materials. Our results from densityfunctional theory confirm the presence of a Zn coordinative bond with a large polarization that is quantitatively affected by different substituents on the organic ligand. Moreover, our findings suggest that the variations in the Zn coordination induced by the functionalization have a negligible effect on the electronic structure of the considered compounds. On the other hand, halogen terminations of the ligands lead to distinct electronic contributions in the vicinity of the frontier region which ultimately reduce the band gap size by a few hundred millielectron volts. Experimental results obtained from X-ray absorption spectroscopy (Zn K-edge) confirm the trends predicted by theory and, together with them, contribute to a better understanding of the structure−property relationships that are needed to tailor ZIFs for target applications.
The process of viscous flow sintering is a phenomenon that is closely linked to the surface properties of the glass particles. In this work, we studied the extreme case of acid-leaching of soda-lime-silicate glass beads of two different particle size distributions and its effects on non-isothermal viscous sintering of powder compacts. Depth profiling of the chemical composition after leaching revealed a near-surface layer depleted in alkali and alkaline earth ions, associated with concurrent hydration as mass loss was detected by thermogravimetry. Heating microscopy showed that acid treatment of glasses shifted the sinter curves to higher temperatures with increasing leaching time. Modelling of the shrinkage with the cluster model predicted a higher viscosity of the altered surface layer, while analysis of the time scales of mass transport of mobile species (Na+, Ca2+ and H2O) during isochronous sintering revealed that diffusion of Na+ can compensate for concentration gradients before sintering begins. Also, exchanged water species can diffuse out of the altered layer, but the depletion of Ca2+ in the altered surface layer persists during the sinter interval, resulting in a glass with higher viscosity, which causes sintering to slow down.
Laser-induced periodic surface structures (LIPSS) represent a unique route for functionalizing materials through the fabrication of surface nanostructures. Commercial AISI 316L stainless steel (SS316L) surfaces are laser treated by ultraviolet 300 ps laser pulses in a laser line scanning (LLS) approach. Processing parameters are optimized (pulse energy of 2.08 µJ, pulse repetition frequency of 300 kHz, and suitable laser scan and sample displacement rates) for the generation of low spatial frequency LIPSS over a large 25 × 25 mm2 area. Different angles of incidence of the laser radiation (0°, 30°, and 45°) and different linear laser beam polarizations (s and p) produce a plethora of rippled surface morphologies at distinct grains. Scanning electron microscopy and 2D Fourier transforms, together with calculations of the optical energy deposited at the treated surfaces using Sipe's first-principles electromagnetic scattering theory, are used to study and analyze in detail these surface morphologies. Combined with electron backscattering diffraction, analyses allow associating site-selectively various laser-induced-surface morphologies with the underlying crystalline grain orientation. Resulting grain orientation maps reveal a strong impact of the grain crystallographic orientation on LIPSS formation and point toward possible strategies, like multi-step processes, for improving the manufacturing of LIPSS and their areal coverage of polycrystalline technical materials.
AbstractThis work addresses the critical need for multifunctional materials and substrate‐independent high‐precision surface modification techniques that are essential for advancing microdevices and sensing elements. To overcome existing limitations, the versatility of mussel‐inspired materials (MIMs) is combined with state‐of‐the‐art multiphoton direct laser writing (DLW) microfabrication. In this way, 2D and 3D MIM microstructures of complex designs are demonstrated with sub‐micron to micron resolution and extensive post‐functionalization capabilities. This study includes polydopamine (PDA), mussel‐inspired linear, and dendritic polyglycerols (MI‐lPG and MI‐dPG), allowing their direct microstructure on the substrate of choice with the option to tailor the patterned topography and morphology in a controllable manner. The functionality potential of MIMs is demonstrated by successfully immobilizing and detecting single‐stranded DNA on MIM micropattern and nanoarray surfaces. In addition, easy modification of MIM microstructure with silver nanoparticles without the need of any reducing agent is shown. The methodology developed here enables the integration of MIMs in advanced applications where precise surface functionalization is essential.
Ergot alkaloids are a group of toxic compounds, formed by fungi on infested grasses. In 2022, the European Commission set into effect maximum levels for the sum of the twelve major ergot alkaloids in multiple foods. To facilitate the laborious and costly individual quantification of the twelve major ergot alkaloids by HPLC–MS/MS or -FLD, we recently reported a sum parameter method (SPM) for ergot alkaloid quantification. Here, derivatization to lysergic acid hydrazide—a derivative of the mutual ergoline backbone in all ergot alkaloids—allowed simplified determination of all ergot alkaloids in flour via HPLC-FLD. For the measurement of more complex matrices like processed foods, we now developed a MS/MS-based SPM. Two internal standards (IS), isotopically labelled at different positions of the molecule, were synthesized and employed in the MS/MS-measurements. Method performance using either the 13CD3-labelled or the 15N2-labelled IS was evaluated on naturally contaminated rye and wheat flour samples as well as on processed food matrices. Employing the 13CD3-labelled IS leads to lower variances and better consistency with the reference data (obtained by the FLD-based SPM) in flour samples compared to the 15N2-labelled IS. The novel method significantly improves the measurement of ergot alkaloids in complex food matrices, due to their increased selectivity and thus lower interferences. Furthermore, the application of isotope labelled IS obviates the need for time-consuming steps like the determination of recovery rate based, matrix specific correction factors as described in the MS/MS-based European standard method for ergot alkaloid quantification (EN 17425).
Li dendrites penetration through solid electrolytes (SEs) challenges the development of solid-state Li batteries (SSLBs). To date, significant efforts are devoted to understand the mechanistic dynamics of Li dendrites nucleation, growth, and propagation in SEs, and various strategies that aim to alleviate and even inhibit Li dendrite formation have been proposed. Nevertheless, most of these conventional strategies require either additional material processing steps or new materials/layers that eventually increase battery cost and complexity. In contrast, using external fields, such as mechanical force, temperature physical field, electric field, pulse current, and even magnetic field to regulate Li dendrites penetration through SEs, seems to be one of the most cost-effective strategies. This review focuses on the current research progress of utilizing external physical fields in regulating Li dendrites growth in SSLBs. For this purpose, the mechanical properties of Li and SEs, as well as the experimental results that visually track Li penetration dynamics, are reviewed. Finally, the review ends with remaining open questions in future studies of Li dendrites growth and penetration in SEs. It is hoped this review can shed some light on understanding the complex Li dendrite issues in SSLBs and potentially guide their rational design for further development.
Bacterial biofilms pose serious problems in medical and industrial settings. One of the major societal challenges lies in the increasing resistance of bacteria against biocides used in antimicrobial treatments, e.g., via overabundant use in medicine, industry, and agriculture or cleaning and disinfection in private households. Hence, new efficient bacteria-repellent strategies avoiding the use of biocides are strongly desired. One promising route to achieve bacteria-repellent surfaces lies in the contactless and aseptic large-area laser-processing of technical surfaces. Tailored surface textures, enabled by different laser-processing strategies that result in topographic scales ranging from nanometers to micrometers may provide a solution to this challenge. This article presents a current state-of-the-art review of laser-surface subtractive texturing approaches for controlling the biofilm formation for different bacterial strains and in different environments. Based on specific properties of bacteria and laser-processed surfaces, the challenges of anti-microbial surface designs are discussed, and future directions will be outlined.
Methane emission by terrestrial invertebrates is restricted to millipedes, termites, cockroaches, and scarab beetles. The arthropod-associated archaea known to date belong to the orders Methanobacteriales, Methanomassiliicoccales, Methanomicrobiales, and Methanosarcinales, and in a few cases also to nonmethanogenic Nitrososphaerales and Bathyarchaeales. However, all major host groups are severely undersampled, and the taxonomy of existing lineages is not well developed. Full-length 16S rRNA gene sequences and genomes of arthropod-associated archaea are scarce, reference databases lack resolution, and the names of many taxa are either not validly published or under-classified and require revision. Here, we investigated the diversity of archaea in a wide range of methane-emitting arthropods, combining phylogenomic analysis of isolates and metagenome-assembled genomes (MAGs) with amplicon sequencing of full-length 16S rRNA genes. Our results allowed us to describe numerous new species in hitherto undescribed taxa among the orders Methanobacteriales (Methanacia, Methanarmilla, Methanobaculum, Methanobinarius, Methanocatella, Methanoflexus, Methanorudis, and Methanovirga, all gen. nova), Methanomicrobiales (Methanofilum and Methanorbis, both gen. nova), Methanosarcinales (Methanofrustulum and Methanolapillus, both gen. nova), Methanomassiliicoccales (Methanomethylophilaceae fam. nov., Methanarcanum, Methanogranum, Methanomethylophilus, Methanomicula, Methanoplasma, Methanoprimaticola, all gen. nova), and the new family Bathycorpusculaceae (Bathycorpusculum gen. nov.). Reclassification of amplicon libraries from this and previous studies using this new taxonomic framework revealed that arthropods harbor only CO2 and methyl-reducing hydrogenotrophic methanogens.
Numerous genus-level lineages appear to be present exclusively in arthropods,suggesting long evolutionary trajectories with their termite, cockroach, and millipede hosts, and a radiation into various microhabitats and ecological nichesprovided by their digestive tracts (e.g., hindgut compartments, gut wall, or anaerobic protists). The distribution patterns among the different host groups are often complex, indicating a mixed mode of transmission and a parallel evolution of invertebrate and vertebrate-associated lineages.
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.
AbstractWe report on gold clusters with around 62 gold atoms and a diameter of 1.15±0.10 nm. Dispersions of the clusters are long‐term stable for two years at ambient conditions. The synthesis was performed by mixing tetrachloroauric acid (HAuCl4 ⋅ 3 H2O) with the ionic liquid 1‐ethyl‐3‐methylimidazolium dicyanamide ([Emim][DCA]) at temperatures of 20 to 80 °C. Characterization was performed with small‐angle X‐ray scattering (SAXS), UV‐Vis spectroscopy, and MALDI‐TOF mass spectrometry. A three‐stage model is proposed for the formation of the clusters, in which cluster growth from gold nuclei takes place according to the Lifshitz‐Slyozov‐Wagner (LSW) model followed by oriented attachment to form colloidal stable clusters.
Gold-based nanoparticles below 2 nm in size are promising as luminescent probes for in vivo bioimaging, owing to their brightness and rapid renal clearance. However, their use as contrast agents in the near-infrared II (NIR-II, 1000–1700 nm) range remains challenging due to their low photoluminescence (PL) quantum yield. To address this, PL enhancement can be achieved by either rigidifying the ligand-shell structure or increasing the size of the ligand shell. In this study, we synthesized ultra-small gold nanoparticles stabilized by co-ligands, namely monothiol and short dithiol molecules. By precisely controlling the amount of reducing agent used during particle preparation, we successfully modulated the physicochemical properties of the co-ligand shell, including its size, composition, and structure. Consequently, we achieved a remarkable 60-fold increase in the absorption cross-section at 990 nm while maintaining the small size of the 1.5-nm metal core. The analytical and optical characterization of our thiol-capped gold nanoparticles indicates that the ligand shell size is governed by the quantity of the reducing agent, which, in turn, impacts the balance between radiative and non-radiative processes, thereby influencing the PL quantum yield.
Early detection of cancer is essential for successful treatment and improvement in patient prognosis. Deregulation of post-translational modifications (PTMs) of proteins, especially phosphorylation, is present in many types of cancer. Therefore, the development of materials for the rapid sensing of low abundant phosphorylated peptides in biological samples can be of great therapeutic value. In this work, we have synthesised fluorescent molecularly imprinted polymers (fMIPs) for the detection of the phosphorylated tyrosine epitope of ZAP70, a cancer biomarker. The polymers were grafted as nanometer-thin shells from functionalised submicron-sized silica particles using a reversible addition-fragmentation chain-transfer (RAFT) polymerisation. Employing the combination of fluorescent urea and intrinsically cationic bis-imidazolium receptor cross-linkers, we have developed fluorescent sensory particles, showing an imprinting factor (IF) of 5.0. The imprinted polymer can successfully distinguish between phosphorylated and non-phosphorylated tripeptides, reaching lower micromolar sensitivity in organic solvents and specifically capture unprotected peptide complements in a neutral buffer. Additionally, we have shown the importance of assessing the influence of counterions present in the MIP system on the imprinting process and final material performance. The potential drawbacks of using epitopes with protective groups, which can co-imprint with targeted functionality, are also discussed.
Mechanochemistry has proven to be a highly effective method for the synthesis of organic compounds. We studied the kinetics of the catalyst-free Knoevenagel reaction between 4-nitrobenzaldehyde and malononitrile, activated and driven by ball milling. The reaction was investigated in the absence of solvents (neat grinding) and in the presence of solvents with different polarities (liquid-assisted grinding). The reaction was monitored using time-resolved in situ Raman spectroscopy and powder X-ray diffraction (PXRD). Our results indicate a direct relationship between solvent polarity and reaction kinetics, with higher solvent polarity leading to faster product (2-(4-nitrobenzylidone)malononitrile) formation. For the first time, we were able to isolate and determine the structure of an intermediate 2-(hydroxy(4-nitrophenyl)methyl)malononitrile based on PXRD data.
The effect of the oscillating metal vapor plume on the keyhole and molten pool behavior during the laser beam welding of AlMg3 aluminum alloys is investigated by experimental and numerical methods. The real-time height of the metal vapor plume is measured by high-speed camera observation. The obtained experimental results are used to evaluate the additional heating source and laser beam attenuation caused by the scattering and absorption based on the Beer–Lambert theory. Furthermore, the dynamic behavior of the metal vapor plume is incorporated into a 3D transient heat transfer and fluid flow model, coupled with the ray tracing method, for the laser beam welding of the AlMg3 alloy. It is found that additional heating resulting from the scattered and absorbed laser beam energy by the metal vapor plume significantly expands the shape of the molten pool on the top region. Moreover, the oscillating metal vapor plume caused the fluctuation of the high-temperature region in the molten pool. The probability of keyhole collapse at the bottom increases 17% due to the oscillating laser power induced by the laser beam attenuation. The internal interplay between the metal vapor plume, molten pool shape, and keyhole collapse is obtained. The developed model has been validated by experiments, which shows a good agreement.
La(FexSi1−x)13 and derived quaternary compounds are well-known for their giant, tunable, magneto- and barocaloric responses around a first-order paramagnetic-ferromagnetic transition near room temperature with low hysteresis. Remarkably, such a transition shows a large spontaneous volume change together with itinerant electron metamagnetic features. While magnetovolume effects are well-established mechanisms driving first-order transitions, purely electronic sources have a long, subtle history and remain poorly understood. Here we apply a disordered local moment picture to quantify electronic and magnetoelastic effects at finite temperature in La(FexSi1−x)13 from first-principles. We obtain results in very good agreement with experiment and demonstrate that the magnetoelastic coupling, rather than purely electronic mechanisms, drives the first-order character and causes at the same time a huge electronic entropy
contribution to the caloric response.
Tailoring negative pressure by crystal defects: Microcrack induced hydride formation in Al alloys
(2023)
Climate change motivates the search for non-carbon-emitting energy generation and storage solutions. Metal hydrides show promising characteristics for this purpose. They can be further stabilized by tailoring the negative pressure of microstructural and structural defects. Using systematic ab initio and atomistic simulations, we demonstrate that an enhancement in the formation of hydrides at the negatively pressurized tip region of the microcrack is feasible by increasing the mechanical tensile load on the specimen. The theoretical predictions have been used to reassess and interpret atom probe tomography experiments for a high-strength 7XXX-aluminium alloy that show a substantial enhancement of hydrogen concentration at structural defects near a stress-corrosion crack tip. These results contain important implications for enhancing the capability of metals as H-storage materials.
Research on per- and polyfluoroalkyl substances (PFAS) frequently incorporates organofluorine measurements, particularly because they could support a class-based approach to regulation. However, standardized methods for organofluorine analysis in a broad suite of matrices are currently unavailable, including a method for extractable organofluorine (EOF) measured using combustion ion chromatography (CIC). Here, we report the results of an international interlaboratory comparison. Seven laboratories representing academia, government, and the private sector measured paired EOF and PFAS concentrations in groundwater and eel (Anguilla rostrata) from a site contaminated by aqueous film-forming foam. Among all laboratories, targeted PFAS could not explain all EOF in groundwater but accounted for most EOF in eel. EOF results from all laboratories for at least one replicate extract fell within one standard deviation of the interlaboratory mean for groundwater and five out of seven laboratories for eel. PFAS spike mixture recoveries for EOF measurements in groundwater and eel were close to the criterion (±30%) for standardized targeted PFAS methods. Instrumental operation of the CIC such as replicate sample injections was a major source of measurement uncertainty. Blank contamination and incomplete inorganic fluorine removal may introduce additional uncertainties. To elucidate the presence of unknown organofluorine using paired EOF and PFAS measurements, we recommend that analysts carefully consider confounding methodological uncertainties such as differences in precision between measurements, data processing steps such as blank subtraction and replicate analyses, and the relative recoveries of PFAS and other fluorine compounds.
In the present study, in-situ observation of Hot Isostatic Pressure (HIP) procedure of laser powder bed fusion manufactured Ti-6Al-4V parts was performed to quantitatively estimate the densifcation rate of the material and the infuence of the defect initial size and shape on such rate. The observations were performed in-situ using the Ultrafast Tomography Paris-Edinburgh Cell and the combination of fast phase-contrast synchrotron X-ray tomography and energy dispersive difraction. With this strategy, we could quantify how the efectiveness of HIP depends on the characteristics of a defect. Smaller defects showed a higher densifcation rate, while the defect shape did not have signifcant efect on such rate.
Bacterial biofilms can pose a serious health risk to humans and are less susceptible
to antibiotics and disinfection than planktonic bacteria. Here, a novel method
for biofilm eradication based on antimicrobial photodynamic therapy utilizing
a nanoparticle in conjunction with a BODIPY derivative as photosensitizer was
developed. Reactive oxygen species are generated upon illumination with
visible light and lead to a strong, controllable and persistent eradication of
both planktonic bacteria and biofilms. One of the biggest challenges in biofilm
eradication is the penetration of the antimicrobial agent into the biofilm and
its matrix. A biocompatible hydrophilic nanoparticle was utilized as a delivery
system for the hydrophobic BODIPY dye and enabled its accumulation within the
biofilm. This key feature of delivering the antimicrobial agent to the site of action
where it is activated resulted in effective eradication of all tested biofilms. Here,
3 bacterial species that commonly form clinically relevant pathogenic biofilms
were selected: Escherichia coli, Staphylococcus aureus and Streptococcus
mutans. The development of this antimicrobial photodynamic therapy tool for
biofilm eradication takes a promising step towards new methods for the much
needed treatment of pathogenic biofilms.
The spatial laser energy absorption inside the keyhole is decisive for the dynamic molten pool behaviors and the resultant weld properties in high-power laser beam welding (LBW). In this paper, a numerical simulation of the LBW process, considering the 3D transient heat transfer, fluid flow, and keyhole dynamics, is implemented, in which the free surface is tracked by the volume-of-fluid algorithm. The underlying laser-material interactions, i.e., the multiple reflections and Fresnel absorption, are considered by an advanced ray-tracing method based on a localized level-set strategy and a temperature-dependent absorption coefficient. The laser energy absorption is analyzed from a time-averaged point of view for a better statistical representation. It is found for the first time that a significant drop in the time-averaged laser energy absorption occurs at the focus position of the laser beam and that the rest of the keyhole region has relatively homogeneous absorbed energy. This unique absorption pattern may lead to a certain keyhole instability and have a strong correlation with the detrimental bulging and narrowing phenomena in the molten pool. The influence of different focus positions of the laser beam on the keyhole dynamics and molten pool profile is also analyzed. The obtained numerical results are compared with experimental measurements to ensure the validity of the proposed model.
The industrial sintering process used to produce metallic matrix pads has been altered to diminish the amount of copper used. Unfortunately, replacing a large part of the copper with iron seems to have reached a limit. In the high-energy, emergency-type rail braking used in this study, the materials are put to the very limit of their usage capacity, allowing us to observe the evolution of the microstructure and mechanical properties of sintered, metallic matrix pads. After the braking test, their compressive behaviour was assessed using digital image correlation (DIC), and their microstructure with scanning electron microscopy (SEM). The worn material has three flat layers with different microstructures and compressive behaviours. The boom layer seems unmodified. Macroscopic and microscopic cracks run through the intermediate layer (2–15 mm depth). The top layer has stiffened thanks to resolidification of copper. The temperature reaches 1000 °C during the braking test, which also explains the carbon diffusion into iron that result in the weakening of iron–graphite interfaces in the pad. Finally, submicronic particles are detected at many open interfaces of the worn and compressed pad. Associated with the predominant role of graphite particles, this explains the weak compressive behaviour of the pads.
AbstractViscous healing of cracks induced by the Vickers indentation in a soda lime magnesium silicate, a soda borosilicate, and a soda aluminosilicate glass (NAS) was studied by laser scanning microscopy. Plots of the crack length, width, and depth normalized to the initial crack length versus time over viscosity merge into single master curves of each of these quantities for each glass. Despite glass properties do not differ strikingly from each other, however, these master curves strongly differ among the glasses. This finding was attributed to a different interplay of various crack healing phenomena. Lateral cracks were found to be responsible for the bulging of the sample surface around the Vickers imprint, which in turn promotes radial crack widening as the main cause of healing delay. The most rapid healing of lateral cracks was observed in NAS in which bulging and crack widening were least pronounced.
The permeation of hydrogen gas was studied in meta-aluminous (tectosilicate) glass powders of Li2O×Al2O3×SiO2 (LAS), Na2O×Al2O3×SiO2 (NAS) and MgO×Al2O3×SiO2 (MAS) systems by pressure loading and vacuum extraction in the temperatures range 210–310 °C. With this method, both the solubility S and the diffusivity D were determined, while the permeability was given by the product SD. For all glasses, S was found to decrease with temperature, while D increased. Since the activation energy of diffusion of H2 molecules exceeded that of dissolution, permeation increased slightly with temperature. When extrapolated to standard conditions (25 °C), the permeability of tectosilicate glasses was found to be only 10-22–10-24 mol H2 (m s Pa)-1, which is 8–10 magnitudes lower than most polymers. Thin glass liners of these compositions are expected to be the most effective barrier for tanks of pressurised hydrogen.
In this review article, the impact of dissolved water on the viscous properties of soda lime silicate melts is addressed against the background of the upcoming switch from natural gas to hydrogen combustion. This change will lead to an increase in the total water content of the glasses by up to 0.4 mol%. In order to better define possible influences of water speciation, water-rich glasses were synthesised under increasing pressure up to the kbar range. It is shown that a distinction must be made between the influence of dissolved OH-groups and H2Omolecules in order to accurately reflect the dependence of isokom temperatures on water content. In addition, an increase of one order of magnitude in the tolerance to higher deformation rates was observed for the range of expected increased water contents during isothermal deformation processes, which is based on the timetemperature superposition principle, i.e. congruent flow curves were determined under isokomal conditions.
Controlled oriented crystallization of glass surfaces is desired for high precision applications, since the uppermost crystal layer significantly influences the properties of the material. In contrast to previous studies, the data presented here deal with separated crystals growing at defect-free surfaces in four atmospheres with different degrees of humidity (ambient/dry air, argon and vacuum). A glass with the composition 2 BaO–TiO2–2.75 SiO2 was heat-treated at 825 °C until fresnoite (Ba2TiSi2O8) grew to a significant size. The crystal growth rate is found to increase with increasing humidity. The morphology of the crystals changes from highly distorted dendrites in the driest atmosphere (vacuum) to circular/spear-head-shaped crystals in the wettest atmosphere (ambient air), which we attribute to a decrease in viscosity of the glass surface due to water uptake. The least distorted crystals appear in the form of depressions of up to 6 µm. This has an influence on the observed crystal orientation, as measured by electron backscatter diffraction (EBSD). The pulled-in crystals change the orientation during growth relative to the flat glass surface due to an enrichment in SiO2 at the crystal fronts. This confirms that the orientation of crystals is not fixed following nucleation.
A round-robin study has been carried out to estimate the impact of the human element in small-angle scattering data analysis. Four corrected datasets were provided to participants ready for analysis. All datasets were measured on samples containing spherical scatterers, with two datasets in dilute dispersions and two from powders. Most of the 46 participants correctly identified the number of populations in the dilute dispersions, with half of the population mean entries within 1.5% and half of the population width entries within 40%. Due to the added complexity of the structure factor, far fewer people submitted answers on the powder datasets. For those that did, half of the entries for the means and widths were within 44 and 86%, respectively. This round-robin experiment highlights several causes for the discrepancies, for which solutions are proposed.
The effect of resting time on the rheological properties of cement suspensions is generally explained by early formed structure and overconsumption of polycarboxylate superplasticizers (PCEs). In this paper, we propose that the influence of resting time on the rheological properties is closely related to size variation of non-absorbed PCE. To identify this, glass bead suspensions were prepared with various amounts of PCE and ionic solution, and their rheological properties were evaluated at various times. We found that the yield stress increases with time at higher PCE concentrations and higher ionic strength solutions. Adsorbed PCE during resting tends to bridge the particles rather than disperse them. In addition, it was found that hydrodynamic radius of PCE increased with resting time, and depletion forces resulting from non-absorbed PCE size changes correlate well with the increased yield stress.
Liquid metal embrittlement (LME) cracking is a phenomenon observed during resistance spot welding (RSW) of zinccoated advanced highstrength steels (AHSS) in automotive manufacturing. In this study, severe cracks are observed at the edge of the sheet under reduced flange widths. These cracks, traversing the AHSS sheet, culminate at the edge with a width of approximately 1.2 mm.
Through combined numerical and experimental investigations, and material testing, these cracks are identified and validated as a new type of LME crack. The mechanism behind this crack formation is attributed to unique geometric conditions that, when compared to center welding, amplify radial material flow by ninefold to 0.87 mm. The resultant tangential tensile stresses approximate 760 MPa, which exceed the yield strength of the examined advanced highstrength steel (AHSS) under heightened temperature conditions, and when combined with liquid zinc, promote the formation of this new type of LME crack.
Simulation-based digital twins have emerged as a powerful tool for evaluating the mechanical response of bridges. As virtual representations of physical systems, digital twins can provide a wealth of information that complements traditional inspection and monitoring data. By incorporating virtual sensors and predictive maintenance strategies, they have the potential to improve our understanding of the behavior and performance of bridges over time. However, as bridges age and undergo regular loading and extreme events, their tructural characteristics change, often differing from the predictions of their initial design. Digital twins must be continuously adapted to reflect these changes. In this article, we present a Bayesian framework for updating simulation-based digital twins in the context of bridges. Our approach integrates information from measurements to account for inaccuracies in the simulation model and quantify uncertainties. Through its implementation and assessment, this work demonstrates the potential for digital twins to provide a reliable and up-to-date representation of bridge behavior, helping to inform decision-making for maintenance and management.
Effect of Tensile Loading and Temperature on the Hydrogen Solubility of Steels at High Gas Pressure
(2023)
The hydrogen solubility in ferritic and martensitic steels is affected by hydrostatic stress, pressure, and temperature. In general, compressive stresses decrease but tensile stresses increase the hydrogen solubility. This important aspect must be considered when qualifying materials for high‐pressure hydrogen applications (e.g., for pipelines or tanks) by using autoclave systems. In this work, a pressure equivalent for compensating the effect of compressive stresses on the hydrogen solubility inside of closed autoclaves is proposed to achieve solubilities that are equivalent to those in pipelines and tanks subjected to tensile stresses. Moreover, it is shown that the temperature effect becomes critical at low temperatures (e.g., under cryogenic conditions for storing liquid hydrogen). Trapping of hydrogen in the microstructure can increase the hydrogen solubility with decreasing temperature, having a solubility minimum at about room temperature. To demonstrate this effect, the generalized law of the hydrogen solubility is parameterized for different steels using measured contents of gaseous hydrogen. The constant parameter sets are verified and critically discussed with respect to the high‐pressure hydrogen experiments.
In this article, a partial selection of experiments on enhancing the impact resistance of structural components with non-metallic, textile-reinforced concrete is discussed. The focus is on the experimental investigations in which the impact resistance of thin, textile-reinforced concrete plates is characterized. The article discusses the materials, fabrics and test setup used. For the experimental work, a drop tower from the Otto Mohr Laboratory, which belongs to the Technische Universtät Dresden, was used. Furthermore, the experimental results are presented and evaluated using different methods. Based on the collected data, a suitable approach to determining the perforation velocity of an impactor through the investigated thin, textile-reinforced concrete plates is shown.
Inputs of plastic impurities into the environment via the application of fertilizers are regulated in Germany and the EU by means of ordinances. Robust and fast analytical methods are the basis of legal regulations. Currently, only macro- and large microplastic contents (>1 mm) are measured. Microplastics (1–1,000 µm), are not yet monitored. Thermal analytical methods are suitable for this purpose, which can determine the mass content and can also be operated fully automatically in routine mode. Thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS) allows the identification of polymers and the determination of mass contents in solid samples from natural environments. In accordance with the German or European Commission (EC) Fertiliser Ordinance, composting plants should be monitored for microplastic particles with this method in the future. In this context a compost plant was sampled. At the end of the rotting process, the compost was sieved and separated in a coarse (>1 mm) and a fine fraction (<1 mm). The fine fraction was processed using density separation comparing NaCl and NaI as possible salt alternative and screened for microplastic masses by TED-GC/MS with additional validation and quality assurance experiments. With TED-GC/MS total microplastics mass contents of 1.1–3.0 μg/mg in finished compost could be detected with polyethylene mainly. What differs much to the total mass of plastics in the coarse fraction with up to 60 μg/mg, which were visually searched, identified via ATR-FTIR and gravimetrically weighted.
The capability to produce complexly and individually shaped metallic parts is one of the main advantages of the laser powder bed fusion (PBF LB/M) process. Development of material and machine specific process parameters is commonly based on results acquired from small cubic test coupons of about 10 mm edge length. Such cubes are usually used to conduct an optimization of process parameters to produce dense material. The parameters are then taken as the basis for the manufacturing of real part geometries. However, complex geometries go along with complex thermal histories during the manufacturing process, which can significantly differ from thermal conditions prevalent during the production of simply shaped test coupons. This may lead to unexpected and unpredicted local inhomogeneities of the microstructure and defect distribution in the final part and it is a root cause of reservations against the use of additive manufacturing for the production of safety relevant parts. In this study, the influence of changing thermal conditions on the resulting melt pool depth of 316L stainless steel specimens is demonstrated. A variation of thermo-graphically measured intrinsic preheating temperatures was triggered by an alteration of inter layer times and a variation of cross section areas of specimens for three distinct sets of process parameters. Correlations between the preheating temperature, the melt pool depth, and occurring defects were analyzed. The limited expressiveness of the results of small density cubes is revealed throughout the systematic investigation. Finally, a clear recommendation to consider thermal conditions in future process parameter optimizations is given.
Covalent organic frameworks (COFs) are a prominent class of organic materials constructed from versatile building blocks via reversible reactions. The quality of imine-linked COFs can be improved by using amine monomers protected with benzophenone forming benzophenone imines. Here, we present a study on substituted benzophenones in COF synthesis via formal transimination. 12 para-substituted N-aryl benzophenone imines, with a range of electron-rich to electron-poor substituents, were prepared and their hydrolysis kinetics were studied spectroscopically. All substituted benzophenone imines can be employed in COF synthesis and lead to COFs with high crystallinity and high porosity. The substituents act innocent to COF formation as the substituted benzophenones are cleaved off. Imines can be tailored to their synthetic demands and utilized in COF formation. This concept can make access to previously unattainable, synthetically complex COF monomers feasible.
This study was carried out to investigate the neutron transmission signal as a function of sample temperature during a welding process. A theoretical description that includes the Debye-Waller factor was used to describe the temperature influence on the neutron crosssections. Neutron imaging using a monochromatic beam helps to observe transmission variations related to the material temperature. In-situ neutron imaging of welding experiments show the distribution of the temperature in bulk steel samples. The performed finite element modelling of expected temperature distributions shows good agreement with the obtained experimental data.
AbstractLaser beam welding has become widely applied in many industrial fields in recent years. Solidification cracks remain one of the most common welding faults that can prevent a safe welded joint. In civil engineering, convolutional neural networks (CNNs) have been successfully used to detect cracks in roads and buildings by analysing images of the constructed objects. These cracks are found in static objects, whereas the generation of a welding crack is a dynamic process. Detecting the formation of cracks as early as possible is greatly important to ensure high welding quality. In this study, two end-to-end models based on long short-term memory and three-dimensional convolutional networks (3D-CNN) are proposed for automatic crack formation detection. To achieve maximum accuracy with minimal computational complexity, we progressively modify the model to find the optimal structure. The controlled tensile weldability test is conducted to generate long videos used for training and testing. The performance of the proposed models is compared with the classical neural network ResNet-18, which has been proven to be a good transfer learning model for crack detection. The results show that our models can detect the start time of crack formation earlier, while ResNet-18 only detects cracks during the propagation stage.
Hybrid laser-arc welding (HLAW) was applied for butt welding of 14.5 mm thick plates of ferritic cryogenic steel X8Ni9 containing 9% Ni, which is used for manufacturing storage and transport facilities of liquefied natural gas (LNG). The weld seam formation and the achievable metallurgical and mechanical properties of the hybrid welds were investigated experimentally for two types of filler wire, an austenitic wire dissimilar to the base metal (BM) and an experimentally produced matching ferritic wire. Safe penetration and uniform distribution of the austenitic filler metal in the narrow hybrid weld could only be achieved in the upper, arcdominated part of the weld. The pronounced heterogeneous distribution of the austenitic filler metal in the middle part and in the root area of the weld could not ensure sufficient notched impact toughness of the weld metal (WM). As a result, a decrease in the impact energy down to 17±3 J was observed, which is below the acceptance level of ≥34 J for cryogenic applications. In contrast, the use of a matching ferritic filler wire resulted in satisfactory impact energy of the hybrid welds of up to 134±52 J at the concerned cryogenic temperature of -196 °C. The obtained results contribute to an important and remarkable conversion in automated manufacturing of LNG facilities. In other words, the results will help to develop a new laser-based welding technology, where both quality and productivity are considered.The efficiency of the developed welding process has been demonstrated by manufacturing a prototype where a segment of the inner wall of large size LNG storage tank was constructed. In this concern, hybrid laser arc welding was conducted in both horizontal (2G) and vertical (3G) positions as a simulation to the actual onsite manufacturing. The prototype was fabricated twice where its quality was confirmed based on non-destructive and destructive examinations.
The structure and composition of ancient gold objects retain information about their long history of manufacture, from the exploitation of the ore to the finishing touches, as well as evidence of their use, deposition, and degradation. By developing an efficient analytical strategy, it is possible to retrieve that information. This chapter sets the necessary foundation 131to explore fully the analytical results presented in the following chapters of this volume. The techniques employed in the analyses of the Egyptian jewellery are described and the analytical parameters provided. For more established techniques, only brief introductions are presented, while more recent developments are presented in greater detail.
Polyamide 4.6 (PA46) is a high-heat-resistant polymer, but it has no dripping resistance under fire. Three commercial grades of PA46 are investigated under UL 94 vertical fire test conditions. Their performances are discussed based on the materials’ structural, thermal, and rheological properties. PA46 presents flaming drops, whereas dripping is prevented in the flame-retarded PA46.
Friction-modified PA46 has increased flaming dripping. Temperature profiles of the specimens under fire and the temperature of the drops are measured by thermocouples. A UL 94 vertical test configuration consisting of two flame applications is designed to assess the quantitative dripping behavior of the set of materials by the particle finite element method (PFEM). Polymer properties (activation energy and Arrhenius coefficient of decomposition, char yield, density, effective heat of combustion, heat of decomposition, specific heat capacity, and thermal conductivity) in addition to rheological responses in high temperatures are estimated and measured as input parameters for the simulations. The dripping behavior obtained by simulated materials corresponds with the experimental results in terms of time and drop size. A consistent picture of the interplay of the different phenomena controlling dripping under fire appears to deliver a better understanding of the role of different materials’ properties
The degradation of a single-site atomically dispersed, model Fe–N–C powder catalyst with high activity is investigated using cryo-Mössbauer spectroscopy. The results indicate a degradation initiated by an Fe2+ to Fe3+ oxidation due to coordination of oxygen to tetrapyrrolic Fe–N4 sites at atmospheric conditions (change between characteristic doublets) before iron(III) oxide is formed (sextet). Thermal reactivation can be used to restore substantial catalytic activity of aged Fe–N–C powders.
Laser melting manufacturing of large elements of lunar regolith simulant for paving on the Moon
(2023)
The next steps for the expansion of the human presence in the solar system will be taken on the Moon. However, due to the low lunar gravity, the suspended dust generated when lunar rovers move across the lunar soil is a significant risk for lunar missions as it can affect the systems of the exploration vehicles. One solution to mitigate this problem is the construction of roads and landing pads on the Moon. In addition, to increase the sustainability of future lunar missions, in-situ resource utilization (ISRU) techniques must be developed. In this paper, the use of concentrated light for paving on the Moon by melting the lunar regolith is investigated. As a substitute of the concentrated sunlight, a high-power CO2 laser is used in the experiments. With this set-up, a maximum laser spot diameter of 100 mm can be achieved, which translates in high thicknesses of the consolidated layers. Furthermore, the lunar regolith simulant EAC-1A is used as a substitute of the actual lunar soil. At the end of the study, large samples (approximately 250 × 250 mm) with interlocking capabilities were fabricated by melting the lunar simulant with the laser directly on the powder bed. Large areas of lunar soil can be covered with these samples and serve as roads and landing pads, decreasing the propagation of lunar dust. These manufactured samples were analysed regarding their ineralogical composition, internal structure and mechanical properties.
Welded joints show large variation of the weld toe geometry along the weld seam, which is one important reason for the comparably large scatter in fatigue life. Therefore, it is crucial to take the local geometry at the weld toe into account, to reduce the conservatism in fatigue assessment of welded joints. This study is based on the IBESS procedure for the calculation of the fatigue strength, whereby the evaluation of local geometrical parameters is carried out by means of 3D surface scans. The approach is validated against 26 fatigue test series. The fatigue life is in general overpredicted, whereas good agreement is achieved for high stress ratio (R = 0.5). A sensitivity analysis conducted with IBESS shows that weld toe radii ρ < 2 mm and flank angle α < 30° have a significant influence on the calculated fatigue strength. In contrast to this, no strong correlation between ρ and the fatigue strength was determined experimentally in this study.
Considering the availability of serological and molecular biological methods, the bioassay has been paled into insignificance, although it is the only experimental method that can be used to demonstrate the infectivity of a virus. We compared goodness-of-fit and predictability power of five models for the quantification of tomato brown rugose fruit virus (ToBRFV) based on local lesion assays: the Kleczkowski model, Furumoto and Mickey models I and II, the Gokhale and Bald model (growth curve model), and the modified Poisson model. For this purpose, mechanical inoculations onto Nicotiana tabacum L. cv. Xanthi nc and N. glutionosa L. with defined virus concentrations were first performed with half-leaf randomization in a Latin square design. Subsequently, models were implemented using Python software and fitted to the number of local lesions. All models could fit to the data for quantifying ToBRFV based on local lesions, among which the modified Poisson model had the best prediction of virus concentration in spike samples based on local lesions, although data of individual indicator plants showed variations. More accurate modeling was obtained from the test plant N. glutinosa than from N. tabacum cv. Xanthi nc. The position of the half-leaves on the test plants had no significant effect on the number of local lesions.
After entry of a quarantine/regulated pathogen, infected plants shall be destroyed, and the cultivated area (e.g., greenhouse) shall be disinfected. Therefore, the selection of an effective disinfectant plays an important role. With the availability of different methods for virus quantification, we investigated the application of quantitative ELISA (qELISA), RT-qPCR (reverse transcription-quantitative polymerase chain reaction), and bioassays for the quantification of disinfectant efficacy. Therefore, we estimated the titer reduction in tomato brown rugose fruit virus (ToBRFV), a regulated pathogen, in plant sap and on germ carriers after treatment with MENNO Florades 4% for 16 h. The virus load before and after the treatment was measured with the mentioned methods. The RT-qPCR and qELISA methods showed very low efficacy in the presence of the disinfectant. Although bioassays are time-consuming, need purified particles for establishing the quantification models, and are less sensitive than RT-qPCR, they were able to quantify the differences in virus titer in the presence/absence of disinfectant. Interestingly, the bioassays reached at least the lower limit sensitivity of a qELISA. By being less sensitive to the presence of the disinfectant, bioassays proved to be the only technique for the determination of the disinfectant efficacy against ToBRFV on different germ carriers as well as on virus-infected plant sap.
Iron aluminides, already reported in the late 19th century, did not cease to attract the interest of scientists and engineers ever since. Besides good oxidation resistance, low density and resource availability, potentials for hightemperature strengths that compete with high-alloy steels were unlocked by low alloy contents. Still, research on alloy design continues, as alloying usually comes at the price of brittleness in low-temperature regimes. A potential candidate is the quinary Fe–Al–Mo–Ti–B system which is strengthened by solid solution and eutectic borides. It was shown to have good strength and outstanding creep resistance under compressive loading up to elevated temperatures. Although the individual effect of alloy additions is well understood in iron aluminides, little is known about the combined effects of alloying concentrations on microstructure, phase stability and mechanical properties. Therefore a systematic study of two Ti-doped near-Fe3Al alloys with varying contents of Mo (2–4 at.%) and B (0.5–1 at.%) was conducted. In total eight different alloys were fabricated by investment casting into ceramic shell molds. Alloys were characterized and compared by grain size, phase transitions, microstructure evolution as well as elemental compositions and volume fractions of phases. For mechanical characterization, macrohardness and microhardness tests as well as tensile tests at ambient and high tempera tures were conducted. Independent of alloy additions, alloys with 24–25 at.% Al exhibit superior proof strength due to a higher matrix hardness. Decreasing B content generally decreases strength by lower secondary phase fractions which contribute via particle hardening. Reducing Mo content decreases both the solute concentration in the matrix and secondary phase fractions. Surprisingly, strength is similar or even superior to alloys with higher Mo content. Strength relations are discussed with a focus on solid-solution hardening theory and other competing strengthening mechanisms.
With the fast development in the field of additive manufacturing, triply periodic minimal surface (TPMS) based porous media have recently found many uses in mechanical property tuning. However, there is still a lack of understanding in their porosity-dependent permeability and electrical as well as thermal conductivity. Here, we perform finite volume simulations on the solid and void domains of the Schoen gyroid (SG), Schwarz primitive (SP) and Schwarz primitive beam (SPB) TPMS with porosities between 63% and 88% in Ansys Fluent. A simple cubic lattice (CL) of equivalent porosity served as reference. The SPB and CL showed up to one order of magnitude higher permeabilities than the SG and SP. However, SG and SP have about 1.3 and 2.6 times the electrical and thermal conductivity of SPB and CL, respectively. Furthermore, the properties of SPB and CL are largely affected by the surface area density, whereas tortuosity variation does not impact permeability and conductivity to a major extent. Finally, empirical relations are adapted to describe the presented data and thus, they may enable future designers of TPMS based porous structures to fine-tune the geometries according to the requirements on permeability and electrical as well as thermal conductivity.