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Paper des Monats
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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.
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.
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.
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.
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 obvious benefits derived from the increasing use of engineered nano-, new, and advanced materials and associated products have to be weighed out by a governance process against their possible risks. Differences in risk perception (beliefs about potential harm) among stakeholders, in particular nonscientists, and low transparency of the underlying decision processes can lead to a lack of support and acceptance of nano-, new, and other advanced material enabled products. To integrate scientific outcomes with stakeholders needs, this work develops a new approach comprising a nine-level, stepwise categorization and guidance system entitled “Knowledge, Information, and Data Readiness Levels” (KaRLs), analogous to the NASA Technology Readiness Levels. The KaRL system assesses the type, extent, and usability of the available data, information, and knowledge and integrates the participation of relevant and interested stakeholders in a cocreation/codesign process to improve current risk assessment, communication, and governance. The novelty of the new system is to communicate and share all available and relevant elements on material related risks in a user/stakeholder-friendly, transparent, flexible, and holistic way and so stimulate reflection, awareness, communication, and a deeper understanding that ultimately enables the discursive process that is needed for the sustainable risk governance of new materials.
This paper reports a systematic study into the effect of nitrogen on iron-catalyzed graphitization of biomass. Chitin, chitosan, N-acetylglucosamine, gelatin and glycine were selected to represent nitrogen-rich saccharides and amino-acid/polypeptide biomass precursors. The materials were pyrolyzed with an iron catalyst to produce carbons with a wide range of chemical and structural features such as mesoporosity and nitrogen-doping. Many authors have reported the synthesis of nitrogen-doped carbons by pyrolysis and these have diverse applications. However, this is the first systematic study of how nitrogen affects pyrolysis of biomass and importantly the catalytic graphitization step. Our data demonstrates that nitrogen inhibits graphitization but that some nitrogen survives the catalytic graphitization process to become incorporated into various chemical environments in the carbon product.
Regardless of the experimental care practiced in acquiring X-ray computed tomography (XCT) data, artifacts might still exist, such as noise and blur. This is typical for fast XCT data acquisitions (e.g., in-situ investigations), or low-dose XCT. Such artifacts can complicate subsequent analysis of the data. Digital filters can moderately cure extensive artifacts. The selection of filter type, intensity, and order of application is not always straight forward. To tackle these problems, a complete sequential multilevel, multi-scale framework: BAM SynthCOND, employing newly designed deep convolutional neural networks (DCNNs), was formulated. Although data conditioning with neural networks is not uncommon, the main complication is that completely artifact-free XCT data for training do not exist. Thus, training data were acquired from an in-house developed library (BAM SynthMAT) capable of generating synthetic XCT material microstructures. Some novel DCNN architectures were introduced (2D/3D ACEnet_Denoise, 2D/3D ACEnet_Deblur) along with the concept of Assertive Contrast Enhancement (ACE) training, which boosts the performance of neural networks trained with continuous loss functions. The proposed methodology accomplished very good generalization from low resemblance synthetic training data. Indeed, denoising, sharpening (deblurring), and even ring artifact removal performance were achieved on experimental post-CT scans of challenging multiphase Al-Si Metal Matrix Composite (MMC) microstructures. The conditioning efficiencies were: 92% for combined denoising/sharpening, 99% for standalone denoising, and 95% for standalone sharpening. The results proved to be independent of the artifact intensity. We believe that the novel concepts and methodology developed in this work can be directly applied on the CT projections prior to reconstruction, or easily be extended to other imaging techniques such as: Microscopy, Neutron Tomography, Ultrasonics, etc.
Adipokinetic hormone (AKH) is a neuropeptide produced in the insect corpora cardiaca that plays an essential role in mobilising carbohydrates and lipids from the fat body to the haemolymph. AKH acts by binding to a rhodopsin-like G protein-coupled receptor (GPCR), the adipokinetic hormone receptor (AKHR). In this study, we tackle AKH ligand and receptor gene evolution as well as the evolutionary origins of AKH gene paralogues from the order Blattodea (termites and cockroaches). Phylogenetic analyses of AKH precursor sequences point to an ancient AKH gene duplication event in the common ancestor of Blaberoidea, yielding a new group of putative decapeptides. In total, 16 different AKH peptides from 90 species were obtained. Two octapeptides and seven putatively novel decapeptides are predicted for the first time. AKH receptor sequences from 18 species, spanning solitary cockroaches and subsocial wood roaches as well as lower and higher termites, were subsequently acquired using classical molecular methods and in silico approaches employing transcriptomic data. Aligned AKHR open reading frames revealed 7 highly conserved transmembrane regions, a typical arrangement for GPCRs.
Phylogenetic analyses based on AKHR sequences support accepted relationships among termite, subsocial (Cryptocercus spp.) and solitary cockroach lineages to a large extent, while putative post-translational modification sites do not greatly differ between solitary and subsocial roaches and social termites. Our study provides important information not only for AKH and AKHR functional research but also for further analyses interested in their development as potential candidates for biorational pest control agents against invasive termites and cockroaches.
Transition metal phosphates (TMPs) have attracted interest as materials for (electro-) catalysis, and electrochemistry due to their low-cost, stability, and tunability. In this work, an automated synthesis platform was used for the preparation of transition metal phosphate crystals to efficiently explore the multidimensional parameter space, determining the phase selection, crystal sizes, shapes. By using X-ray diffraction and spectroscopy-based methods and electron microscopy imaging, a complete characterization of the phase stability fields, phase transitions, and crystal morphology/sizes was achieved. In an automated three-reactant synthesis, the individual effect of each reactant species NH4+, M2+, and PO43- on the formation of transition metal phosphate phases: M-struvite NH4MPO4·6H2O, M-phosphate octahydrate M3(PO4)2·8H2O with M = Ni, Co and an amorphous phase, was investigated. The NH4+ concentration dictates the phase composition, morphology, and particle size in the Ni-system (crystalline Ni-struvite versus amorphous Ni-PO4 phase), whereas in the Co-system all reactant species - NH4+, Co2+, and PO43- - influence the reaction outcome equivalently (Co-struvite vs. Co-phosphate octahydrate). The coordination environment for all crystalline compounds and of the amorphous Ni-PO4 phase was resolved by X-ray absorption spectroscopy, revealing matching characteristics to its crystalline analogue, Ni3(PO4)2·8H2O. The automated synthesis turned out to be significantly advantageous for the exploration of phase diagrams due to its simple modularity, facile traceability, and enhanced reproducibility compared to a typical manual synthesis.
Safety characteristics are used to keep processes, including flammable gases, vapors, and combustible dusts, safe. In the standards for the determination of safety characteristics of gases and vapors, the induction spark is commonly used. However, classic transformers are hard to obtain, and replacement with new electronic transformers is not explicitly allowed in the standards. This article presents the investigation of five gases that are normally used to calibrate devices for the determination of safety characteristics, the maximum experimental safe gap (MESG), with an electronic transformer, and the values are compared to the ones that are obtained with the standard transformer. Additionally, calorimetric measurements on the net energy of both ignition sources were performed as well as open-circuit voltage measurements. It is concluded that the classic type of transformer can be replaced by the new type obtaining the same results for the MESG and introducing the same amount of energy into the system.
Excessive discharge of quaternary ammoniumdisinfectants such as benzalkonium chloride (BAC) into aquatic systems can trigger several physiological responses in environmental microorganisms. In this study, we isolated a less-susceptible strain of Aeromonas hydrophila to BAC, designated as INISA09, froma wastewater treatment plant in Costa Rica. We characterized its phenotypic response upon exposure to three dierent concentrations of BAC and characterizedmechanisms related to its resistance using genomic and proteomic approaches. The genome of the strain, mapped against 52 dierent sequenced A. hydrophila strains, consists of approximately 4.6Mb with 4,273 genes. We found a massive genome rearrangement and thousands of missense mutations compared to the reference strain A. hydrophila ATCC 7966.
We identified 15,762 missense mutations mainly associated with transport, antimicrobial resistance, and outer membrane proteins.
In addition, a quantitative proteomic analysis revealed a significant upregulation of several efflux pumps and the downregulation of porins when the strain was exposed to three BAC concentrations.Other genes related tomembrane fatty acid metabolism and redox metabolic reactions also showed an altered expression.
Our findings indicate that the response of A. hydrophila INISA09 to BAC primarily occurs at the envelop level, which is the primary target of BAC. Our study elucidates the mechanisms of antimicrobial susceptibility in aquatic environments against a widely used disinfectant and will help better understand howbacteria can adapt to biocide pollution. To our knowledge, this is the first study addressing the resistance to BAC in an environmental A. hydrophila isolate. We propose that this bacterial species could also serve as a new model to study antimicrobial pollution in aquatic environments.
Advanced experimental and numerical approaches are being developed to
capture the localization of plasticity at the nanometer scale as a function of the multiscale and heterogeneous microstructure present in metallic materials.
These innovative approaches promise new avenues to understand microstructural effects on mechanical properties, accelerate alloy design, and enable more accurate mechanical property prediction. This article provides an overview of emerging approaches with a focus on the localization of plasticity by crystallographic slip. New insights into the mechanisms and mechanics of strain localization are addressed. The consequences of the localization of plasticity by deformation slip for mechanical properties of metallic materials are also detailed.
Mistle: bringing spectral library predictions to metaproteomics with an efficient search index
(2023)
Motivation: Deep learning has moved to the forefront of tandem mass spectrometry-driven proteomics and authentic prediction for peptide fragmentation is more feasible than ever. Still, at this point spectral prediction is mainly used to validate database search results or for confined search spaces. Fully predicted spectral libraries have not yet been efficiently adapted to large search space problems that often occur in metaproteomics or proteogenomics.
Results: In this study, we showcase a workflow that uses Prosit for spectral library predictions on two common metaproteomes and implement an indexing and search algorithm, Mistle, to efficiently identify experimental mass spectra within the library. Hence, the workflow emulates a classic protein sequence database search with protein digestion but builds a searchable index from spectral predictions as an in-between step.
We compare Mistle to popular search engines, both on a spectral and database search level, and provide evidence that this approach is more accurate than a database search using MSFragger. Mistle outperforms other spectral library search engines in terms of run time and proves to be extremely memory efficient with a 4- to 22-fold decrease in RAM usage. This makes Mistle universally applicable to large search spaces, e.g. covering comprehensive sequence databases of diverse microbiomes.
Availability and implementation: Mistle is freely available on GitHub at https://github.com/BAMeScience/Mistle.
Climate change is becoming one of the greatest challenges facing our society, particularly due to the continued use of fossil fuels. The steadily increasing demand for energy and the continuously growing world population will further intensify these challenges. The development of renewable energies is therefore of central importance. The 2020 EU Energy Roadmap aims to increase the share of renewable energies (gross energy consumption) to 55% by 2050.
Hydrogen (H2) has the highest potential to become the primary renewable energy source. It is envisioned that by 2050 up to 24% of the total energy demand of Europe is to be ensured by H2. However, a decisive disadvantage of the climate friendly alternatives is the massive containment demand, which needs to be highly secure, cost efficient and easily extractable.
Underground geological formations (UGF) represent a seemingly optimal alternative to meet the rapidly increasing storage demand. In this context, many studies are currently underway to determine the feasibility and risks of UGF. However, little or no consideration is being given to microbiology. Therefore, in this Research Topic we will focus on achieving a greater understanding of the impact microorganisms exert on UGF, with a particular emphasis on interdisciplinary studies.
As many subsurface microbial communities can use H2 as an electron donor, production of seemingly undesirable metabolic byproducts, such as hydrogen sulfide, methane, and acids, are also to be expected. However, the rate of the H2 conversion by the microorganisms, how their metabolic activities impact the UGF on a short-term and long-term scale, the extent of damages microorganisms exert on the infrastructure, or potential use of microorganisms to enhance UGF are just a few questions that require urgent research to assess the role of microorganisms in this new anthropogenic use of the subsurface environment. These and many questions can be addressed in this article collection. In particular, understanding microbial community changes and activity rates will help assess operational and environmental risks, develop mitigation strategies and provide new insights on life under extreme conditions (i.e., pressure, salinity).
In this Research Topic, the editorial team particularly welcomes Original Research, Hypothesis and Theory, Method, and Review manuscripts that deal with the latest advances in microbiology in formations that are planned or currently prepared for hydrogen storage, from both fundamental and practical points of view. The ultimate objective is to promote a deeper understanding into the sustainability of UGF and generate interdisciplinary research involving microbiologists, reservoir engineers, geologists, chemists, physicists.
The topics of interest include, but are not limited to:
• Microbial diversity in different underground hydrogen storage sites or formations currently being considered for hydrogen storage
• Mechanism and impact of microbial growth under high H2 pressure
• Potential role of microorganisms in the short-term and long-term storage of hydrogen
• Potential influences of microorganisms on the hydrogen storage infrastructure systems, e.g., microbiologically influenced corrosion, biofilm growth
• Hydrogen-solid-microorganism interactions, including the influence of microbial growth on UGF geological parameters
• Mechanism and modelling of microbial impact on hydrogen storage
UGF relevant for this Research Topic include porous media, salt caverns, deep aquifers, hard rock caverns and depleted oil/gas reservoirs.
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.
Quenching and partitioning (Q&P) steels are characterized by an excellent combination of strength and ductility, opening up great potentials for advanced lightweight components. The Q&P treatment results in microstructures with a martensitic matrix being responsible for increased strength whereas interstitially enriched metastable retained austenite (RA) contributes to excellent ductility. Herein, a comprehensive experimental characterization of microstructure evolution and austenite stability is carried out on a 42CrSi steel being subjected to different Q&P treatments. The microstructure of both conditions is characterized by scanning electron microscopy as well as X‐ray diffraction (XRD) phase analysis. Besides macroscopic standard tensile tests, RA evolution under tensile loading is investigated by in situ XRD using synchrotron and laboratory methods. As a result of different quenching temperatures, the two conditions considered are characterized by different RA contents and morphologies, resulting in different strain hardening behaviors as well as strength and ductility values under tensile loading. In situ synchrotron measurements show differences in the transformation kinetics being rationalized by the different morphologies of the RA. Eventually, the evolution of the phase specific stresses can be explained by the well‐known Masing model.
An automated and straightforward detection and data treatment strategy for the determination of the protein relative concentration in individual human cells by single cell–inductively coupled plasma–time-of-flight mass spectrometry (sc-ICP-ToF-MS) is proposed. Metal nanocluster (NC)-labeled specific antibodies for the target proteins were employed, and ruthenium red (RR) staining, which binds to the cells surface, was used to determine the number of cell events as well as to evaluate the relative volume of the cells. As a proof of concept, the expression of hepcidin, metallothionein-2, and ferroportin employing specific antibodies labeled with IrNCs, PtNCs, and AuNCs, respectively, was investigated by sc-ICP-ToF-MS in human ARPE-19 cells. Taking into account that ARPE-19 cells are spherical in suspension and RR binds to the surface of the cells, the Ru intensity was related to the cell volume (i.e., the cell volume is directly proportional to (Ru intensity)3/2), making it possible to determine not only the mass of the target proteins in each individual cell but also the relative concentration. The proposed approach is of particular interest in comparing cell cultures subjected to different supplementations. ARPE-19 cell cultures under two stress conditions were compared: a hyperglycemic model and an oxidative stress model. The comparison of the control with treated cells shows not only the mass of analyzed species but also the relative changes in the cell volume and concentration of target proteins, clearly allowing the identification of subpopulations under the respective treatment.
The crystallization proceeds by the advance of the crystal faces into the disordered phase at the expense of the material excess, the supersaturation. Using a conservation constraint for the transformation ratio α∈[0,1] as complementing the rescaled supersaturation to 1 and a kinetic law for the normal growth velocity as function of the supersaturation raised to power g, the growth order, we derive an equation for the rate of transformation dα/dt. We integrate it for the six combinations of the three spatial dimensions D = 1, 2, 3 and the two canonical values of g = 1, 2 towards obtaining expressions for αDg. The same equation, with g = 1 and D = n (n is the so called Avrami exponent) is obtained when taking only the linear in α term from the Taylor’s expansion around α = 0 of the model equation of Johnson-Mehl-Avrami-Kolmogorov (JMAK). We verify our model by fitting datasets of α21 and α31 (from α = 0 to αupper = 0.999) with JMAK to obtain from the fit n = 1.725, 2.43, resp. We show
further how the values of n depend on the value of αupper to which the fit is performed starting always from 0. Towards building a validation protocol, we start with validating α21 with published results.
The impact of high additions of vegetable oil (12 vol%) on the mechanical and microstructural properties of metakaolin-slag-based alkali-activated materials (AAMs) was studied. The addition of oil resulted in a slight decrease in initial polymerization kinetics but did not affect the final degree of reaction. AAM-oil-composite-mortars exhibited approximately ∼30% lower compressive strength primarily due to the entrainment of air voids. Newly formed soap phases significantly reduced the volume of small capillary and gel pores (pore radii <15 nm), leading to a decrease in specific inner surface area by a factor of up to 15. The porosity modification induced by the oil addition greatly enhanced the resistance of AAMs against sulfuric acid attack, shifting the dominant processes from diffusion and cracks to framework-dissolution controlled by the inherent phase stabilities. Following the immersion in sulfuric acid (pHstat = 2) for 8 weeks, the depth of corroded layer decreased by 70% and no cracks due to expansive phases were observed. These promising findings suggest that the incorporation of vegetable oil in AAMs has the potential to address durability concerns associated with diffusion-based corrosion processes, thereby expanding the range of future applications.
AISI 2205 duplex stainless steel is used in a variety of industries, including the chemical and petrochemical industries. This is due to its high tensile strength combined with good ductility and corrosion resistance. However, in laser beam welding, these properties are negatively afected by the high cooling rates typical of the welding process. The resulting higher ferrrite content in the weld metal than in the base material leads to a reduction in the ductility and corrosion resistance of the welded joint. To overcome this problem, in this study, thick plates were coated by direct energy deposition (DED) prior to laser beam welding, whereas a duplex powder mixture containing a higher nickel concentration was used as a coating material. To improve the weld quality for the proposed two-step process, a method of additional material deposition instead of conventional tack weld was investigated. The resulting welded joints showed a well-balanced austenite to ferrite ratio and their properties and microstructure were verifed by metallographic analysis, electron backscatter difraction and Charpy impact testing. Using the standard ASTM G48 test method, it was found that the corrosion resistance of the welds was improved by a factor of four in average compared to the conventionally welded joints. The resulting properties, such as good ductility and corrosion resistance, of the welds with pre-coated edges showed good agreement with those of the base metal and confrmed the proposed two-step process as a promising alternative to the conventional approaches for welding thick duplex stainless steel plates.
The fundamental processes of nucleation and crystallization are widely observed in systems relevant to material synthesis and biomineralization; yet most often, their mechanism remains unclear. In this study, we unravel the discrete stages of nucleation and crystallization of Fe3(PO4)2·8H2O (vivianite). We experimentally monitored the formation and transformation from ions to solid products by employing correlated, time-resolved in situ and ex situ approaches. We show that vivianite crystallization occurs in distinct stages via a transient amorphous precursor phase. The metastable amorphous ferrous phosphate (AFEP) intermediate could be isolated and stabilized. We resolved the differences in bonding environments, structure, and symmetric changes of the Fe site during the transformation of AFEP to crystalline vivianite through synchrotron X-ray absorption spectroscopy at the Fe K-edge. This intermediate AFEP phase has a lower water content and less distorted local symmetry, compared to the crystalline end product vivianite. Our combined results indicate that a nonclassical, hydration-induced nucleation and transformation driven by the incorporation and rearrangement of water molecules and ions (Fe2+ and PO4 3−) within the AFEP is the dominating mechanism of vivianite formation at moderately high to low vivianite supersaturations (saturation index ≤ 10.19). We offer fundamental insights into the aqueous, amorphous-to-crystalline transformations in the Fe2+−PO4 system and highlight the different attributes of the AFEP, compared to its crystalline counterpart.
In this study, the wavefield radiated from a building to its surroundings is identified and extracted from M4.6 earthquake recordings collected by sensors installed in a building and on the nearby athletic field in Matera (Italy) using a new approach for soil-structure interaction assessment. The proposed approach for earthquake data analysis combines in an innovative way two methods already used in seismology and engineering seismology: deconvolution and polarization analysis. The approach enables the identification, reconstruction, and characterization of the wavefield radiated from a vibrating building into its surroundings, and the estimation of the amount of energy associated with it. The approach consists of four steps: estimation of the resonant frequencies of the building, deconvolution of the earthquake recordings from a building and its surroundings, identification of the seismic phases, reconstruction of the signal transmitted from the building to its surroundings, and estimation of its energy, and polarization analysis. Analysis of recordings of the M4.6 event highlighted that the motion related to the wavefield radiated from the building to the ground was mostly linearly polarized in the radial and transverse planes, while a clear ellipticity was observed only in the horizontal plane. The wavefield radiated from the building might be dominated by unconventionally polarized surface waves, i.e., quasi-Rayleigh waves or a combination of quasi-Rayleigh and quasi-Love waves. The results indicated that the energy transmitted from the analyzed vibrating building to its surroundings was significant and decreased the ground motion shaking due to the out-of-phase motion.
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.
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.
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.
The interest in using computer simulations of dimensional x-ray computed tomography (dXCT) for various metrological purposes—such as measurement planning, performance prediction, performance optimisation and, finally, measurement uncertainty estimation—is increasing along with the ever-growing demand for more reliable measurements with dXCT. However, before a piece of simulation software can be used for tasks related to coordinate metrology, it has to be ensured that it is able to simulate physical laws, characteristic effects and basic CT system functionalities correctly and with sufficient accuracy. In short, the software must be qualified for dimensional metrology tasks. As one part of such a qualification process, a method is presented here for determining conformity intervals of 2D tests (projection-based tests) based on 3D tests (testing based on dimensional evaluations in a reconstructed volume) for the assessment of dXCT simulation software. The method consists of varying relevant parameter values in order to verify their influence on 3D measurement results. The results of the 3D tests with varied parameter values are then transferred to the quantities tested in the 2D tests and used as the basis for determining conformity intervals. Two approaches are applied for determining whether or not a variation of a parameter value is significant: (a) statistical and (b) heuristic. Two examples are presented, each based on simulated images, which show the application of the two different approaches for determining conformity intervals for the results of the 2D tests.
We examine the performance of a number of single-atom M−N/C electrocatalysts with a common structure in order to deconvolute the activity of the framework N/C support from the metal M−N4 sites in M−N/Cs. The formation of the N/C framework with oordinating nitrogen sites is performed using zinc as a templating agent. After the formation of the electrically conducting carbon−nitrogen metal-coordinating network, we (trans)metalate with different metals producing a range of different catalysts (Fe−N/C, Co−N/C, Ni−N/C, Sn−N/C, Sb−N/C, and Bi−N/C) without the formation of any metal particles. In these materials, the structure of the carbon/nitrogen framework remains unchanged-only the coordinated metal is substituted. We assess the performance of the subsequent catalysts in acid, near-neutral, and alkaline environments toward the oxygen reduction reaction (ORR) and ascribe and quantify the performance to a combination of metal site activity and activity of the carbon/nitrogen framework. The ORR activity of the carbon/nitrogen framework is about 1000-fold higher in alkaline than it is in acid, suggesting a change in mechanism. At 0.80 VRHE, only Fe and Co contribute ORR activity significantly beyond that provided by the carbon/nitrogen framework at all pH values studied. In acid and near-neutral pH values (pH 0.3 and 5.2, respectively), Fe shows a 30-fold improvement and Co shows a 5-fold improvement, whereas in alkaline pH (pH 13), both Fe and Co show a 7-fold improvement beyond the baseline framework activity. The site density of the single metal atom sites is estimated using the nitrite adsorption and stripping method. This method allows us to deconvolute the framework sites and metal-based active sites. The framework site density of catalysts is estimated as 7.8 × 1018 sites g−1. The metal M−N4 site densities in Fe−N/C and Co−N/C are 9.4 × 1018 sites−1 and 4.8 × 1018 sites g−1, respectively.
This work investigates the microstructure formed in friction stir welds of FCC alloys, focused on two multiprincipal alloys: a CoCrFeMnNi high-entropy alloy (HEA) and a CoCrNi medium-entropy alloy (MEA). A commercial stainless steel AISI 304 is used for comparison. The largest nugget was formed in the MEA, while the smallest was formed in the HEA. Grain refinement occurs in the stirred zone in all welds. Discontinuous dynamic recrystallisation is the predominant restoration mechanism during friction stir welding of the three investigated alloys. A sharp decrement in the Σ3 boundary fraction occurs in the stirred zone of the AISI 304 and HEA welds, while comparable values with the base metal are found for the MEA weld. The peak in the maximum index of crystallographic texture is observed on the advancing side of the stirred zone of the AISI 304 weld. A strong <001> θ-fibre texture is formed in the advancing side of the nugget in the AISI 304 from a well-established {123} <634> S-type texture in the base metal. Multiple crystallographic texture components without specific fibres are identified in most regions of the welds, indicating the complex shear path history during friction stir welding.
Multi-Principal-Element or High-Entropy Alloys (MPEAs/HEAs) have gained increasing interest in the past two decades largely due to their outstanding properties such as superior mechanical strength and corrosion resistance. However, research studies on their processability are still scarce. This work assesses the effect of different machining conditions on the machinability of these novel alloys, with the objective of advancing the introduction of MPEA systems into industrial applications. The present study focuses on the experimental analysis of finish-milling conditions and their effects on the milling process and resulting surface finish of CoCrFeNi, Al0.3CoCrFeNi and Al0.3CoCrFeNiMo0.2 alloys fabricated via Spark Plasma Sintering. Ball-nose-end milling experiments have been carried out various milling parameters such as cutting speed, feed per cutting edge, and ultrasonic assistance. In situ measurements of cutting forces and temperature on the tool edge were performed during the experiments, and surface finish and tool wear were analyzed afterwards. The results exhibited decreasing cutting forces by means of low feed per cutting edge and reduced process temperatures at low cutting speed, with the use of ultrasonic-assisted milling. It was shown that the machinability of these modern alloys through conventional, as well as modern machining methods such as ultrasonic-assisted milling, is viable, and common theories in machining can be transferred to these novel MPEAs.
Ring-expansion polymerizations (REPs) catalyzed by two cyclic tin catalysts (2-stanna-1.3-dioxa-4,5,6,7-dibenzazepine [SnBiph] and
2,2-dibutyl-2-stanna-1,3-dithiolane [DSTL]) are performed at 140 °C in bulk.
Small amounts (4 vol%) of chlorobenzene or other solvents are added to
facilitate transesterification reactions (ring–ring equilibration) in the solid poly(l-lactide)s. In the mass range up to m/z 13 000 crystalline PLAs displaying a so-called saw-tooth pattern in the MALDI-TOF mass spectra are obtained indicating the formation of extended-ring crystals. The characteristics of extended-ring crystallites and folded-ring crystallites are discussed. Furthermore, extremely high melting temperatures (Tm’s up to 201.2 °C) and melting enthalpies (𝚫Hm’s up to 106 J g−1)) are found confirming that 𝚫Hm max, the 𝚫Hm of a perfect crystal, is around or above 115 J g−1 in contrast to literature data.
We present how mesoporosity can be engineered in transition metal phosphate (TMPs) materials in a template-free manner. The method involves the transformation of a precursor metal phosphate phase, called M-struvite (NH4MPO4·6H2O, M = Mg2+, Ni2+, Co2+, NixCo1−x2+). It relies on the thermal decomposition of crystalline M-struvite precursors to an amorphous and simultaneously mesoporous phase, which forms during degassing of NH3 and H2O. The temporal evolution of mesoporous frameworks and the response of the metal coordination environment were followed by in situ and ex situ scattering and diffraction, as well as X-ray spectroscopy. Despite sharing the same precursor struvite structure, different amorphous and mesoporous structures were obtained depending on the involved transition metal. We highlight the systematic differences in absolute surface area, pore shape, pore size, and phase transitions depending on the metal cation present in the analogous M-struvites. The amorphous structures of thermally decomposed Mg-, Ni- and NixCo1−x-struvites exhibit high surface areas and pore volumes (240 m2 g−1 and 0.32 cm−3 g−1 for Mg and 90 m2 g−1 and 0.13 cm−3 g−1 for Ni). We propose that the low-cost, environmentally friendly M-struvites could be obtained as recycling products from industrial and agricultural wastewaters. These waste products could be then upcycled into mesoporous TMPs through a simple thermal treatment for further application, for instance in (electro)catalysis.
The complex nature of liquid water saturation of polymer electrolyte fuel cell (PEFC) catalyst layers (CLs) greatly affects the device performance. To investigate this problem, we present a method to quantify the presence of liquid water in a PEFC CL using small-angle X-ray scattering (SAXS). This method leverages the differences in electron densities between the solid catalyst matrix and the liquid water filled pores of the CL under both dry and wet conditions. This approach is validated using ex situ wetting experiments, which aid the study of the transient saturation of a CL in a flow cell configuration in situ. The azimuthally integrated scattering data are fitted using 3D morphology models of the CL under dry conditions. Different wetting scenarios are realized in silico, and the corresponding SAXS data are numerically simulated by a direct 3D Fourier transformation. The simulated SAXS profiles of the different wetting scenarios are used to interpret the measured SAXS data which allows the derivation of the most probable wetting mechanism within a flow cell electrode.
Die Brechung von Röntgenstrahlen (Röntgenrefraktion) an Grenzflächen zwischen Materialien unterschiedlicher Dichte ist analog zur Ablenk-ung von sichtbarem Licht an z.B. Glasoberflächen. Es gibt jedoch zwei wesentliche Unterschiede:
a) konvexe Grenzflächen verursachen Divergenz (d.h. der Brechungsindex n ist kleiner als 1), und
b) die Ablenkungswinkel sind sehr klein, und reichen von einigen Bogensekunden bis zu einigen Bogenminuten (d.h. n ist nahe bei 1);
Wie auch bei sichtbarem Licht ist die Ablenkungsrichtung der Röntgenstrahlen abhängig von der Orientierung der durchstrahlten Grenzfläche. Aufgrund dieser Eigenschaften eignen sich Röntgenrefraktionsmethoden hervorragend für:
a) die Erkennung und Quantifizierung von Defekten wie Poren und Mikrorissen und
b) die Bewertung von Porosität und Partikeleigenschaften wie Orientierung, Größe und räumliche Verteilung.
Wir zeigen die Anwendung der Röntgenrefraktionsradiographie (2,5D Technik) und der -tomographie (3D Technik) für die Untersuchung verschiedener Probleme in der Werkstoffwissenschaft und -technologie:
a) Sintern von SiC-Grünkörpern
b) Porositätsanalyse in Dieselpartikelfiltersilikaten
c) Faser-Matrix-Haftung in Metall- und Polymermatrixverbundwerkstoffen
d) Mikrorissbildung in Glaskeramik.
Wir zeigen, dass der Einsatz von Röntgenrefraktionsmethoden quantitative Ergebnisse liefert, die direkt als Parameter in Werkstoffmodellen verwendet werden können.
The application and benefits of Semantic Web Technologies (SWT) for managing, sharing, and (re-)using of research data are demonstrated in implementations in the field of Materials Science and Engineering (MSE). However, a compilation and classification are needed to fully recognize the scattered published works with its unique added values. Here, the primary use of SWT at the interface with MSE is identified using specifically created categories. This overview highlights promising opportunities for the application of SWT to MSE, such as enhancing the quality of experimental processes, enriching data with contextual information in knowledge graphs, or using ontologies to perform specific queries on semantically structured data. While interdisciplinary work between the two fields is still in its early stages, a great need is identified to facilitate access for nonexperts and develop and provide user-friendly tools and workflows. The full potential of SWT can best be achieved in the long term by the broad acceptance and active participation of the MSE community. In perspective, these technological solutions will advance the field of MSE by making data FAIR. Data-driven approaches will benefit from these data structures and their connections to catalyze knowledge generation in MSE.
The peak broadening in neutron diffraction experiments on tensile specimens of pure Al (99.8%) and an Al-Mg alloy pre-deformed at different creep strains is analysed. These results are combined with the kernel angular misorientation of electron backscatter diffraction data from the creep-deformed microstructures. It is found that differently oriented grains possess different microstrains. These microstrains vary with creep strain in pure Al, but not in the Al-Mg alloy. It is proposed that this behaviour can explain the power-law breakdown in pure Al and the large creep strain observed in Al-Mg. The present findings further corroborate a description of the creep-induced dislocation structure as a fractal, predicated on previous work.
Phased-Array-Prüfköpfe für luftgekoppelte Ultraschallprüfung auf Basis von zellulären Kunststoffen
(2023)
Luftgekoppelte Ultraschallprüfung setzt sich immer häufiger gegen die konventionelle Ultraschallprüfung von Leichtbaukomponenten durch, und zwar in vielen Industriezweigen von der Holzindustrie bis zur Luftfahrt. Während die Phased-Array-Technik mittlerweile zu dem industriellen Standard im Bereich der Prüfung mit Ankopplung gehört, wird luftgekoppelte Ultraschallprüfung meist mit zwei Wandlern in Durchschallung durchgeführt. Deswegen werden Vorteile der Phased-Array-Technik wie beispielsweise elektronische Fokussierung oder Schwenkung des Einschallwinkels für luftgekoppelte Prüfung selten genutzt.
In diesem Beitrag werden die laufenden Arbeiten an der Entwicklung eines neuen Phased-Array-Geräts vorgestellt, mit dem Schwerpunkt an der Charakterisierung der Prüfköpfe und ihrer Schallfelder. Das Gerät besteht aus einem linearen Phased-Array-Prüfkopf, einer Sende- und einer Empfangseinheit. Die Hauptinnovation unserer Arbeit ist die Anwendung von zellulären Kunststoffen für den Bau eines Arrays, wobei der Sender mit Hochspannung von ca. 1500 V angeregt wird. Geladene zelluläre Polymere werden auch Ferroelektrete oder Piezoelektrete genannt. Sie weisen ein sehr niedriges Elastizitätsmodul und dadurch eine niedrige akustische Impedanz auf, so dass auf den Einbau von Anpassschichten verzichtet werden kann.
Eine sehr niedrige mechanische Kreuzkopplung bei Ferroelektreten ermöglicht eine unabhängige Anregung einzelner Elemente, was bei Piezokompositen deutlich schwieriger wäre. Die Entwicklung der Array-Prüfköpfe wurde durch Berechnungen des Schallfeldes unterstützt, die auf Punktquellensynthese basieren. Die beabsichtigte Anwendung von Phased-Array-Prüfköpfen und des Prüfsystems sind die Durchschallung mit Fokussierung, elektronischer Scan und die Schwenkung des Einschallwinkels zur Anregung von geführten Wellen, angewandt an carbonfaserverstärkten Kunststoffen und ähnlichen Materialien. Die Anwendung von geführten Wellen bietet die Perspektive, Bauteile mit einseitiger Zugänglichkeit zu prüfen.
Bei der Prüfung von Werkstücken mit empfindlichen Oberflächen oder auch hydrophilen Werkstoffen sind traditionelle ultraschallbasierte zerstörungsfreie Prüfmethoden wie die Kontakttechnik oder die Tauchtechnik in vielen Anwendungsfällen aufgrund der Flüssigkeitsankopplung nicht anwendbar.
Die luft-gekoppelte Ultraschallprüfung umgeht diese Problematik und eröffnet neue Prüfszenarien. Derzeit werden zwei Varianten der Schallerzeugung als vielversprechend angesehen: ferroelektrische Folien und thermoakustische Dünnschichtwandler. Thermoakustische Wandler ermöglichen die resonanzfreie Erzeugung von Ultraschall und somit kurze zeitliche Impulse sowie eine sehr breitbandige Anregung. Durch die Verwendung von gekrümmten Substraten ist sowohl eine Herstellung von planaren als auch fokussierten Wandlern möglich.
Dieser Beitrag präsentiert die letzten Forschungsergebnisse im Bezug auf thermoakustischen Wandlern, welche derzeit in einen thermoakustischen Gruppenstrahler münden. Gruppenstrahler erlauben die simultane Änderung des Einschallwinkels, sowie die Verschiebung des Fokuspunktes während der Verwendung.
Durch die Verbindung beider Schlüsseltechnologien, der thermoakustischen Anregung und des Gruppenstrahlerprinzips, wird das Spektrum der klassischen ZfP-Anwendungen, sowie moderner Ansätze wie der Anregung von geführten Wellen oder der Strukturüberwachung erheblich erweitert und bereichert.
Dabei soll innerhalb dieses Beitrages auf die Modellierung des Schallfeldes, die elementweise Charakterisierung und verschiedene Anwendungsszenarien eingegangen werden.
Nickel alloys are cost intensive materials and generally classified as difficult-to-cut material. However, machining of these materials is needed especially in case of alloy 36 (1.3912), which is commonly used in mould construction for the production of fibre-reinforced composites. With regard to repair, modification and manufacturing of such components, additive manufacturing offers significant economic advantages. Nevertheless, subsequent machining steps are needed to achieve the final component contour and defined surface conditions. Dependent on the material and machining process conditions, detrimental tensile residual stresses may be the result on the machined surface, having negative impact on the component performance and safety. In this investigation, machining experiments were carried out on wire arc additive manufactured components made of alloy 36, varying the cutting speed and the feed rate. In addition, the conventional milling process (CM) was compared with a modern, hybrid machining process, the ultrasonic-assisted milling (US). The cutting forces and the surface-near residual stresses were analysed using X-ray diffraction. A significant improvement of the machinability as well as the surface integrity by using the ultrasonic assistance was observed, especially at low cutting speeds. The CM induced mainly tensile residual stresses, the US mainly compressive residual stresses.
A new simplified and effective method has been formalised to estimate the Constant Amplitude Fatigue Limit (CAFL) of stress-relieved steel welded joints subjected to uniaxial push–pull loading and failing from the weld toe. Starting from the sharp V-notch assumption of the NSIF approach and the cyclic R-curve of the material in the heat affected zone, the proposed method identifies the CAFL as threshold level of the local stress field at the V-notched weld toe in the uncracked configuration. Such threshold stress field assures the crack arrest at the V-notched weld toe, according to the cyclic R-curve analysis. The method has been validated against experimental results and proved effective for a straightforward assessment of the CAFL of welded joints, as the stable crack propagation analysis of classical fracture mechanics approaches can be avoided.
The expansive production of data in materials science, their widespread sharing and repurposing requires educated support and stewardship. In order to ensure that this need helps rather than hinders scientific work, the implementation of the FAIR-data principles (Findable, Accessible, Interoperable, and Reusable) must not be too narrow. Besides, the wider materials-science community ought to agree on the strategies to tackle the challenges that are specific to its data, both from computations and experiments. In this paper, we present the result of the discussions held at the workshop on “Shared Metadata and Data Formats for Big-Data Driven Materials Science”. We start from an operative definition of metadata, and the features that a FAIR-compliant metadata schema should have. We will mainly focus on computational materials-science data and propose a constructive approach for the FAIRification of the (meta)data related to ground-state and excited-states calculations, potential-energy sampling, and generalized workflows. Finally, challenges with the FAIRification of experimental (meta)data and materials-science ontologies are presented together with an outlook of how to meet them.
Through experimental observation and auxiliary numerical simulation, this investigation studies the different types of grain refinement of 5754 aluminum alloy laser beam welding by applying a transverse oscillating magnetic field. Scanning electron microscope results have proved that the application of a magnetic field can reduce the average crystal branch width and increase its number. The interaction between the induced eddy current generated by the Seebeck effect and the applied external magnetic field produces a Lorentz force, which is important for the increase in the number of crystal branches. Based on the theory of dendrite fragmentation and the magnetic field-induced branches increment, the grain size reduction caused by the magnetic field is studied. Furthermore, the effects of the magnetic field are analyzed by combining a phase field method model and simulations of nucleation and grain growth. The grain distribution and average grain
size after welding verify the reliability of the model. In addition, the introduction of a magnetic field can increase the number of periodic three-dimensional solidification patterns. In the intersection of two periods of solidification patterns, the metal can be re-melted and then re-solidified, which prevents the grains, that have been solidified and formed previously, from further growth and generates some small cellular grains in the new fusion line. The magnetic field increases the building frequency of these solidification structures and thus promotes this kind of grain refinement.
The amount of absorbed energy in the keyhole as well as its spatial and temporal distribution is essential to model the laser beam welding process. The recoil pressure, which develops because of the evaporation process induced by the absorbed laser energy at the keyhole wall, is a key determining factor for the macroscopic flow of the molten metal in the weld pool during high-power laser beam welding. Consequently, a realistic implementation of the effect of laser radiation on the weld metal is crucial to obtain reliable and accurate simulation results. In this paper, we discuss manyfold different improvements on the laser-material interaction, namely, the ray tracing method, in the numerical simulation of the laser beam welding process. The first improvement relates to locating the exact reflection points in the ray tracing method using a so-called cosine condition in the determination algorithm for the intersection of reflected rays and the keyhole surface. A second correction refers to the numerical treatment of the Gaussian distribution of the laser beam, whose beam width is defined by a decay of the laser intensity by a factor of 1/e2, thus ignoring around 14% of the total laser beam energy. In the third step, the changes in the laser radiation distribution in the vertical direction were adapted by using different approximations for the converging and the diverging regions of the laser beam, thus mimicking the beam caustic. Finally, a virtual mesh refinement was adopted in the ray tracing routine. The obtained numerical results were validated with experimental measurements.
The precipitation of struvite, a magnesium ammonium phosphate hexahydrate (MgNH₄PO₄ · 6H₂O) mineral, from wastewater is a promising method for recovering phosphorous. While this process is commonly used in engineered environments, our understanding of the underlying mechanisms responsible for the formation of struvite crystals remains limited. Specifically, indirect evidence suggests the involvement of an amorphous precursor and the occurrence of multi-step processes in struvite formation, which would indicate non-classical paths of nucleation and crystallization. In this study, we use synchrotron-based in situ x-ray scattering complemented by cryogenic transmission electron microscopy to obtain new insights from the earliest stages of struvite formation. The holistic scattering data captured the structure of an entire assembly in a time-resolved manner. The structural features comprise the aqueous medium, the growing struvite crystals, and any potential heterogeneities or complex entities. By analysing the scattering data, we found that the onset of crystallization causes a perturbation in the structure of the surrounding aqueous medium. This perturbation is characterized by the occurrence and evolution of Ornstein-Zernike fluctuations on a scale of about 1 nm, suggesting a non-classical nature of the system. We interpret this phenomenon as a liquid-liquid phase separation, which gives rise to the formation of the amorphous precursor phase preceding actual crystal growth of struvite. Our microscopy results confirm that the formation of Mg-struvite includes a short-lived amorphous phase, lasting >10 s.
The vehicle–track interaction generates forces and consequently vibrations in the environment. The interaction has been analysed by the simultaneous measurements of vehicle, track and ground vibrations during test runs with varied train speeds. The special effects of the passage over a bridge and through a tunnel are studied and compared with the measurements on a conventional ballasted surface line. The maximum amplitudes, narrow band and one-third octave band spectra are presented for the axle-box accelerations and for the track, bridge and ground vibrations. The different frequencies and frequency bands are related to wheel out-of-roundness, track alignment errors, the sleeper passage and the wheelset–track resonance. An axle impulse component has been observed at the track, at the near-field soil and as a scattered version in the far field. Specific results can be found for the bridge track, where clearly speed-dependent bridge resonances occur due to the axle sequence of the train, and for the tunnel track where soft rail pads are responsible for a strong amplification around the wheelset–track resonance. On the other hand, the axle impulses are strongly reduced by the tunnel track, and the scattered axle impulse component is not as relevant as for the surface track. As a consequence, a strong mid-frequency amplitude reduction of the tunnel compared to the surface line has been measured for low and high train speeds by the Federal Institute of Material Research and Testing (BAM) and by other institutes.
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.
Stereolithography processes such as lithography-based ceramic manufacturing (LCM) are technologies that can produce centimeter-sized structures in a reasonable time frame. However, for some parts specifications, they lack resolution. Two-photon-polymerization (2PP) ensures the highest geometric accuracy in additive manufacturing so far. Nevertheless, building up parts in sizes as large as a few millimeters or even centimeters is a time-consuming process, which makes the production of 2PP printed parts very costly. Regarding feedstock specification, the requirements for 2PP are different to those for LCM, and generally, feedstocks are designed to meet requirements for only one of these manufacturing technologies. In an attempt to fabricate highly precise ceramic components of a rather large size, it is necessary to develop a feedstock that suits both light-based technologies, taking advantage of LCM’s higher productivity and 2PP’s accuracy. Hybridization should bring the desired precision to the region of interest on reasonably large parts without escalating printing time and costs. In this study, specimens gained from a transparent feedstock with yttria stabilized zirconia (YSZ) particles of 5 nm at 70 wt% were presented. The resin was originally designed to suit 2PP, while being also printable with LCM. This work demonstrates how hybrid parts can be sintered into full YSZ ceramics.
Recently, efforts towards the development of patient-specific 3D printed scaffolds for bone tissue engineering from bioactive ceramics have continuously intensified. For reconstruction of segmental defects after subtotal mandibulectomy a suitable tissue engineered bioceramic bone graft needs to be endowed with homogenously distributed osteoblasts in order to mimic the advantageous features of vascularized autologous fibula grafts, which represent the standard of care, contain osteogenic cells and are transplanted with the respective blood vessel. Consequently, inducing vascularization early on is pivotal for bone tissue engineering. The current study explored an advanced bone tissue engineering approach combining an advanced 3D printing technique for bioactive resorbable ceramic scaffolds with a perfusion cell culture technique for pre-colonization with mesenchymal stem cells, and with an intrinsic angiogenesis technique for regenerating critical size, segmental discontinuity defects in vivo applying a rat model. To this end, the effect of differing Si-CAOP (silica containing calcium alkali orthophosphate) scaffold microarchitecture arising from 3D powder bed printing (RP) or the Schwarzwalder Somers (SSM) replica fabrication technique on vascularization and bone regeneration was analyzed in vivo. In 80 rats 6-mm segmental discontinuity defects were created in the left femur.
This paper presents a novel approach for developing sustainable building materials through Sequential Learning. Data sets with a total of 1367 formulations of different types of alkali-activated building materials, including fly ash and blast furnace slag-based concrete and their respective compressive strength and CO2-footprint, were compiled from the literature to develop and evaluate this approach. Utilizing this data, a comprehensive computational study was undertaken to evaluate the efficacy of the proposed material design methodologies, simulating laboratory conditions reflective of real-world scenarios. The results indicate a significant reduction in development time and lower research costs enabled through predictions with machine learning. This work challenges common practices in data-driven materials development for building materials. Our results show, training data required for data-driven design may be much less than commonly suggested. Further, it is more important to establish a practical design framework than to choose more accurate models. This approach can be immediately implemented into practical applications and can be translated into significant advances in sustainable building materials development.
The propagation of ground vibrations is theoretically analysed with frequency-wavenumber and simplified methods. Experimental methods are presented which can characterise the site-specific ground vibrations by wave velocities, stiffness and damping. Measurements with hammer and train excitation have been performed at several sites. The one-third octave spectra show the stiffness-dependent amplitudes and the low- and high-frequency filter effects due to the layering and the damping of the soil. Specific train effects, an additional high-frequency filter, the sleeper passage frequency, and an amplified mid-frequency component can be clearly found. The attenuation with distance is analysed in detail where the theoretical exponential and the empirical frequency-dependent power law are considered. Hammer and train excitation show the same site-specific effects which are mainly due to the stronger or weaker damping of the soil. The train attenuation is generally weaker than the hammer attenuation. The attenuation exponent of the power law, which is strongly dependent on the site and the frequency, is reduced for the train vibration by 0.3 to 0.5 in agreement with the theory. Reasons are discussed for the overall power law and for the dominating mid-frequency component.
Surface-functionalized polymer beads encoded with molecular luminophores and nanocrystalline emitters such as semiconductor nanocrystals, often referred to as quantum dots (QDs), or magnetic nanoparticles are broadly used in the life sciences as reporters and carrier beads. Many of these applications require a profound knowledge of the chemical nature and total number of their surface functional groups (FGs), that control bead charge, colloidal stability, hydrophobicity, and the interaction with the environment and biological systems. For bioanalytical applications, also the
number of groups accessible for the subsequent functionalization with, e.g., biomolecules or targeting ligands is relevant. In this study, we explore the influence of QD encoding on the amount of carboxylic acid (COOH) surface FGs of 2 μm polystyrene microparticles (PSMPs). This is done for frequently employed oleic acid and oleylamine stabilized, luminescent core/shell CdSe QDs and two commonly used encoding procedures. This included QD addition during bead formation by a thermally induced polymerization reaction and a post synthetic swelling procedure. The accessible number of COOH groups on the surface of QD-encoded and pristine beads was quantified by two colorimetric assays, utilizing differently sized reporters and electrostatic and covalent interactions. The results were compared to the total number of FGs obtained by a conductometric titration and Fourier transform infrared spectroscopy (FTIR). In addition, a comparison of the impact of QD and dye encoding on the bead surface chemistry was performed. Our results demonstrate the influence of QD encoding and the QD-encoding strategy on the number of surface FG that is ascribed to an interaction of the QDs with the carboxylic acid groups on the bead surface. These findings are of considerable relevance for applications of nanoparticle-encoded beads and safe-by-design concepts for nanomaterials.
Epoxy R-Glass Fiber-Reinforced Polymer (GFRP) composite plates were hydrothermally aged at 60 ◦C for 23, 75, and 133 days. The water content reached 0.97 wt%, 1.45 wt% and 1.63 wt%, respectively. The studied GFRP matrix was inert to hydrolysis or chain scission, allowing for investigation of irreversible changes in the fiber-matrix interphase due to hydrothermal aging upon re-drying. During each period, a subset of the specimens was removed from the water bath and dried in a chamber. The weight loss upon drying was explained with epoxy leaching (impurities), sizing-rich interphase hydrolysis, glass fiber surface hydrolysis, accumulated degradation products escaping, and water changing state from bound to free. The influence of hydrothermal aging on the fiber-matrix interfacial properties was investigated. Lower interfacial strength of hydrothermally aged (wet)
samples was attributed to plasticization of the epoxy, plasticization and degradation of the sizing-rich interphase (including formation of hydrolytic flaws), and hydrolytic degradation of the glass fiber surface. The kinetics of epoxy-compatible epoxysilane W2020 sizing-rich interphase hydrolysis provided an estimate of ca. 1.49%, 4.80%, and 8.49% of the total composite interphase degraded after 23, 75, and 133 days, respectively. At these conditions, the interface lost 39%, 48%, and 51% of its strength. Upon re-drying the specimens, a significant part of the interfacial strength was regained. Furthermore, an upward trend was observed, being 13%, 10% and 3% strength, respectively; thus, indicating a possibility of partial recovery of properties.
Laser-induced breakdown spectroscopy (LIBS) is becoming a more mature technology every year with new variants such as laser ablation molecular isotopic spectrometry, reheating by various discharge techniques, and multiple pulse excitation schemes, in which sometimes lasers of different pulse lengths are used. However, lasers with inherent parameters like pulse length and repetition rate are still almost exclusively employed. Recent years have witnessed the advent of novel high-repetition-rate laser concepts for machining processes, like welding, milling, and engraving. Here, a comprehensive study of single-pulse LIBS spectra of a single aluminum target is presented to showcase the applicability of flexible high duty-cycle master oscillator power amplifier (MOPA) lasers. Although traditional flashlamp-pumped Fabry–Pérot lasers only permit a variation in the pulse energy and are operated at very low duty-cycles, MOPA lasers add repetition rate and pulse length as variable parameters. A thorough analysis of the temporal plasma behavior revealed the emission dynamic to closely match the excitation laser pulse pattern. An aluminum sample’s spectral response was shown to be significantly impacted by variations in both rate and length. Although the spectral emission strength of the elemental lines of Al, Sr, and Ca all peaked at slightly different parameter settings, the strongest impact was found on the relative abundance of molecular AlO bands. Unlike in previous laser ablation molecular isotopic spectrometry (LAMIS) publications, the latter could be readily detected with a good intensity and well-resolved spectral features without any temporal gating of the detector. This finding, together with the fact that MOPA lasers are both inexpensive and dependable, makes for a promising combination for future studies including the detection of diatomic band structures.
Monopiles are currently the predominant foundation type for offshore wind turbines in Europe. Due to the increasing dimensions of the turbines, pile diameters beyond 10m become necessary. A design-relevant failure mode of monopiles is the local buckling of the pile wall in the embedded sections. Relevant buckling guidelines do not consider the soil-structure interaction specifically, although the embedment may allow for a reduction of wall thickness. However, Eurocode-based design concepts require a validation with comparative buckling cases for validation, either in terms of buckling curve parameters for both the algebraic stress-based and semi-numerical LBA/MNA design concept or as a calibration factor kGMNIA for fully numerical GMNIA calculations. These parameters are not yet available for embedded shells. To close this gap, we have conducted experiments on piles embedded in sand to investigate local buckling under soil-structure-interaction. The results will be used to calibrate numerical models. This research was carried out as part of the VERBATIM research project, funded by PTJ/BMWK and supported by the Carbon Trust's Offshore Wind Accelerator consortium.
Mobile proximal gamma-ray spectrometry (GS) is an emerging approach to estimate soil texture directly in the field. It relies on gamma radiation emitted during the natural decay of potassium-40 (K-40) and other isotopes. The K-40 counts are correlated with total K content, mineralogical soil composition and therefore with soil texture. Yet, it is not clear if K fertilisation impacts the ratio of K-40 to total K which would necessitate to take the fertilisation history into account for soil sensing applications. To elucidate this question, a well-documented long-term experiment was selected. The soils of the Rengen grassland experiment (55 plots) were investigated for total K (XRF-K) and for K-40 via mobile proximal GS. No significant differences in XRF-K and K-40 were found between the treatments with and without K fertilisation, although formely published results point to negative and positive K balances, respectively. Fertiliser analysis revealed a ratio of K-40 to total K that was almost identical to the natural abundance of 0.0117%. It was concluded that it is not necessary to take K fertilisation history into account when predicting soil texture from mobile proximal GS on agricultural land for, e.g., precision farming purposes.
Cyclic and linear poly(L-lactide)s by ring-expansion polymerization with Bu2SnO, Oct2SnO, and Bu2SnS
(2023)
To elucidate the usefulness of commercial Bu2SnO as catalyst for syntheses of linear and/or cyclic polylactides L-Lactide was polymerized in bulk with variation of the LA/Cat ratio, temperature and time. Based on a ring-expansion polymerization (REP) mechanism cyclic polylactides (PLAs) with weight average molecular weights in the range of 200,000–300,000 are obtained at the highest temperature (180 °C). Polymerizations at 150 °C yielded crystalline, mainly cyclic polylactides which, after annealing, showed high melting temperatures (up to 197.5 °C) and high crystallinities (>80%). Polymerization at 120 °C confirmed the trend towards more linear chains with lower temperatures but yielded extended-ring crystals showing a “saw-tooth pattern” in the mass spectra. Oct2SnO gave similar results as Bu2SnO. Bu2SnS proved a sluggish polymerization catalyst, but a good transesterification catalyst in solid PLA.
An analytical expression for the frequency response function of a coupled pedestrian-bridge system is presented and evaluated using an experimental measurement campaign performed on the Folke Bernadotte Bridge in Stockholm, Sweden. A finite element model and the modal models that consider the human–structure interaction effect are calibrated with respect to the measurements. The properties of the spring–mass–damper model representing the pedestrians were identified, considering the different structural modes of the system. Good agreement was obtained between the experimental and theoretical frequency response functions. A sensitivity analysis of the obtained solution was performed, validating the determined analytical expression for the frequency response function of the coupled pedestrian-bridge system that takes into account the human–structure interaction effect.
Almost all building materials in civil engineering have an open porosity and interact with or are affected by the environmental conditions. Structures might suffer from effects such as moisture adsorption, carbonation, corrosion, penetration of salt ions and chemical substances, etc. In the hygroscopic range, these processes are mostly driven by diffusion. Due to the confinement of small pores (less than1 µm), the Knudsen effect reduces the molecular diffusion. This reduction can become more significant in case of temporal changing pore systems because of physisorption of water vapor, carbonation, or chemisorption.
In this study, unstabilised earth blocks and earth masonry are investigated. In a first step, the pore size distribution of the blocks is measured and sorption isotherms are recorded in experiments. Besides the ordinary physisorption, the involved clay minerals undergo swelling or shrinking due to chemisorption. The following two effects must be considered: first, the reduction of the available pore space by the adsorbed water layer. For this, the Hillerborg sorption theory is used, which is a combination of the well-known Brunauer-Emmett-Teller sorption theory and the Kelvin equation. This allows the computation of adsorbed water layers even in curved pore geometries. Second, the variation of the initial pore size distribution due to chemisorption needs to be modelled. Based on these two models, the effective diffusion coefficient can be predicted. For validation, arrays of relative humidity sensors were embedded into a free-standing earth masonry wall. This monitoring was carried out over more than a year to have a broad variety of environmental conditions and was located in Berlin, Germany.
The prediction of the effective diffusion coefficient can also be transferred to other processes and allows the investigation of materials having temporarily changing pore systems. Examples are the carbonation of cementitious materials, alkali silica reaction, calcium leaching of long-lasting structures, etc. These effects are prominent in the meso-pore range and might significantly alter the effective diffusion coefficient.
Hierarchically porous, high‐surface‐area silica materials are excellent candidates for multiple applications like catalysis and environmental remediation. Shaping these materials with additive manufacturing (AM) techniques, like robocasting, could enable their use with the benefit of on‐demand, customized shaping and maximizing performance. Herein, ordered mesoporous silica COK‐12 slurries were robocasted into monoliths, containing different ratios of uncalcined COK‐12 and sodium bentonite (0–25 wt.%). The rheology of the mixed slurries is characterized by lower flow indexes (0.69 vs. 0.32) and higher yield stresses (96 vs. 259 Pa) compared to pure COK‐12 ones. Monoliths were printed in woodpile structures and calcined at 600°C. Micro‐CT measurements showed a linear shrinkage of 25% after calcination. Mechanical characterization showed increased uniaxial strength (0.20 ± 0.07 to 1.0 ± 0.3 MPa) with increasing binder/solids ratio from 13 to 25%. The amorphous, mesoporous structure of COK‐12 was retained. The structures exhibited open porosities of 52 ± 4% and showed higher specific mesopore volumes, and increased average mesopore size (6 vs. 8 nm) compared to COK‐12. Small‐angle x‐ray scattering analysis revealed an increased lattice parameter (10.3 vs. 11.0 nm) and reduced wall thickness (3.1 nm vs. 4.1 nm) of the COK‐12 in the monoliths. These properties indicate suitability for their application as porous supports and adsorbents.
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 frequency-domain (FD) method provides an alternative to the commonly used time-domain (TD) approach in characterizing the luminescence kinetics of luminophores, with its own strengths, e.g., the capability to decouple multiple lifetime components with higher reliability and accuracy. While extensively explored for characterizing luminophores with down-shifted emission, this method has not been investigated for studying nonlinear luminescent materials such as lanthanide-doped upconversion nanoparticles (UCNPs), featuring more complicated kinetics. In this work, employing a simplified rate-equation model representing a standard two-photon energy-transfer upconversion process, we thoroughly analyzed the response of the luminescence of UCNPs in the FD method. We found that the FD method can potentially obtain from a single experiment the effective decay rates of three critical energy states of the sensitizer/activator ions involved in the upconversion process. The validity of the FD method is demonstrated by experimental data, agreeing reasonably well with the results obtained by TD methods.
The flow properties of powdery or granular filling substances for dangerous goods packagings are safety-relevant parameters. To specify the flow behavior, the angle of repose is measured in the recognized test centers for dangerous goods packagings in Germany. Previous investigations performed on non-hazardous substances revealed that some of the methods currently used have disadvantages in application. Additionally, for occupational health and safety reasons, it was generally viewed critically to carry out measurements of the angle of repose for dangerous goods at all. Instead, the dimensionless Hausner ratio to describe the flow behavior was proposed.
In this work, the investigations were extended to real hazardous substances to concretize the assessment. Five exemplary hazardous substances were tested for their angle of repose using the methods commonly applied in the test centers. The Hausner ratio was also determined. In addition, the influence of a different climatic preconditioning on the angle of repose measurement was examined using three selected non-hazardous bulk materials.
The results show that the measurement of the angle of repose is not fundamentally excluded for dangerous goods. However, for reasons of applicability, repeatability and occupational health and safety, only the ISO method can be applied for dangerous filling substances. This method provides conservative results regarding a safety-related evaluation of flow properties for the transport of dangerous goods.
In principle, both the ISO method and the determination of the Hausner ratio can be used for dangerous goods. It is also essential especially with finely powdered filling goods, to carry out controlled preconditioning.
Gasquellenlokalisierungen (Gas Source Localization, GSL) tragen dazu bei, die Folgen von Industrieunfällen und Naturkatastrophen zu mildern. Während die GSL, wenn von Menschen durchgeführt, gefährlich und zeitaufwändig ist, können Schwärme von wendigen und kostengünstigen Nanodrohnen die Effizienz und Sicherheit der Suche erhöhen. Da die geringe Nutzlast von Nanodrohnen die Sensor- und Rechenressourcen einschränkt, werden Strategien zur Koordination des Roboterschwarms verwendet, die von biologischen Schwärmen, wie Kolonien sozialer Insekten, inspiriert sind. Die meisten Schwarm-GSL-Strategien verwenden das Maximum der Gaskonzentrationsverteilung zur Schätzung der Gasquellenposition. Experimente legen jedoch nahe, dass die Intermittenz der Gasverteilung vielversprechender ist. In diesem Beitrag wird eine neuartige GSL-Strategie für Schwärme vorgestellt, die auf Pheromonkommunikation und Intermittenz der Gasverteilung basiert. Die Agenten, d.h. die Nanodrohnen, emittieren Pheromonmarker in einer virtuellen Umgebung, wenn sie eine neue Gaswolke feststellen. Die Agenten werden durch virtuelle Kräfte gesteuert und nutzen abwechselnd das Wissen des Schwarms, indem sie dem Pheromongradienten folgen, oder erkunden den Suchraum, indem sie einen Zufallspunkt ansteuern. Zur Kollisionsvermeidung werden die Agenten durchgehend von anderen Agenten und Wänden abgestoßen. Die Strategie wurde auf drei Nanodrohnen implementiert und durch ein Experiment in einem Innenraum mit einer statischen Gasquelle validiert. Die Ergebnisse zeigen eine Verbesserung gegenüber maximabasierten Verfahren und geringe Lokalisierungsfehler in Windrichtung.
The development of hydrogen technologies entails high safety requirements in distribution and dispensing infrastructure. Therefore, it is necessary to pursue research on material compatibility in hydrogen, especially for critical parts with tribological issues.
The focus of this study is to evaluate the influence of hydrogen on a wider range of commercially available polymer materials. Thereby, the friction and wear behavior of different grades of TPE, POM, PA66, PA12, PPA, PEEK, PPS, PTFE, PAI, PI and PBI were investigated against a rotating steel disk (AISI 304). Filled and unfilled polymers from different suppliers were evaluated at room temperature in air, vacuum and hydrogen gas (H2) as well as in liquid hydrogen at - 253°C (LH2).
The sliding behavior of the polymer materials is discussed by means of surface analyses, whereby special attention is paid to the formation of a transfer film.
According to the results at ambient temperature, the effect of hydrogen environment on the tribological behavior of neat polymers may be related to lack of moisture, but also to saturated hydrocarbons in gaseous hydrogen. In liquid hydrogen, the best tribological performances were achieved with neat PA polymers as well as PPS and PI composites.
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 main objective was to assess homogeneity of two bimodal gold materials, namely nPsize1 and nPSize2, containing approximately 1:1 and 10:1 particle number-based ratio of ~30nm and ~60nm particles. Particle number-based concentration within the two size fractions was determined with spICP-MS using the particle frequency method of calibration.
Abstract
In the post-processing of large maritime components, a considerable amount of waste in the form of milling and grinding chips is produced. At the same time, additive manufacturing technologies have shown great potential in producing high-volume parts for maritime applications, allowing novel design approaches and short lead times. In this context, this study presents a sustainable approach to recycle and use aluminium bronze waste material, generated during post-processing of large cast ship propellers, as feedstock for laser-powder directed energy deposition. The recycling technology used to produce powder batches is inductive re-melting in combination with ultrasonic atomization. The derived metal powders are characterized using digital image analysis, powder flowability tests, scanning electron microscopy as well as energy dispersive X-ray spectroscopy. Compared to conventional metal powders produced by gas atomization, the recycled material shows excellent sphericity and a powder size distribution with a higher content of finer and coarser particles. Metallographic sections of deposited additively produced specimens show an increased hardness and reduced ductility, but also competitive densities and higher yield and ultimate tensile strength compared to cast material. The process chain shows high potential for the maritime sector to enable circular and sustainable manufacturing.
Defensive behavior is linked to altered surface chemistry following infection in a termite society
(2023)
The care-kill response determines whether a sick individual will be treated or eliminated from an insect society, but little is known about the physiological underpinnings of this process. We exploited the stepwise infection dynamics of an entomopathogenic fungus in a termite to explore how care-kill transitions occur, and identify the chemical cues behind these shifts. We found collective responses towards pathogen-injected individuals to vary according to severity and timing of pathogen challenge, with elimination, via cannibalism, occurring sooner in response to a severe active infection. However, injection with inactivated fungal blastospores also resulted in increased albeit delayed cannibalism, even though it did not universally cause host death. This indicates that the decision to eliminate an individual is triggered before pathogen viability or terminal disease status has been established. We then compared the surface chemistry of differently challenged individuals, finding increased amounts of long-chained methyl-branched alkanes with similar branching patterns in individuals injected with both dead and viable fungal blastospores, with the latter showing the largest increase. This coincided with the highest amounts of observed cannibalism as well as signs of severe moribundity. Our study provides new mechanistic insight into the emergent collective behaviors involved in the disease defense of a termite society.
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.
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.
Im Rahmen des BMBF-geförderten Forschungsprojekts ReMin – REALight werden in einem Projektteam aus Industriepartnern und Forschungseinrichtungen unter Koordination der Bauhaus-Universität Weimar leichte Gesteinskörnungen aus Bau- und Abbruchabfällen und industriellen Nebenprodukten auf thermischem Weg hergestellt. Die Aufgabe der Bundesanstalt für Materialforschung und -prüfung (BAM) ist es, diese im Drehrohrofen erzeugten Blähgranulate für gebundene Anwendungen in Beton und Mörtel umfassend zu charakterisieren. Gemeinsam mit der Opus Denkmalpflege GmbH wird die Applikation feiner, gebrochener Blähgranulate in leichten Steinergänzungsmörteln für die Restaurierung von Sandsteinobjekten untersucht. Hierzu wird ein zweischichtiges Mörtelsystem bestehend aus einem Füll- und einem Deckmörtel entwickelt. Erste Ergebnisse der Rezepturentwicklung verschiedener kalkhaltiger Leichtmörtel mit gebrochenen Blähgranulaten werden vorgestellt. Die neuen Leichtmörtel sind hinsichtlich der entwickelten Druckfestigkeit gleichwertig gegenüber herkömmlichen Restauriermörteln.
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.
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.
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
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.
The 2-methoxyphenol units (G-units) in lignin are modified by demethylation and oxidation to provide the activated lignin as one part of an advanced biobased two-component (2K) adhesive system, which exhibits promising shear strengths in dry and underwater applications. The activation of lignin is straightforward and generates quinones via demethylation and periodate oxidation. These act as Michael acceptors and react smoothly with multi-thiol-star polymers to yield thiol-catechol connectivities (TCCs). The mussel-inspired material platform acts as a very robust and versatile adhesive, combining low-cost and readily available lignin with multi-thiols to achieve outstanding adhesion strengths of up to 15 MPa in dry application. In particular, the 2K system is compatible with the marine biological environment and shows no acute toxicity to sensitive organisms such as fish eggs. Thus, one possible application of this material could be an adhesive for setting temperature-resistant corals in damaged reefs.
Against the backdrop of numerous security breaches and cyber-attacks, organizations need to take measures to secure their data and information. However, the well-known management system standard ISO/IEC 27001 for information security has shown a lower adoption rate – in terms of annual ISO survey data – than was previously expected by scholars and practitioners. Through the lens of Rogers' diffusion of innovation theory, we consider the adoption of ISO/IEC 27001 as a 'preventive innovation' and aim to identify factors that help gain a better understanding of its adoption. Therefore, we conducted a survey among German organizations on the use and impact of management system standards, explicitly distinguishing between organizations that implement ISO/IEC 27001 and those that are additionally certified against this standard. This study provides insights and contributes to an advanced understanding of motives, impacts, barriers, and useful measures to increase adoption of ISO/IEC 27001. Our findings may be useful to organizations considering the adoption of this management system standard, to certification bodies providing certification services, and to policymakers seeking means to improve information security in organizations.
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.
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.
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.
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.
Die neue Generation von bainitischen Schmiedestählen bietet auf der einen Seite ein erhebliches Festigkeitspotenzial, das es im Sinne des Leichtbaus auch für zyklisch belastete Sicherheitsbauteile zu heben gilt. Auf der anderen Seite geht mit dieser Festigkeitssteigerung im Vergleich zu Vergütungsstählen ein Verlust an Duktilität und Zähigkeit einher. Am Beispiel des Demonstratorbauteils Achsschenkel ging das Forschungsvorhaben der Frage nach, wie ein Freigabeprozess zu gestalten ist, damit das Festigkeitspotenzial der neuen Stähle zuverlässig ausgenutzt werden kann. Als Ergebnis wird eine Vorgehensweise dargestellt, die den Eigenschaften der neuen Generation von Schmiedestählen Rechnung trägt, um den sicheren Betrieb der Komponenten zu gewährleisten.
An observation of the fracture process in front of the crack tip inside a dentin sample by means of ex-situ X-ray computed tomography after uniaxial compression at different deformation values was carried out in this work. This ex-situ approach allowed the microstructure and fracturing process of human dentin to be observed during loading. No cracks are observed up to the middle part of the irreversible deformation in the samples at least visible at 0.4μm resolution. First cracks appeared before the mechanical stress reached the compression strength. The growth of the cracks is realized by connecting the main cracks with satellite cracks that lie ahead of the main crack tip and parallel its trajectory. When under the stress load the deformation in the sample exceeds the deformation at the compression strength of dentin, an appearance of micro-cracks in front of the main cracks is observed. The micro-cracks are inclined (~60°) to the trajectory of the main cracks. The further growth of the main cracks is not realized due to the junction with the micro-cracks; we assume that the micro-cracks dissipate the energy of the main crack and suppressed its growth. These micro-cracks serve as additional stress accommodations, therefore the samples do not break apart after the compression test, as it is usually observed under bending and tension tests.
Die Einführung von Wasserstoff als sicherer Energieträger braucht eine robuste Wissensbasis, darauf aufgebaute Werkzeuge zur Auslegung und Sicherheitsbewertung von Wasserstofftechnologien und ein international harmonisiertes Regelwerk. Viele der innovativen Technologien implizieren Wasserstoff bei hohen Drücken und/oder kryogenen Temperaturen, mit denen in verteilten Anwendungen erstmalig private Nutzer in Kontakt kommen. Um überkonservative, teure Sicherheitslösungen zu vermeiden, gleichzeitig aber die Einsetzbarkeit und Sicherheit von Wasserstoffanwendungen zu demonstrieren und die Akzeptanz für die Technologie aufrecht zu halten, muss auch die Sicherheitsforschung mit den Trends der technologischen Entwicklung Schritt halten, oder sie besser noch antizipieren. So beschreibt dieser Überblicksartikel nicht nur den gegenwärtigen Stand der Kenntnisse und Technik bezüglich Wasserstoffsicherheit, sondern auch ihre Weiterentwicklung.
Alkali-aktivierte Hüttensandbetone – CO2-reduzierte Bindemittel mit hohem Korrosionsschutzpotential
(2023)
Durch den Ersatz von Portlandzement können alkali-aktivierte Bindemittel einen bedeutenden Beitrag zur Verringerung der durch die Zementklinkerherstellung verursachten CO2-Emissionen leisten. Für die Verwendung von alkali-aktivierten Bindemitteln in Stahlbetonkonstruktionen, die Chloriden oder Carbonatisierung ausgesetzt sind, ist die Fähigkeit des Stahls, den passiven Zustand zu erreichen und aufrechtzuerhalten, von großer Bedeutung. Die Prozesse der Deckschichtbildung von Stahl in alkali-aktivierten Materialien unterscheiden sich jedoch zum Teil grundlegend von denen in Portlandzementen. Alkali-aktivierte Hüttensandbetone weisen gute technische Eigenschaften auf, bisher fehlen jedoch grundlegende Kenntnisse bzgl. ihrer schützenden Wirkung bei korrosiven Angriffen. Dies ist vor allem auf ihre sulfidhaltige Porenlösung zurückzuführen, welche die elektrochemischen Eigenschaften der Stahloberfläche beeinflusst und die Verwendung herkömmlicher Bewertungsmaßstäbe erschwert. Es werden erste Ergebnisse eines DFG-Forschungsprojektes vorgestellt, in dem das Passivierungsverhalten von Stahl in alkali-aktivierten Hüttensandmörteln unterschiedlicher Zusammensetzungen sowie in Mörteln auf Basis hüttensandhaltiger Normzemente untersucht wird. Über einen Zeitraum von mindestens 28 Tagen werden an Zylinderprüfkörpern im 3-Elektroden-Aufbau das Ruhepotential sowie die Polarisationswiderstände der Stahlelektroden ermittelt.
REALight ‐ Leichtgranulate und REA‐Gips aus feinkörnigen sulfatbelasteten Bau‐ und Abbruchabfällen
(2023)
Ziel des Projekts REALight ist die Entwicklung einer Referenzanlage zur Herstellung von Leichtgranulaten (leichte Gesteinskörnungen) aus Bau‐ und Abbruchabfällen und zur Gipsrückgewinnung. Als Rohstoffe werden bisher ungenutzte oder auf niedrigem Niveau eingesetzte Bau‐ und Abbruchabfälle und industrielle Nebenprodukte verwendet. Als Produkte werden leichte Gesteinskörnungen hergestellt. Die Sulfatabtrennung durch eine thermische Zersetzung bildet die Grundlage für die zusätzliche Gewinnung von Rauchgasentschwefelungs‐Gips (REA‐Gips). Das Projekt wird im Rahmen der Fördermaßnahme „Ressourceneffiziente Kreislaufwirtschaft – Bauen und Mineralische Stoffkreisläufe (ReMin)” gefördert. ReMin ist eine Maßnahme zur Umsetzung des BMBF‐Forschungskonzepts „Ressourceneffiziente Kreislaufwirtschaft” als Teil der BMBF Strategie „Forschung für nachhaltige Entwicklung – FONA”. Ziel der Förderung ist es, den Ausbau der Kreislaufwirtschaft voranzutreiben. Im Mittelpunkt steht dabei die Bauwirtschaft mit ihrer hohen Nachfrage nach Rohstoffen und gleichzeitig großen Mengen an anfallenden mineralischen Abfällen. Am Projekt REALight sind 12 Partner aus verschiedenen Bereichen der Baustoffherstellung und ‐anwendung, Abfallaufbereitung, Verfahrenstechnik sowie Forschung und Entwicklung beteiligt.
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.
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.
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.
Im Jahr 2020 fielen in Deutschland rund 220 Millionen Tonnen mineralische Bau- und Abbruchabfälle an, die als Sekundärrohstoffquelle genutzt werden können. Trotz hoher Recyclingquoten wird ein Teil der mineralischen Bau- und Abbruchabfälle immer noch deponiert oder in Anwendungen mit geringen Qualitätsanforderungen eingesetzt, da ein effektives Recycling dieser heterogenen Abfälle recht kompliziert ist. Bauschutt ist ein heterogener, SiO2-reicher Sekundärrohstoff, der sich aus einem Gemisch verschiedener abgebrochener Baumaterialien wie Ziegel, Betonfertigteile, Leichtbeton, Porenbeton, Kalksandsteine, Natursteine, Gips und Mörtel zusammensetzt. Die genaue Zusammensetzung hängt von der Abbruchstelle, der Vorsortierung und der Wiederaufbereitung in der Recyclinganlage ab. Eine direkte Wiederverwendung als rezyklierte Gesteinskörnung ist aufgrund der uneinheitlichen Zusammensetzung und des bis zu 50 %igen Feinanteils nach der mechanischen Aufbereitung nicht zulässig. Eine Möglichkeit, Mauerwerksschutt effektiv zu recyceln, ist die rohstoffliche Verwertung über ein chemisch-hydrothermales Umwandlungsverfahren, das poröse Granulate erzeugt. Durch die Porenstruktur dieser hydrothermal gehärteten Granulate ergeben sich Anwendungsmöglichkeiten als Filter- oder Wasserspeichermaterial, die über den Bausektor hinausgehen. Diese neuartigen Granulate können leichte Gesteinskörnungen natürlichen Ursprungs (z. B. Lavasand, Bimsstein) oder Körner aus natürlichen Rohstoffen (z. B. Blähton) ersetzen. Die neue Recyclingstrategie spart natürliche Ressourcen. Im Vergleich zur Herstellung von Blähton ist der Energieverbrauch wesentlich geringer. Ziel des Verbundprojektes HYTEGRA war die Entwicklung eines Verfahrens zur Herstellung von leichten Gesteinskörnungen aus SiO2- und CaO-reichen Sekundärrohstoffen. Als Rohstoffe wurden Mauerwerksschutt als SiO2-Quelle und Papierasche aus der energetischen Verwertung von Reststoffen der Altpapierverwertung als CaO-Quelle eingesetzt. Der komplette Prozess von der mechanisch-physikalischen Aufbereitung über die Bildung des Grüngranulats bis zur hydrothermalen Härtung wurde entwickelt und im Labormaßstab getestet. Die Anwendungen des hydrothermal gehärteten Granulats als Wasserspeichermaterial für die innere Nachbehandlung von hochfestem Beton, Pflanzensubstrat und Filtermaterial in Bodenfiltern zur Abwasserreinigung wurden untersucht. Der Beitrag gibt einen Überblick über die wichtigsten Ergebnisse des erfolgreich abgeschlossenen Verbundforschungsprojekts HYTEGRA.
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.
Refractory chemically complex alloys with bcc-based microstructures show great potential for high-temperature applications but most of them exhibit limited room-temperature ductility, which remains a challenge. One such example is the AlMo0.5NbTa0.5TiZr alloy, mainly consisting of a nano-scaled structure with an ordered B2 matrix and a high-volume fraction of aligned cuboidal and coherently embedded A2 precipitates. This work aims to investigate how the cooling rate after hot isostatic pressing of the AlMo0.5NbTa0.5TiZr alloy affects its microstructure and its resulting hardness and fracture toughness at room temperature. A slow cooling rate of 5 °C/min leads to a coarse microstructure consisting of aligned slabs (mean A2 precipitate ≈ 25 nm) with a nanohardness of about 8 GPa. In contrast, after the fastest cooling rate (30 °C/min), the A2 precipitates become more cubic with an edge length of ≈ 16 nm, resulting in an increase in nanohardness by 10 %. The fracture toughness is roughly independent of the cooling rate and its mean value (≈ 4.2 MPa∙m1/2) resembles that of some B2 intermetallics and other A2/B2 alloys. As the lattice misfit between the A2 and B2 phases is known to play a key role in microstructure formation and evolution, its temperature dependence between 20 and 900 °C was investigated. These findings offer insights into the evolution of the microstructure and room-temperature mechanical properties of the AlMo0.5NbTa0.5TiZr alloy, which could help the development of advanced chemically complex alloys.
Understanding the mechanical behavior of silicon nanowires is essential for the implementation of advanced nanoscale devices. Although bending tests are predominantly used for this purpose, their findings should be properly interpreted through modeling. Various modeling approaches tend to ignore parts of the effective parameter set involved in the rather complex bending response. This oversimplification is the main reason behind the spread of the modulus of elasticity and strength data in the literature. Addressing this challenge, a surface-based nanomechanical model is introduced in this study. The proposed model considers two important factors that have so far remained neglected despite their significance: (i) intrinsic stresses composed of the initial residual stress and surface-induced residual stress and (ii) anisotropic implementation of surface stress and elasticity. The modeling study is consolidated with molecular dynamics-based study of the native oxide surface through reactive force fields and a series of nanoscale characterization work through in situ threepoint bending test and Raman spectroscopy. The treatment of the test data through a series of models with increasing complexity demonstrates a spread of 85 GPa for the modulus of elasticity and points to the origins of ambiguity regarding silicon nanowire properties, which are some of the most commonly employed nanoscale building blocks. A similar conclusion is reached for strength with variations of up to 3 GPa estimated by the aforementioned nanomechanical models. Precise consideration of the nanowire surface state is thus critical to comprehending the mechanical behavior of silicon nanowires accurately. Overall, this study highlights the need for a multiscale theoretical framework to fully understand the size-dependent mechanical behavior of silicon nanowires, with fortifying effects on the design and reliability assessment of future nanoelectromechanical systems.
A pseudosymmetric description of the crystal lattice derived from a single wideangle Kikuchi pattern can have several causes. The small size (<15%) of the sector covered by an electron backscatter diffraction pattern, the limited precision of the projection centre position and the Kikuchi band definition are crucial. Inherent pseudosymmetries of the crystal lattice and/or structure also pose a challenge in the analysis of Kikuchi patterns. To eliminate experimental errors as much as possible, simulated Kikuchi patterns of 350 phases have been analysed using the software CALM [Nolze et al. (2021). J. Appl. Cryst. 54, 1012–1022] in order to estimate the frequency of and reasons for pseudosymmetric crystal lattice descriptions. Misinterpretations occur in particular when the atomic scattering factors of non-equivalent positions are too similar and reciprocal-lattice points are systematically missing. As an example, a pseudosymmetry prediction depending on the elements involved is discussed for binary AB compounds with B1 and B2 structure types. However, since this is impossible for more complicated phases, this approach cannot be directly applied to compounds of arbitrary composition and structure.
Fatigue tests were performed on the forged aluminum alloy EN AW-2618A in the T61 state. Different stress ratios (R = -1, R = 0.1) were selected to study the influence of mean stress on fatigue life. Two overaged states (10 h/230 ◦C, 1000 h/230 ◦C) were also tested to investigate the influence of overaging on fatigue life. Transmission electron microscopy (TEM) was used to characterize the precipitates (S-phase), which are mainly responsible for the strength of the alloy. A fractographic analysis was also performed to determine the failure mode. Overaging reduces the fatigue life compared to the T61 state. The longer the aging time, the lower the fatigue resistance. The reason is the decrease in (yield) strength, which correlates with the radius of the S-phase: the precipitate radius increases by a factor of approximately two for the overaged states compared to the initial state. The analysis of the fracture surfaces showed crack initiation occurs predominantly on the outer surface and is
associated with the primary phases.
The derivation of a crystal structure and its phase-specific parameters from a single wide-angle backscattered Kikuchi diffraction pattern requires reliable extraction of the Bragg angles. By means of the first derivative of the lattice profile, an attempt is made to determine fully automatically and reproducibly the band widths in simulated Kikuchi patterns. Even under such ideal conditions (projection centre, wavelength and lattice plane traces are perfectly known), this leads to a lattice parameter distribution whose mean shows a linear offset that correlates with the mean atomic number Z of the pattern-forming phase. The consideration of as many Kikuchi bands as possible reduces the errors that typically occur if only a single band is analysed. On the other hand, the width of the resulting distribution is such that higher image resolution of diffraction patterns, employing longer wavelengths to produce wider bands or the use of higher interference orders is less advantageous than commonly assumed.
A band width determination using the first derivative of the band profile systematically underestimates the true Bragg angle. Corrections are proposed to compensate for the resulting offset Δa/a of the mean lattice parameters derived from as many Kikuchi band widths as possible. For dynamically simulated Kikuchi patterns, Δa/a can reach up to 8% for phases with a high mean atomic number Z, whereas for much more common low-Z materials the offset decreases linearly. A predicted offset Δa/a = f(Z) is therefore proposed, which also includes the unit-cell volume and thus takes into account the packing density of the scatterers in the material. Since Z is not always available for unknown phases, its substitution by Zmax, i.e. the atomic number of the heaviest element in the compound, is still acceptable for an approximate correction. For simulated Kikuchi patterns the offset-corrected lattice parameter deviation is Δa/a < 1.5%. The lattice parameter ratios, and the angles α, β and γ between the basis vectors, are not affected at all.1.5%. The lattice parameter ratios, and the angles , and between the basis vectors, are not affected at all.
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.