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AbstractMicroplastics (MP) can be detected in all environmental systems. Marine and terrestrial aquatic systems, especially the transported suspended solids, have often been the focus of scientific investigations in the past. Sediments of aquatic river systems, on the other hand, were often ignored due to the time‐consuming sample preparation and analysis procedures. Spectroscopic measurement methods counting particle numbers are hardly suitable as detection methods, because there are plenty of natural particles next to a small number of MP particles. Integral methods, such as thermoanalytical methods are determining the particle mass independently of the inorganic components.In this study, a workflow for sample preparation via density separation and subsequent analysis by thermal extraction desorption‐gas chromatography/mass spectrometry is presented, which leads to representative and homogeneous samples and allows fast and robust MP mass content measurements suitable for routine analysis. Polymers were identified and quantified in all samples. Polyethylene and styrene‐butadiene rubber are the dominant polymers, besides polypropylene and polystyrene. Overall, total polymer masses between 1.18 and 337.0 µg/g could be determined. Highest MP concentrations in riverbed sediment are found in sites characterized by low flow velocities in harbors and reservoirs, while MP concentrations in sandy/gravelly bed sediments with higher flow velocities are small.
The LOBSTER (Deringer et al., 2011;Maintz et al., 2013 ,2016 ;Nelson et al., 2020 ) software aids in extracting quantum-chemical bonding information from materials by projecting the plane-wave based wave functions from density functional theory (DFT) onto an atomic orbital basis. LobsterEnv, a module implemented in pymatgen (Ong et al., 2013) by some of the authors of this package, facilitates the use of quantum-chemical bonding information obtained from LOBSTER calculations to identify neighbors and coordination environments. LobsterPy is a Python package that offers a set of convenient tools to further analyze and summarize the LobsterEnv outputs in the form of JSONs that are easy to interpret and process. These tools enable the estimation of (anti) bonding contributions, generation of textual descriptions, and visualization of LOBSTER computation results. Since its first release, both LobsterPy and LobsterEnv capabilities have been extended significantly. Unlike earlier versions, which could only automatically analyze Crystal Orbital Hamilton Populations (COHPs) (Dronskowski & Blöchl, 1993), both can now also analyze Crystal Orbital Overlap Populations (COOP) (Hughbanks & Hoffmann, 1983) and Crystal Orbital Bond Index (COBI) (Müller et al., 2021). Extracting the information about the most important orbitals contributing to the bonds is optional, and users can enable it as needed. Additionally, bonding-based features for machinelearning (ML) studies can be engineered via the sub-packages “featurize” and “structuregraphs”. Alongside its Python interface, it also provides an easy-to-use command line interface (CLI) that runs automatic analysis of the computations and generates a summary of results and publication-ready figures. LobsterPy has been used to produce the results in Ngo et al. (2023), Chen et al. (2024), Naik et al. (2023), and it is also part of Atomate2 (2023) bonding analysis workflow for generating bonding analysis data in a format compatible with the Materials Project (Jain et al., 2013) API.
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.
AbstractThe high-temperature corrosion behaviors of the equimolar CrCoNi medium-entropy alloy and CrMnFeCoNi high-entropy alloy were studied in a gas atmosphere consisting of a volumetric mixture of 10% H2O, 2% O2, 0.5% SO2, and 87.5% Ar at 800 °C for up to 96 h. Both alloys were initially single-phase fcc with a mean grain size of ~ 50 μm and a homogeneous chemical composition. The oxide layer thickness of CrMnFeCoNi increased linearly with exposure time while it remained constant at ~ 1 μm for CrCoNi. A Cr2O3 layer and minor amounts of (Co,Ni)Cr2O4 developed on the latter while three oxide layers were detected on the former, i.e., a thin and continuous chromium rich oxide layer at the oxide/alloy interface, a dense (Mn,Cr)3O4 layer in the center and a thick and porous layer of Mn3O4 and MnSO4 at the gas/oxide interface. Additionally, a few metal sulfides were observed in the CrMnFeCoNi matrix. These results were found to be in reasonable agreement with thermodynamic calculations.
The production of plastics is rising since they have been invented. Micro, submicro- and nanoplastics are produced intentionally or generated by environmental processes, and constitute ubiquitous contaminants which are ingested orally by consumers. Reported health concerns include intestinal translocation, inflammatory response, oxidative stress and cytotoxicity. Every digestive milieu in the gastrointestinal tract does have an influence on the properties of particles and can cause changes in their effect on biological systems. In this study, we subjected plastic particles of different materials (polylactic acid, polymethylmethacrylate, melamine formaldehyde) and sizes (micro- to nano-range) to a complex artificial digestion model consisting of three intestinal fluid simulants (saliva, gastric and intestinal juice). We monitored the impact of the digestion process on the particles by performing Dynamic Light Scattering, Scanning Electron Microscopy and Asymmetric Flow Field-Flow Fractionation. An in vitro model of the intestinal epithelial barrier was used to monitor cellular effects and translocation behavior of (un)digested particles. In conclusion, artificial digestion decreased cellular interaction and slightly increased transport of all particles across the intestinal barrier. The interaction with organic matter resulted in clear differences in the agglomeration behavior. Moreover, we provide evidence for polymer-, size- and surface-dependent cellular effects of the test particles.
We present Jobflow, a domain-agnostic Python package for writing computational workflows tailored for high-throughput computing applications. With its simple decorator-based approach, functions and class methods can be transformed into compute jobs that can be stitched together into complex workflows. Jobflow fully supports dynamic workflows where the full acyclic graph of compute jobs is not known until runtime, such as compute jobs that launch
other jobs based on the results of previous steps in the workflow. The results of all Jobflow compute jobs can be easily stored in a variety of filesystem- and cloud-based databases without the data storage process being part of the underlying workflow logic itself. Jobflow has been intentionally designed to be fully independent of the choice of workflow manager used to dispatch the calculations on remote computing resources. At the time of writing, Jobflow
workflows can be executed either locally or across distributed compute environments via an adapter to the FireWorks package, and Jobflow fully supports the integration of additional workflow execution adapters in the future.
Laser powder bed fusion of metallic components (PBF-LB/M) is gaining acceptance in industry. However, the high costs and lengthy qualification processes required for printed components create the need for more effective in-situ monitoring and testing methods. This article proposes multispectral Optical Tomography (OT) as a new approach for monitoring the PBF-LB/M process. Compared to other methods, OT is a low-cost process monitoring method that uses long-time exposure imaging to observe the build process. However, it lacks time resolution compared to expensive thermographic sensor systems. Monochromatic OT (1C-OT) is already commercially available and observes the building process layer-wise using a single wavelength window in the NIR range. Multispectral OT (nC-OT) utilizes a similar setup but can measure multiple wavelength ranges per location simultaneously. By comparing the classical 1C-OT and nC-OT approaches, this article examines the advantages of nC-OT (two channel OT and RGB-OT) in reducing the false positive rate for process deviations and approximating maximum temperatures for a better comparison between different build processes and materials. This could ultimately reduce costs and time for part qualification. The main goal of this contribution is to assess the advantages of nC-OT compared to 1C-OT for in-situ process monitoring of PBF-LB/M.
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.
Titanium and its alloys are known to allow the straightforward laser-based manufacturing of ordered surface nanostructures, so-called high spatial frequency laser-induced periodic surface structures (HSFL). These structures exhibit sub-100 nm spatial periods – far below the optical diffraction limit. The resulting surface functionalities are usually enabled by both, topographic and chemical alterations of the nanostructured surfaces. For exploring these effects, multi-method characterizations were performed here for HSFL processed on Ti–6Al–4V alloy upon irradiation with near-infrared ps-laser pulses (1030 nm, ≈1 ps pulse duration, 1–400 kHz) under different laser scan processing conditions, i.e., by systematically varying the pulse repetition frequency and the number of laser irradiation passes. The sample characterization involved morphological and topographical investigations by scanning electron microscopy (SEM), atomic force microscopy (AFM), tactile stylus profilometry, as well as near-surface chemical analyses hard X-ray photoelectron spectroscopy (HAXPES) and depth-profiling time-of-flight secondary ion mass spectrometry (ToF-SIMS). This provides a quantification of the laser ablation depth, the geometrical HSFL characteristics and enables new insights into the depth extent and the nature of the non-ablative laser-induced near-surface oxidation accompanying these nanostructures. This allows to answer the questions how the processing of HSFL can be industrially scaled up, and whether the latter is limited by heat-accumulation effects.
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.
Black writing materials of different types and compositions have varied in use over time and different geographical regions. With this paper, we would like to contribute to their study by listing and reviewing recipes for black writing inks that were in circulation in the Carolingian Empire as well as by referencing the archaeometric analyses of the black inks used in the manuscripts. The studies presented here that involved the humanities and natural sciences provide new insights into how the scholars of the early Medieval Ages organized manuscripts.
Admixtures are important constituents to enhance the performance of concrete. They allow for more efficient use of binders which can mitigate negative environmental impacts from producing cement-based materials. Commonly used rheology modifying agents like polycarboxylate ethers or cellulose ethers are synthetic or semi-synthetic, respectively. This requires additional energy consumption for their production and global supply chains particularly for many developing regions, which will be large consumers of concrete in the future. However, many locally available bio-based polysaccharides could be effectively used instead. These polymers are often overlooked by engineers and scientists due to their limited distribution and inherent complexity, yet they represent an underleveraged source of precursors for admixtures. This study investigates the action mechanisms of some bio-based rheology modifying agents, i.e., acacia gum and miscanthus gum, and provides a comparison to a conventionally modified starch. The results show that the mechanism of action of these polymers is closely related to the composition of the mixture, mixing regime, and the composition of the aqueous phase. Depending on the agent, either plasticizing or stabilizing effects on rheology can be revealed.
This study was carried out to investigate the neutron transmission signal as a function of sample temperature during a welding process. A theoretical description that includes the Debye-Waller factor was used to describe the temperature influence on the neutron crosssections. Neutron imaging using a monochromatic beam helps to observe transmission variations related to the material temperature. In-situ neutron imaging of welding experiments show the distribution of the temperature in bulk steel samples. The performed finite element modelling of expected temperature distributions shows good agreement with the obtained experimental data.
In this study, a wound dressing composed of an alginate dialdehyde−gelatin (ADA-GEL) hydrogel incorporated by astaxanthin (ASX) and 70B (70:30 B2O3/CaO in mol %) borate bioactive glass (BBG) microparticles was developed through 3D printing. ASX and BBG particles sti.ened the composite hydrogel construct and delayed its in vitro degradation compared to the pristine hydrogel construct, mainly due to their cross-linking role, likely arising from hydrogen bonding between the ASX/BBG particles and ADA-GEL chains. Additionally, the composite hydrogel construct could hold and deliver ASX steadily. The composite hydrogel constructs codelivered biologically active ions (Ca and B) and ASX, which should lead to a faster, more e.ective wound-healing process. As shown through in vitro tests, the ASX-containing composite hydrogel promoted fibroblast (NIH 3T3) cell adhesion, proliferation, and vascular endothelial growth factor expression, as well as keratinocyte (HaCaT) migration, thanks to the antioxidant activity of ASX, the release of cell-supportive Ca2+ and B3+ ions, and the biocompatibility of ADA-GEL. Taken together, the results show that the ADA-GEL/BBG/ASX composite is an attractive biomaterial to develop multipurposed wound-healing constructs through 3D printing.
Iron aluminides, already reported in the late 19th century, did not cease to attract the interest of scientists and engineers ever since. Besides good oxidation resistance, low density and resource availability, potentials for hightemperature strengths that compete with high-alloy steels were unlocked by low alloy contents. Still, research on alloy design continues, as alloying usually comes at the price of brittleness in low-temperature regimes. A potential candidate is the quinary Fe–Al–Mo–Ti–B system which is strengthened by solid solution and eutectic borides. It was shown to have good strength and outstanding creep resistance under compressive loading up to elevated temperatures. Although the individual effect of alloy additions is well understood in iron aluminides, little is known about the combined effects of alloying concentrations on microstructure, phase stability and mechanical properties. Therefore a systematic study of two Ti-doped near-Fe3Al alloys with varying contents of Mo (2–4 at.%) and B (0.5–1 at.%) was conducted. In total eight different alloys were fabricated by investment casting into ceramic shell molds. Alloys were characterized and compared by grain size, phase transitions, microstructure evolution as well as elemental compositions and volume fractions of phases. For mechanical characterization, macrohardness and microhardness tests as well as tensile tests at ambient and high tempera tures were conducted. Independent of alloy additions, alloys with 24–25 at.% Al exhibit superior proof strength due to a higher matrix hardness. Decreasing B content generally decreases strength by lower secondary phase fractions which contribute via particle hardening. Reducing Mo content decreases both the solute concentration in the matrix and secondary phase fractions. Surprisingly, strength is similar or even superior to alloys with higher Mo content. Strength relations are discussed with a focus on solid-solution hardening theory and other competing strengthening mechanisms.
A giant Zn segregation transition is revealed using CALPHAD-integrated density-based modeling of segregation into Fe grain boundaries (GBs). The results show that above a threshold of only a few atomic percent Zn in the alloy, a substantial amount of up to 60 at.% Zn can segregate to the GB. We found that the amount of segregation abruptly increases with decreasing temperature, while the Zn content in the alloy required for triggering the segregation transition decreases. Direct evidence of the Zn segregation transition is obtained using high-resolution scanning transmission electron microscopy. Base on the model, we trace the origin of the segregation transition back to the low cohesive energy of Zn and a miscibility gap in Fe-Zn GB, arising from the magnetic ordering effect, which is confirmed by ab-initio calculations. We also show that the massive Zn segregation resulting from the segregation transition greatly assists with liquid wetting and reduces the work of separation along the GB. The current predictions suggest that control over Zn segregation, by both alloy design and optimizing the galvanization and welding processes, may offer preventive strategies against liquid metal embrittlement.
Viscosity modifying agents: Key components of advanced cement-based materials with adapted rheology
(2022)
Viscosity modifying agents (VMAs) are essential ingredients for the production of flowable cement-based materials. This paper presents an overview of commonly used VMAs and attempts to shed some light on the underlying physics at the origin of their mechanisms of action. The main molecular parameters of VMA controlling the rheological properties of the cement pore solution are highlighted. As the mechanisms of action of VMAs in cement-based materials are closely related to their affinity with the surface of cement particles, the adsorption of the main VMA types is discussed. The effect of VMAs on flow properties and stability of cement-based materials is presented for VMAs added without any superplasticizer, and then in systems incorporating both VMAs and superplasticizers. Finally, the effect of VMAs in enhancing concrete properties to secure adequate performance of different construction applications, and perspectives for future developments of novel cement-based materials made with VMAs are showcased.
FAIR (findable, accessible, interoperable and reusable) data usage is one of the main principals that many of the research and funding organizations include in their strategic plans, which means that following the main principals of FAIR data is required in many research projects. The definition of data being FAIR is very general. When implementing that for a specific application or project or even setting a standardized procedure within a working group, a company or a research community, many challenges arise. In this contribution, an overview about our experience with different methods and tools is outlined.
We begin with a motivation on potential use cases for the application of FAIR data with increasing complexity starting from a reproducible research paper over collaborative projects with multiple participants such as Round-Robin tests up to data-based models within standardization codes, applications in machine learning or parameter estimation of physics-based simulation models.
In a second part, different options for structuring the data (including metadata schema) are discussed. The first one is the openBIS system, which is an open-source lab notebook and PostgreSQL based data management system. A second option is a semantic representation using RDF based on ontologies for the domain of interest.
In a third section, requirements for workflow tools to automate data processing are discussed and their integration into reproducible data analysis is presented with an outlook on required information to be stored as metadata in the database.
Finally, the presented procedures are exemplarily demonstrated for the calibration of a temperature dependent constitutive model for additively manufactured mortar. A metadata schema for a rheological measurement setup is derived and implemented in an openBIS database. After a short review of a potential numerical model predicting the structural build-up behavior, the automatic workflow to use the stored data for model parameter estimation is demonstrated.
In this article, we present two Coptic papyri, P 11934 and P 11935 from the Berlin collection excavated in Ashmunein (ancient Hermopolis) by Otto Rubensohn in 1906. We employ a multi-disciplinary approach that takes into account both their materiality – writing support as well as ink – and their content, as has become ‘best practice’. 1 Material aspects of written documents have traditionally been the purview of papyrologists. Recently developed methods of scientific analysis generate sets of archaeometric data with the potential to improve understanding of the materiality of ancient document production, as well as to yield new evidence for genuine papyrological research questions. To achieve this, a large corpus of comparative data needs to be built. Our contribution offers a first step in this direction. We aim at presenting the papyri, which were selected because of the ink corrosion during conservation work at the Berlin collection, in a format that is exhaustive both for material and textual aspects. The inks from both papyri were analysed using a combination of techniques, contributing to our better understanding of the development of ink technology in Late Antiquity.
The prediction of the properties of the materials used in the operation of components is of enormous importance, in order to accelerate the development process of new components. To evaluate new materials in terms of their performance (in a component), the development of new innovative methods is necessary. These methods can also be summarized under the term lab-to-field or materials – upscaling, meaning materials being characterised in a laboratory and their properties being upscaled to the component performance by means of e.g. simulation. i-TRIBOMAT is a EU funded project (H2020, GA Nr. 814494) aiming at building an Open Innovation Test Bed for tribological material characterization and offering corresponding services from tribological characterization of new materials to simulation models for predicting the performance of industrial components. By bundling the infrastructure, know-how for characterization and building a digital platform, i-TRIBOMAT becomes the world’s largest open innovation test bed for tribological material characterization.
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.
Microplastic particles with sizes between 1 to 1000 μm are widely distributed worldwide. Origin, transport pathways and fate are poorly known, as sampling, sample preparation and detection methods are major challenges. In addition, reference materials that mimic environmental particles are lacking. Most challenging is the yield of MP particle production and the need for resource-intensive grinding with liquid nitrogen. In this paper, a machine is designed to produce aged microplastic particles as reference material candidates with high yield. The machine is based on ultraviolet aging of a thin foil and mechanical fragmentation using clean air. An example of aging and fragmentation of high density polyethylene with additional physical and chemical characterization of shape, size, aging state by carbonyl index and density is presented.
Duplex stainless steels (DSS) are frequently used, especially in applications requiring high strength combined with high corrosion resistance in aggressive media. Examples include power plant components and maritime structures. During welding of these steels, local variations in chemical composition can occur. This results in ferritization of the material and negatively affects the mechanical properties of the components. In this work, tungsten inert gas (TIG) welding experiments were performed with DSS. Chemical composition analysis was realized in situ by using Laser Induced Breakdown Spectroscopy (LIBS). The aim of the work is to quantitatively measure the chemical composition in the weld seam of various DSS and to identify possible influences of welding parameters on the microstructure of the material. The chemical concentrations of the main alloying elements Cr, Ni, Mn on the surface of the sample during the welding process and the cooling process were measured. Mn and Ni are austenite stabilizers and their content increases during welding by using certain high alloyed filler material. Spectra were recorded every 1.3 s at a spacing of approximately 2 mm. During the cooling process the location of the measurement was not changed. The LIBS method is proofed to be suitable for the quantitative representation of the chemical compositions during the welding process.
Optical Thermometry is popular among researchers because of its non-contact, high sensitivity, and fast measurement properties. In the present experiment, Er3+/Yb3+/K+ co-doped NaYF4 nanoparticles with different K+ concentrations were synthesized by solvothermal method, and the samples showed bright upconversion green emission under the excitation of a 980 nm laser. The powder X-ray diffractometer and transmission electron microscope were used to characterize the crystal structure and its surface morphology, respectively. The spectral characteristics of nanoparticles with K+ doping concentration from 10% to 30% (Molar ratio) were investigated by fluorescence spectroscopy, and it was observed that the fluorescence intensity reached the maximum at the K+ concentration of 20%, after which the intensity weakened when the K+ content continued to increase. According to the dependence between the luminescence intensity of the sample and the laser power density and fluorescence lifetime, the intrinsic mechanism was carefully investigated. Temperature-dependent spectra of the samples were recorded in the temperature range of 315–495 K, and the maximum values of absolute sensitivity (Sa) and relative sensitivity (Sr) were measured at 0.0041 K−1 (455 K) and 0.9220%K−1 (315 K). The experimental results show that K+/Er3+/Yb3+ triple-doped NaYF4 green fluorescent nanoparticles (GFNs) have good prospects for applications in display devices, temperature sensing, and other fields.
Showcasing research from the Federal Institute for Material Research and Testing Berlin and Fraunhofer Institute for Celltherapy and Immunology Branch Bioanalytics and Bioprocesses Potsdam.
Bio-SAXS of single-stranded DNA-binding proteins: Radiation protection by the compatible solute ectoine.
We aimed to increase the possible undisturbed exposure time during bio-SAXS measurements of single-stranded DNA-binding proteins. Therefore small angle X-ray scattering was performed on Gene-V Protein (G5P/GVP), which is involved in DNA repair processes. To achieve this, irradiations were performed in presence and absence of the hydroxyl-radical scavenger and osmolyte Ectoine, which showed efficient radiation protection and prevented protein aggregation, thus allows for a non-disturbing way to improve structure-determination of biomolecules.
Laser beam welding is a widely used joining technique in many industrial applications. This is mainly due to its many unique advantages, especially compared to conventional arc welding processes. These advantages include, among others, highly concentrated energy deposition, low total heat input and a capacity to penetrate deep into the material while causing only small welding distortions.
However, at the same time, the small dimension of the laser spot, high solidification rates, and small dimensions of the weld pool itself can provoke issues regarding the assembly tolerances of the workpiece, the hot-cracking phenomena, as well as keyhole-induced bubbles escaping from the melt.
Weld pool shapes in laser beam welding are elongated at the external, free surfaces under the action of the main driving forces in the melt – such as recoil pressure and surface tension forces – while being shorter in the internal areas of the weld pool. This leads to a regular solidification sequence from the internal zones toward the free surfaces, e.g. from the bottom to the top in partial penetration welding. However, in recent studies reported in the literature and seen in the experimental and numerical investigations of BAM Bundesanstalt für Materialforschung und -prüfung in Berlin, it was found that an internal narrowing phenomenon can occur that is often accompanied by a distinct bulging of the weld bead in deeper zones.
As the internal behaviour of the melt during the process is hardly optically accessible, several numerical models and experimental techniques were established to visualise the mechanisms of the formation of the bulging and the narrowing phenomenon and to reveal the consequences on the solidification sequence, pore formation, and filler metal dilution.
This study reflects typical consumer textile washing behaviour while taking into account existing standards in the household appliance and garment industries. Two garments were washed repeatedly with artificial dirt and detergent 30 times. The collected washing water was separated using fractional filtration. Textile physical tests were used to follow property changes of the garments, the microplastic release is determined using thermoextraction/desorbtion–gas chromatography/mass spectrometry and the total organic carbon was measured as a sum parameter for the organic bonded carbon. This article shows the importance of a reality‐based approach when investigating microplastics of textile origin in the laundry care process. Deposits of detergent and dirt on the textiles were detected. The total mass of sieve residues was much higher than the release of synthetic polymers. The cotton content of the garments causes a much higher fibre release than synthetic fibres. Both will lead to false results by purely gravimetric analysis because nonpolymer fibres will be included microplastic mass. The results cannot be generalised only by the main polymer type, knowledge of the textile construction must be included for final evaluation.
Colours on East Asian Maps
(2023)
Maps and colours have a close connection. Drawn or printed in black on white, subsequently added colours enhance maps with additional information. Colours were not just there to improve maps aesthetically, but they regulated how they were read and thus reinforced their meanings, significances and ideas. Colour is an important key to a more precise understanding of the map’s purposes and uses; moreover, colours are also an important aspect of a map’s materiality. The material scientific analysis makes it possible to find out more about the making of colours and the process of colouring maps. By skillfully deploying colours, map colourists were able to create mimetic representations of nature or codify information in an abstract form. The use of colours involved many considerations as to the materials. ‘Reading’ colours in this way gives a glimpse into the social lives of mapmakers as well as map users and reveals the complexity of the historical and social context in which maps were produced and how the maps were actually made. Within the scope of the three-year joint research project Coloured Maps (2018–2021), we undertook an in-depth and systematic study of hand-drawn and hand-coloured maps from East Asia in the Museum am Rothenbaum (MARKK) in Hamburg and produced between the seventeenth and twentieth centuries.
With a multi-perspective approach and transdisciplinary methods (humanities and the sciences), we were able to pool and compare the research results from different fields of research on Asian maps. The aim of this publication is to provide a first general overview of the subject of colours on maps in East Asia in the period from the seventeenth to the early twentieth century and to stimulate further research on the topic.
Metastable austenitic stainless steel (304L) samples with a rectangular cross-section were plastically deformed in torsion during which they experienced multiaxial stresses that led to a complex martensitic phase distribution owing to the transformation induced plasticity effect. A three-dimensional characterization of the phase distributions in these cm-sized samples was carried out by wavelength-selective neutron tomography. It was found that quantitatively correct results are obtained as long as the samples do not exhibit any considerable preferential grain orientation. Optical microscopy, electron backscatter diffraction, and finite element modeling were used to verify and explain the results obtained by neutron tomography. Altogether, neutron tomography was shown to extend the range of microstructure characterization methods towards the meso- and macroscale.
In recent years, thermoextraction/desorption-gas chromatography/mass spectrometry (TED-GC/MS) has been developed as a rapid detection method for the determination of microplastics (MP) mass contents in numerous environmentally relevant matrices and, in particular, for the measurement of polymers in water samples without time-consuming sample preparation. The TED-GC/MS method was applied to investigate a typical European municipal wastewater system for possible MP masses. Such investigations are important in view of the recent revision of the Urban Wastewater Treatment Directive. Four different representative sampling sites were selected: greywater (domestic wastewater without toilet), combined sewer, and influent and effluent of a wastewater treatment plant (WWTP). All samples were collected by fractional filtration. Filtration was carried out over mesh sizes of 500, 100, 50, and in some cases, 5 µm. Polyethylene (PE), polypropylene (PP), and polystyrene (PS) were detected in all samples, with the PE fraction dominating in all cases. Styrene-butadiene rubber which serves as an indication of tire abrasion, was only found in the influent of the WWTP. The highest MP mass contents were found in the combined sewer, so MP can become a source of pollution during heavy rain events when the capacity limits of the effluent are reached, and the polluted effluent is released uncontrolled into the environment. Based on the studies, MP retention from the WWTP could be estimated to be approximately 96%. Few trends in polymer type or mass contents were detected within the different fractions of the samples or when comparing samples to each other.
Tracking waterborne microplastic (MP) in urban areas is a challenging task because of the various sources and transport pathways involved. Since MP occurs in low concentrations in most wastewater and stormwater streams, large sample volumes need to be captured, prepared, and carefully analyzed. The recent research in urban areas focused mainly on MP emissions at wastewater treatment plants (WWTPs), as obvious entry points into receiving waters. However, important transport pathways under wet-weather conditions are yet not been investigated thoroughly. In addition, the lack of comprehensive and comparable sampling strategies complicated the attempts for a deeper understanding of occurrence and sources. The goal of this paper is to (i) introduce and describe sampling strategies for MP at different locations in a municipal catchment area under dry and wet-weather conditions, (ii) quantify MP emissions from the entire catchment and two other smaller ones within the bigger catchment, and (iii) compare the emissions under dry and wet-weather conditions. WWTP has a high removal rate of MP (>96%), with an estimated emission rate of 189 kg/a or 0.94 g/[population equivalents (PEQ · a)], and polyethylene (PE) as the most abundant MP. The specific dry-weather emissions at a subcatchment were ≈30 g/(PEQ · a) higher than in the influent of WWTP with 23 g/(PEQ · a). Specific wet-weather emissions from large sub-catchment with higher traffic and population densities were 1952 g/(ha · a) higher than the emissions from smaller catchment (796 g/[ha · a]) with less population and traffic. The results suggest that wet-weather transport pathways are likely responsible for 2–4 times more MP emissions into receiving waters compared to dry-weather ones due to tire abrasion entered from streets through gullies. However, more investigations of wet-weather MP need to be carried out considering additional catchment attributes and storm event characteristics.
The importance of high-temperature materials made of iron aluminides (FeAl) has been increasing in light weight applications, e.g., airplane turbines, due to the high material’s specific strength. However, the highly economic production by means of permanent mold casting involves special microstructures for Fe26Al4Mo0.5Ti1B alloy components leading to difficult machinability for subsequent finishing milling and low surface qualities. Major effects of tool and machining parameter variation incorporating ultrasonic assistance on the milling process and surface integrity are shown. Loads for tool and component surface are significantly adjustable to enable an economic process chain regarding the surface integrity of safety-relevant components.
Trace elements play an important role in the fine-tuning of complex material properties. This study focuses on the correlation of microstructure, lattice misfit and creep properties. The compositionally complex alloy Al10Co25Cr8Fe15Ni36Ti6 (in at. %) was tuned with high melting trace elements Hf and W. The microstructure consists of a γ matrix, γ' precipitates and the Heusler phase and it is accompanied by good mechanical properties for high temperature applications. The addition of 0.5 at.% Hf to the Al10Co25Cr8Fe15Ni36Ti6 alloy resulted in more sharp-edged cubic γ′ precipitates and an increase in the Heusler phase amount. The addition of 1 at.% W led to more rounded γ′ precipitates and the dissolution of the Heusler phase. The shapes of the γ' precipitates of the alloys Al9.25Co25Cr8Fe15Ni36Ti6Hf0.25W0.5 and Al9.25Co25Cr8Fe15Ni36Ti6Hf0.5W0.25, that are the alloys of interest in this paper, create a transition from the well-rounded precipitates in the alloy with 1% W containing alloy to the sharp angular particles in the alloy with 0.5% Hf. While the lattice misfit has a direct correlation to the γ' precipitates shape, the creep rate is also related to the amount of the Heusler phase. The lattice misfit increases with decreasing corner radius of the γ' precipitates. So does the creep rate, but it also increases with the amount of Heusler phase. The microstructures were investigated by SEM and TEM, the lattice misfit was calculated from the lattice parameters obtained by synchrotron radiation measurements.
Mechanochemistry offers a unique opportunity to modify and manipulate crystal forms, often providing new products as compared with conventional solution methods. While promising, there is little known about how to control the solid form through mechanochemical means, demanding dedicated investigations. Using a model organic cocrystal system (isonicotinamide:glutaric acid), we here demonstrate that with mechanochemistry, polymorphism can be induced in molecular solids under conditions seemingly different to their conventional thermodynamic (thermal) transition point. Whereas Form II converts to Form I upon heating to 363 K, the same transition can be initiated under ball milling conditions at markedly lower temperatures (348 K). Our results indicate that mechanochemical techniques can help to reduce the energy barriers to solid form transitions, offering new insights into controlling polymorphic forms. Moreover, our results suggest that the nature of mechanochemical transformations could make it difficult to interpret mechanochemical solid form landscapes using conventional equilibrium-based tools.
Solidification cracking is still a serious problem in laser beam welding, especially in the welding of thick-walled plates. The influence of weld pool geometry on solidification cracking in partial penetration welding of thick plates is investigated within scope of this study. Therefore, a specific experimental setup of steel and quartz glass in butt configuration and on the side with high-speed camera were used to record the weld pool shape. In addition, the influence of laser inclination angle on the weld pool geometry and on solidification crack formation was investigated. The results show a bulge in the weld pool root, which is separated from an upper region by a necking region. This leads to a case where there are three different longitudinal region lengths with different solidification zones. This temporal sequence of solidification strongly promotes the formation of solidification cracks in the weld root.
With additive manufacturing in the powder bed, the component size is limited by the installation space. Joint welding of additively manufactured parts offers a possibility to remove this size limitation. However, due to the specific stress and microstructure state in the additively built material, it is unclear to what extent existing evaluation rules of joint welding are also suitable for welds on additive components. This is investigated using laser beam welding of additively manufactured pipe joints. The welds are evaluated by means of visual inspection, metallographic examinations as well as computed tomography. The types of defects found are comparable to conventional components. This is an indicator that existing evaluation regulations also map the possible defects occurring for weld seams on additive components.
The study deals with the influence of the heat input and the resulting cooling times on the microstructure and Charpy impact toughness of single-pass laser hybrid welded 20-mm thick high-strength steel S690QL. The main focus is on the change of the mechanical properties over the entire seam thickness. The cooling times were measured in-situ using a pyrometer and an optical fibre in three different depths of the seam where Charpy impact test specimens were also later taken. Thereby, three different heat inputs from 1.3 kJ/mm to 2 kJ/mm were investigated. Despite the observed decreased values of both t8/5-cooling time and the Charpy impact toughness in the root part of the seam, the required impact toughness of 38 J/cm2 could be reached in dependance on applied heat input, especially at the heat input of 1.6 kJ/mm.
With regard to efficient production, it is desirable to combine the respective advantages of additively and conventionally manufactured components. Particularly in the case of large-volume components that also include filigree or complex structures, it makes sense to divide the overall part into individual elements, which afterwards have to be joined by welding.
The following research represents a first step in fundamentally investigating and characterizing the joint welding of Laser Powder Bed Fusion (L-PBF) components made of Inconel 718. For this purpose, bead-on-plate welds were performed on plates manufactured using the L-PBF process and compared with the conventionally manufactured material. Conventional laser beam welding was used as welding process. The weld geometry was investigated as a function of the L-PBF build-up orientation. It was found that the welding depth and weld geometry differ depending on this orientation and in comparison to the conventional material.
In an interdisciplinary collaboration, restorers, art historians, and scientists examined Guilio Romano’s The Madonna with the Wash-Basin of 1525 (Dresden State Art Collections). Insights into the painting technique along with art historical comparisons provided the opportunity for a better understanding of the painting’s genesis, in particular concerning an early reworking of the background by the artist. A recovery and reconstruction of the earlier version of the background is now possible. The discovery of zinc in distinct passages of the painting, as well as the grey-black pigment stibnite and glass particles used as a supplement in paint layers are of special interest. The technological investigation initiated a discussion about the circumstances of the revision, as well as the painting’s relation to Vasari’s Lives of Artists.
Polychromatic and wavelength-selective neutron transmission radiography were applied during bead-on-plate welding on 5 mm thick sheets on the face side of martensitic low transformation temperature (LTT) steel plates using gas tungsten arc welding (GTAW). The in situ visualization of austenitization upon welding and subsequent α’-martensite formation during cooling could be achieved with a temporal resolution of 2 s for monochromatic imaging using a single neutron wavelength and of 0.5 s for polychromatic imaging using the full spectrum of the beam (white beam).
The spatial resolution achieved in the experiments was approximately 200 µm. The transmitted monochromatic neutron beam intensity at a wavelength of λ = 0.395 nm was significantly reduced during cooling below the martensitic start temperature M s since the emerging martensitic phase has a ~10% higher attenuation coefficient than the austenitic phase. Neutron imaging was significantly influenced by coherent neutron scattering caused by the thermal motion of the crystal lattice (Debye–Waller factor), resulting in a reduction in the neutron transmission by approx. 15% for monochromatic and by approx. 4% for polychromatic imaging.
Laser metal deposition (LMD) as an additive manufacturing technique became increasingly important in recent years and thus the demand for component safety. This is the reason, for the need for reliable in-situ defect detection techniques. For laser beam weld seams an optical measurement technique based on an optical flow algorithm was successfully used to define the critical straining conditions that lead to hot cracking. This algorithm was adapted for bead-on-plate weld seams on LMD deposited layers of IN718 alloy while performing external strain on the specimen in an externally loaded hot cacking test facility. The resulting transversal hot cracks along the weld seam were localized via X-Ray inspection and the type of cracking confirmed by Scanning Electron Microscopy (SEM). The strain distribution was measured in the vicinity of the solidification front and correlated to the detected hot cracks. Based on the results this technique could be adopted for LMD experiments.
Glasses in the systems Me2O-ZnO-B2O3 with Me = Li, Na, K, Rb (MeZB), Na2O-ZnO-CuO-B2O3 (NZCuB), CaO-ZnO-B2O3 (CaZB), and Li2O-PbO-B2O3 (LPbB) as a reference, were studied by differential thermal analysis, dilatometry, rotational viscometry, and heating microscopy. A decrease of viscosity and sintering range was found with decreasing number of fourfold coordinated boron. The viscosity of the alkali zinc borate glasses varies only slightly. LPbB and CaZB stand out by their reduced and increased viscosities, respectively. Sodium, potassium, and calcium zinc borate glasses possess a fragility above 76. All glasses were sintered to full density before crystallization. Mostly binary zinc borate phases govern crystallization. A ternary crystalline phase was detected only in the potassium containing sample. The Weinberg glass stability parameter ranges between 0.07 and 0.12. This is caused by the presence of several crystalline phases and varying melting points of even the same crystalline phase in different glass matrices.
Low melting Li2O-PbO-B2O3, Me2O-ZnO-B2O3, Me = Li, Na, K, Rb and CaO-ZnO-B2O3 glasses were studied with Raman and infrared spectroscopies to advance the structural understanding of zinc borate glasses as potential candidates for substitution of lead containing glasses. Although the effect of type of alkali ions on the number (N4) of fourfold coordinated boron (B4) in the glasses is small, the alkali ions direct the type of borate groups, i.e., pentaborate in lithium, sodium, and calcium zinc borate glasses, as well as diborate in potassium and rubidium containing ones. Both groups were simultaneously found in Li2O-PbO-B2O3. Alkali ions are mainly responsible for the formation of B4-units and metaborate. Zinc ions favorably compensate non-bridging oxygen and partially form ZnO4. With decreasing N4 and field strength of the alkali ions the atomic packing density, glass transition temper ature and Young’s Modulus also decrease. The coefficient of thermal expansion increases with decreasing N4.
During resistance spot welding of zinc-coated advanced high-strength steels (AHSSs) for automotive production, liquid metal embrittlement (LME) cracking may occur in the event of a combination of various unfavorable influences. In this study, the interactions of different welding current levels and weld times on the tendency for LME cracking in third-generation AHSSs were investigated. LME manifested itself as high penetration cracks around the circumference of the spot welds for welding currents closely below the expulsion limit. At the same time, the observed tendency for LME cracking showed no direct correlation with the overall heat input of the investigated welding processes. To identify a reliable indicator of the tendency for LME cracking, the local strain rate at the origin of the observed cracks was analyzed over the course of the welding process via finite element simulation. While the local strain rate showed a good correlation with the process-specific LME cracking tendency, it was difficult to interpret due to its discontinuous course. Therefore, based on the experimental measurement of electrode displacement during welding, electrode indentation velocity was proposed as a descriptive indicator for quantifying cracking tendency.
BAM is currently building up a platform of novel nanoRMs relying on iron oxide nanoparticles of different shape, size and surface chemistry. Iron oxide was chosen as a core material because of its relevance to the material and life sciences.
As a first candidate of this series, we present cubic iron oxide nanoparticles with a nominal edge length of 8 nm. These particles were synthesized by thermal decomposition of iron oleate in high boiling organic solvents adapting well-known literature procedures. After dilution to a concentration suitable for electron microscopy (TEM and SEM) as well as for small-angle X-ray scattering (SAXS) measurements, the candidate nanoRM was bottled and assessed for homogeneity and stability by both methods following the guidelines of ISO 17034 and ISO Guide 35.
The particle sizes obtained by both STEM-in-SEM and TEM are in excellent agreement with a minimum Feret of 8.3 nm ± 0.7 nm. The aspect ratio (AR) of the iron oxide cubes were extracted from the images as the ratio of minimum Feret to Feret resulting in an AR of 1.18 for TEM to 1.25 for SEM. Alternatively, a rectangular bounding box was fitted originating from the minimum Feret and the longest distance through the particle in perpendicular direction. This led to AR values of 1.05 for TEM and 1.12 for SEM, respectively. The results confirm the almost ideal cubic shape.
In order to bridge the gap between lab-scale and industrial-scale production of graphene it is necessary to develop processes, equipment and measurement procedures to control the material features. One of the crucial reasons of graphene’s limited commercialization is the lack of standard procedures to properly characterize and define the material chemical and structural properties down to the nanometer level. This leads to many issues regarding material synthesis repeatability, inappropriateness choice of measurands and measurement reproducibility which heavily affect the consistency of the material performance.
In our study, a comparative analysis is performed on two different series (G5 and G6) of industrial graphene powders, each series produced with four types of functionalization: raw graphene, oxygen-functionalized, nitrogen-functionalized and fluorine-functionalized. All the 8 sample variants were analyzed from a chemical and morphological point of view in the form of powders prepared as slightly pressed in metallic sample holders.
The results of the comparative chemical analyses XPS and EDS show a good agreement in the concentration values for all the elements present in the samples, despite the different analysis volumes addressed by the two techniques. For this reason, the samples can be considered homogeneous in both lateral and vertical direction.
A clear influence of the morphology on the composition is evident. Therefore, such correlative measurements of morphology and composition are necessary for a comprehensive characterization of industrial graphene flakes.
The Directed Energy Deposition process is used in a wide range of applications including the repair, coating or modification of existing structures and the additive manufacturing of individual parts. As the process is frequently applied in the aerospace industry, the requirements for quality assurance are extremely high. Therefore, more and more sensor systems are being implemented for process monitoring. To evaluate the generated data, suitable methods must be developed. A solution, in this context, was the application of artificial neural networks (ANNs). This article demonstrates how measurement data can be used as input data for ANNs. The measurement data were generated using a pyrometer, an emission spectrometer, a camera (Charge-Coupled Device) and a laser scanner. First, a concept for the extraction of relevant features from dynamic measurement data series was presented. The developed method was then applied to generate a data set for the quality prediction of various geometries, including weld beads, coatings and cubes. The results were compared to ANNs trained with process parameters such as laser power, scan speed and powder mass flow. It was shown that the use of measurement data provides additional value. Neural networks trained with measurement data achieve significantly higher prediction accuracy, especially for more complex geometries.
Duplex stainless steels combine the positive properties of its two phases, austenite and ferrite. Due to its good corrosion resistance, high tensile strength and good ductility it has multiple applications. But laser beam welding of duplex steels changes the balanced phase distribution in favor of ferrite. This results in a higher vulnerability to corrosion and a lower ductility. In this study different powder combinations consisting of duplex and nickel for coating layers by laser metal deposition are investigated. Afterwards laser tracks are welded, and the temperature cycles measured. The ferrite content of the tracks are analyzed by feritscope, metallographic analysis and Electron Backscatter Diffraction. The goal is the development of a powder mixture allowing for a duplex microstructure in a two-step process, where firstly the edges of the weld partners are coated with the powder mixture by LMD and secondly those edges are laser beam welded. The powder mixture identified by the pretests is tested in the two-step process and analyzed by metallographic analysis, energy dispersive X-ray spectroscopy and Vickers hardness tests. The resulting weld seams show a balanced duplex microstructure with a homogenous nickel distribution and a hardness of the weld seam similar to the base material.
Medium and High Entropy Alloys (MEA/HEA) are recently developed material classes, providing manifold applications, e.g., due to extraordinary structural properties. In that connection, the machinability as important issue for the processing of these materials was not in the scientific focus. This study focusses on experimental analysis of milling process conditions including ultrasonic assisted milling (USAM) and their effects on the resulting surface integrity of equiatomic CoCrFeNi-MEA specimens. For that reason, milling parameters (cutting speed, feed per cutting edge) were systematically varied for both conventional milling and USAM. The surface integrity was analyzed in terms of topography, defects, and residual stresses. Especially USAM leads to a decrease of occurring cutting forces and, hence, to an improvement of the surface integrity. Beneficial effects were observed in terms of lower tensile residual stresses at high cutting speed and feed per cutting edge.