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Copper sulfide shows some unique physico-chemical properties that make it appealing as a cathode active material (CAM) for solid-state batteries (SSBs). The most peculiar feature of the electrode reaction is the reversible formation of μm-sized Cu crystals during cycling, despite its large theoretical volume change (75%). Here, the dynamic microstructural evolution of CuS cathodes in SSBs is studied using in situ synchrotron X-ray tomography. The formation of μm-sized Cu within the CAM particles can be clearly followed. This process is accompanied by crack formation that can be prevented by increasing the stack pressure from 26 to 40 MPa. Both the Cu inclusions and cracks show a preferential orientation perpendicular to the cell stack pressure, which can be a result of a z-oriented expansion of the CAM particles during lithiation. In addition, cycling leads to a z-oriented reversible displacement of the cathode
pellet, which is linked to the plating/stripping of the Li counter electrode. The pronounced structural changes cause pressure changes of up to 6 MPa within the cell, as determined by operando stack pressure measurements. Reasons for the reversibility of the electrode reaction are discussed and are attributed to the favorable combination of soft materials.
Grain boundaries (GBs) are planar lattice defects that govern the properties of many types of polycrystalline materials. Hence, their structures have been investigated in great detail. However, much less is known about their chemical features, owing to the experimental difficulties to probe these features at the atomic length scale inside bulk material specimens. Atom probe tomography (APT) is a tool capable of accomplishing this task, with an ability to quantify chemical characteristics at near-atomic scale. Using APT data sets, we present here a machine-learning-based approach for the automated quantification of chemical features of GBs. We trained a convolutional neural network (CNN) using twenty thousand synthesized images of grain interiors, GBs, or triple junctions. Such a trained CNN automatically detects the locations of GBs from APT data. Those GBs are then subjected to compositional mapping and analysis, including revealing their in-plane chemical decoration patterns. We applied this approach to experimentally obtained APT data sets pertaining to three case studies, namely, Ni-P, Pt-Au, and Al-Zn-Mg-Cu alloys. In the first case, we extracted GB specific segregation features as a function of misorientation and coincidence site lattice character. Secondly, we revealed interfacial excesses and in-plane chemical features that could not have been found by standard compositional analyses. Lastly, we tracked the temporal evolution of chemical decoration from early-stage solute GB segregation in the dilute limit to interfacial phase separation, characterized by the evolution of complex composition patterns. This machine-learning-based approach provides quantitative, unbiased, and automated access to GB chemical analyses, serving as an enabling tool for new discoveries related to interface thermodynamics, kinetics, and the associated chemistry-structure-property relations.
Using the creation relaxation algorithm developed for the atomistic modeling of the high-dose irradiation limit of crystalline systems, we explore the limits of the structural rejuvenation of a highly excited model binary glass. This high-energy athermal amorphous structure exhibits a direct transition to homogeneous plastic flow and a microstructure that is largely insensitive to this flow, being characterized by a porous system-spanning network of minimally frustrated structural motifs. The observed homogeneous plasticity is mediated by the same string-like structural excitations, which mediate structural relaxation and microplasticity at finite temperature in more relaxed structures. This highly rejuvenated structural asymptote is not far from the structural state of regions, which have experienced athermal shear localization in more relaxed samples, suggesting an optimally rejuvenated glassy structure will always be limited by that produced by shear localization.
Plants and microorganisms, besides the climate, drive nitrogen (N) cycling in ecosystems. Our objective was to investigate N losses and N acquisition strategies along a unique ecosystem-sequence (ecosequence) ranging from arid shrubland through Mediterranean woodland to temperate rainforest. These ecosystems differ in mean annual precipitation, mean annual temperate, and vegetation cover, but developed on similar granitoid soil parent material, were addressed using a combination of molecular biology and soil biogeochemical tools. Soil N and carbon (C) contents, δ15N signatures, activities of N acquiring extracellular enzymes as well as the abundance of soil bacteria and fungi, and diazotrophs in bulk topsoil and rhizosphere were determined. Relative fungal abundance in the rhizosphere was higher under woodland and forest than under shrubland. This indicates toward plants' higher C investment into fungi in the Mediterranean and temperate rainforest sites than in the arid site. Fungi are likely to decompose lignified forest litter for efficient recycling of litter-derived N and further nutrients. Rhizosphere—a hotspot for the N fixation—was enriched in diazotrophs (factor 8 to 16 in comparison to bulk topsoil) emphasizing the general importance of root/microbe association in N cycle. These results show that the temperate rainforest is an N acquiring ecosystem, whereas N in the arid shrubland is strongly recycled. Simultaneously, the strongest 15N enrichment with decreasing N content with depth was detected in the Mediterranean woodland, indicating that N mineralization and loss is highest (and likely the fastest) in the woodland across the continental transect. Higher relative aminopeptidase activities in the woodland than in the forest enabled a fast N mineralization. Relative aminopeptidase activities were highest in the arid shrubland. The highest absolute chitinase activities were observed in the forest. This likely demonstrates that (a) plants and microorganisms in the arid shrubland invest largely into mobilization and reutilization of organically bound N by exoenzymes, and (b) that the ecosystem N nutrition shifts from a peptide-based N in the arid shrubland to a peptide- and chitin-based N nutrition in the temperate rainforest, where the high N demand is complemented by intensive N fixation in the rhizosphere.
Storage is still limiting the implementation of hydrogen as an energy carrier to integrate the intermittent operation of renewable energy sources. Among different solutions to the currently used compressed or liquified hydrogen systems, physical adsorption at cryogenic temperature in porous materials is an attractive alternative due to its fast and reversible operation and the resulting reduction in storage pressure. The feasibility of cryoadsorption for hydrogen storage depends mainly on the performance of the used materials for the specific application, where metal-organic frameworks or MOFs are remarkable candidates. In this work, gravimetric and volumetric hydrogen uptakes at 77 K and up to 100 bar of commercially available MOFs were measured since these materials are made from relatively cheap and accessible building blocks. These materials also show relatively high porous properties and are currently near to large-scale production. The measuring device was calibrated at different room temperatures to calculate an average correction factor and standard deviation so that the correction deviation is included in the measurement error for better comparability with different measurements. The influence of measurement conditions was also studied, concluding that the available adsorbing area of material and the occupied volume of the sample are the most critical factors for a reproducible measurement, apart from the samples’ preparation before measurement. Finally, the actual volumetric storage density of the used powders was calculated by directly measuring their volume in the analysis cell, comparing that value with the maximum volumetric uptake considering the measured density of crystals. From this selection of commercial MOFs, the materials HKUST-1, PCN-250(Fe), MOF-177, and MOF-5 show true potential to fulfill a volumetric requirement of 40 g·L−1 on a material basis for hydrogen storage systems without further packing of the powders.
he mutual influence of F and OH groups in neighboring sites in topaz (Al2SiO4(F,OH)2) was investigated using magic angle spinning nuclear magnetic resonance (MAS NMR) and Raman spectroscopy. The splitting of 19F and 1H NMR signals, as well as the OH Raman band, provides evidence for hydrogen bond formation within the crystal structure. Depending on whether a given OH group has another OH group or fluoride as its neighbor, two different hydrogen bond constellations may form: either OH···O···HO or F···H···O. The proton accepting oxygen was determined to be part of the SiO4 tetrahedron using 29Si MAS NMR. Comparison of the MAS NMR data between an OH-bearing and an OH-free topaz sample confirms that the 19F signal at −130 ppm stems from F− ions that take part in H···F bonds with a distance of ∼ 2.4 Å, whereas the main signal at −135 ppm belongs to fluoride ions with no immediate OH group neighbors. The Raman OH sub-band at 3644 cm−1 stems from OH groups neighboring other OH groups, whereas the sub-band at 3650 cm−1 stems from OH groups with fluoride neighbors, which are affected by H···F bridging. The integrated intensities of these two sub-bands do not conform to the expected ratios based on probabilistic calculations from the total OH concentration. This can be explained by a difference in the polarizability of the OH bond between the different hydrogen bond constellations or partial order or unmixing of F and OH, or a combination of both. This has implications for the quantitative interpretation of Raman data on OH bonds in general and their potential use as a probe for structural (dis-)order. No indication of tetrahedrally coordinated Al was found with 27Al MAS NMR, suggesting that the investigated samples likely have nearly ideal Al/Si ratios, making them potentially useful as high-density electron microprobe reference materials for Al and Si, as well as for F.
The superior properties of high-entropy multi-functional materials are strongly connected with their atomic heterogeneity through many different local atomic interactions. The detailed element-specific studies on a local scale can provide insight into the primary arrangements of atoms in multicomponent systems and benefit to unravel the role of individual components in certain macroscopic properties of complex compounds. Herein, multi-edge X-ray absorption spectroscopy combined with reverse Monte Carlo simulations was used to explore a homogeneity of the local crystallographic ordering and specific structure relaxations of each constituent in the equiatomic single-phase facecentered cubic CrMnFeCoNi high-entropy alloy at room temperature. Within the considered fitting approach, all five elements of the alloy were found to be distributed at the nodes of the fcc lattice without any signatures of the additional phases at the atomic scale and exhibit very close statistically averaged interatomic distances (2.54 – 2.55 Å) with their nearest-neighbors. Enlarged structural displacements were found solely for Cr atoms. The macroscopic magnetic properties probed by conventional magnetometry demonstrate no opening of the hysteresis loops at 5 K and illustrate a complex character of the long-range magnetic order after field-assisted cooling in ± 5 T. The observed magnetic behavior is assigned to effects related to structural relaxations of Cr. Besides, the advantages and limitations of the reverse Monte Carlo approach to studies of multicomponent systems like high-entropy alloys are highlighted.
Tungsten-tungsten carbide (W/W2C) composites are considered as possible structural materials for future nuclear fusion reactors. Here, we report on the effect of helium (He) implantation on microstructure evolution of polycrystalline W/W2C composite consolidated by field-assisted sintering technique (FAST), homogenously implanted at room temperature with 1 MeV 4He+ ions at the fluence of 8 × 1016 ions cm−2 and annealed at 1873 K for 20 minutes. Samples were analysed by scanning and transmission electron microscopy to study the presence and size of He bubbles. Monomodal He bubbles in W (30-80 nm) are limited to point defects and grain boundaries, with a considerable void denuded zone (150 nm). Bubbles do not form in W2C, but at the W|W2C interface and are considerably larger (200-400 nm). The experimental observations on He behaviour and migration in W and W2C were assessed by density functional theory (DFT) calculations, suggesting He migration and accumulation in the composite are determined by the effective He-He binding in clusters, which will give rise to decohesion. In the presence of He clusters, the decohesion of bulk W into free surfaces is energetically highly favourable but not sufficient in the W2C; hence bubbles are only observed in W grains and interfaces and not within bulk W2C.
Fast and accurate determination of the protein content of a sample is an important and non-trivial task of many biochemical, biomedical, food chemical, pharmaceutical, and environmental research activities. Different methods of total protein determination are used for a wide range of proteins with highly variable properties in complex matrices. These methods usually work reasonably well for proteins under controlled conditions, but the results for non-standard and complex samples are often questionable. Here, we compare new and well-established methods, including traditional amino acid analysis (AAA), aromatic amino acid analysis (AAAA) based on the amino acids phenylalanine and tyrosine, reversed-phase liquid chromatography of intact proteins with UV absorbance measurements at 220 and 280 nm (LC-220, LC-280), and colorimetric assays like Coomassie Blue G-250 dye-binding assay (Bradford) and bicinchoninic acid (BCA) assay. We investigated different samples, including proteins with challenging properties, chemical modifications, mixtures, and complex matrices like air particulate matter and pollen extracts. All methods yielded accurate and precise results for the protein and matrix used for calibration. AAA, AAAA with fluorescence detection, and the LC-220 method yielded robust results even under more challenging conditions (variable analytes and matrices). These methods turned out to be well-suited for reliable determination of the protein content in a wide range of samples, such as air particulate matter and pollen.
Detailed microstructural characterization of the AlMo0.5NbTa0.5TiZr refractory high entropy superalloy in the as-cast state is reported for first time and compared with the state annealed at 1400 oC for 24 h. The former shows a dendritic structure, with a mixture of A2/B2 phases < 20 nm in both the dendritic and interdendritic regions. A mostly amorphous phase, rich in Al and Zr, is found within the interdendritic region. The annealed state reproduced the combination of A2/B2/Al-Zr-rich phases reported previously. Calculations from two relevant ThermoCalc databases were compared with the experimental results. Equilibrium calculations were compared with results for the annealed alloy, whereas solidification paths calculated using Scheil-Gulliver model were used for comparison with the as-cast alloy. A previously hypothesized spinodal decomposition during cooling as the mechanism responsible for the patterned A2/B2 microstructure is confirmed via the CALPHAD calculations, pointing to its use as an efficient design tool for such alloys. Finally, the comparison between the experimental and computational findings allowed better understanding the solidification path and equilibrium stability of this alloy, giving a base to make better decisions on the field of new refractory superalloy design.
Through the application of scientific methods of analysis to a corpus of medieval manuscripts found in the Cairo Genizah, this work aims to gain a better understanding of the writing materials used by Jewish communities at that time, shedding new light not only on the production of manuscripts in the Middle Ages, but also on the life of those Jewish communities.
The development of earth-abundant catalysts for selective electrochemical CO2 conversion is a central challenge. Cu-Sn bimetallic catalysts can yield selective CO2 reduction toward either CO or formate. This study presents oxide-derived Cu-Sn catalysts tunable for either product and seeks to understand the synergetic effects between Cu and Sn causing these selectivity trends. The materials undergo significant transformations under CO2 reduction conditions, and their dynamic bulk and surface structures are revealed by correlating observations from multiple methods—X-ray absorption spectroscopy for in situ study, and quasi in situ X-ray photoelectron spectroscopy for surface sensitivity. For both types of catalysts, Cu transforms to metallic Cu0 under reaction conditions. However, the Sn speciation and content differ significantly between the catalyst types: the CO-selective catalysts exhibit a surface Sn content of 13 at. % predominantly present as oxidized Sn, while the formate-selective catalysts display an Sn content of ≈70 at. % consisting of both metallic Sn0 and Sn oxide species. Density functional theory simulations suggest that Snδ+ sites weaken CO adsorption, thereby enhancing CO selectivity, while Sn0 sites hinder H adsorption and promote formate production. This study reveals the complex dependence of catalyst structure, composition, and speciation with electrochemical bias in bimetallic Cu catalysts.
An immobilization of graphene oxide (GO) into a matrix of polyvinyl formaldehyde (PVF) foam as an eco-friendly, low cost, superior, and easily recovered sorbent of Pb ions from an aqueous solution is described. The relationships between the structure and electrochemical properties of PVF/GO composite with implanted Pb ions are discussed for the first time. The number of alcohol groups decreased by 41% and 63% for PVF/GO and the PVF/GO/Pb composite, respectively, compared to pure PVF. This means that chemical bonds are formed between the Pb ions and the PVF/GO composite based on the OH groups. This bond formation causes an increase in the Tg values attributed to the formation of a strong surface complexation between adjacent layers of PVF/GO composite. The conductivity increases by about 2.8 orders of magnitude compared to the values of the PVF/GO/Pb composite compared to the PVF. This means the presence of Pb ions is the main factor for enhancing the conductivity where the conduction mechanism is changed from ionic for PVF to electronic conduction for PVF/GO and PVF/GO/Pb.
The discussed comparative analyses of Roman Imperial pigment balls and fragmentary murals unearthed in the ancient cities of Aventicum and Augusta Raurica (Switzerland) by means of Raman microspectroscopy pertain to a predecessor study on trace compounds in Early Medieval Egyptian blue (St. Peter, Gratsch, South Tyrol, Northern Italy). The plethora of newly detected associated minerals of the raw materials surviving the synthesis procedure validate the use of quartz sand matching the composition of sediments transported by the Volturno river into the Gulf of Gaeta (Campania, Southern Italy) with a roasted sulphidic copper ore and a mixed-alkaline plant ash as fluxing agent. Thus, the results corroborate a monopolised pigment production site located in the northern Phlegrean Fields persisting over the first centuries A.D., this in line with statements of the antique Roman writers Vitruvius and Pliny the Elder and recent archaeological evidences. Beyond that, Raman spectra reveal through gradual peak shifts and changes of band width locally divergent process conditions and compositional inhomogeneities provoking crystal lattice disorder in the chromophoric cuprorivaite as well as the formation of a copper-bearing green glass phase, the latter probably in dependency of the concentration of alkali flux, notwithstanding that otherwise solid-state reactions predominate the synthesis.
The roles extracellular polymeric substances (EPS) play in mineral attachment and weathering were studied using genetically modified biofilms of the rock-inhabiting fungus Knufia petricola strain A95. Mutants deficient in melanin and/or carotenoid synthesis were grown as air-exposed biofilms. Extracted EPS were quantified and characterised using a combination of analytical techniques. The absence of melanin affected the quantity and composition of the produced EPS: mutants no longer able to form melanin synthesised more EPS containing fewer pullulan-related glycosidic linkages. Moreover, the melanin-producing strains attached more strongly to the mineral olivine and dissolved it at a higher rate. We hypothesise that the pullulan-related linkages, with their known adhesion functionality, enable fungal attachment and weathering. The released phenolic intermediates of melanin synthesis in the Δsdh1 mutant might play a role similar to Fe-chelating siderophores, driving olivine dissolution even further. These data demonstrate the need for careful compositional and quantitative analyses of biofilm-created microenvironments.
Polymers of intrinsic microporosity (PIMs) are promising candidates for the active layer in gas separation membranes due to their high permeability and reasonable permselectivity. These appealing properties originate from a microporous structure as a result of inefficient segment packing in the condensed state due to a combination of a ladder-like rigid backbone and sites of contortion. However, this class of polymers suffers from a significant decrease in the permeability with time due to physical aging, whereby typically, the permselectivity increases. The initial microporous structures approach a denser state via local rearrangements, leading to the reduction of the permeability. Hence, a detailed characterization of the molecular mobility in such materials can provide valuable information on physical aging. In this work, the dielectric behavior of PIM-1 films and their behavior upon heating (aging) were revisited by isothermal frequency scans during different heating/cooling cycles over a broad temperature range between 133 and 523 K (−140 to 250 °C). In addition, the obtained results were compared with data of samples that were annealed at ambient temperatures over different time scales. Multiple dielectric processes were observed: several relaxation processes due to local fluctuations and a Maxwell−Wagner−Sillars polarization effect related to the microporosity. The temperature dependence of the rates of all processes follows the Arrhenius law where the estimated activation energy depends on the nature of the process. The influence of the thermal history (aging) on the processes is discussed in detail.
A global transition towards more sustainable, affordable and reliable energy systems is being stimulated by the Paris Agreement and the United Nation's 2030 Agenda for Sustainable Development. This poses a challenge for the corrosion industry, as building climate‐resilient energy systems and infrastructures brings with it a long‐term direction, so as a result the long‐term behaviour of structural materials (mainly metals and alloys) becomes a major prospect. With this in mind “Corrosion Challenges Towards a Sustainable Society” presents a series of cases showing the importance of corrosion protection of metals and alloys in the development of energy production to further understand the science of corrosion, and bring the need for research and the consequences of corrosion into public and political focus. This includes emphasis on the limitation of greenhouse gas emissions, on the lifetime of infrastructures, implants, cultural heritage artefacts, and a variety of other topics.
The elastic constants are the most basic mechanical properties of a material and are needed for any structural analysis of a component. For example, they have a major influence on the eigenfrequencies of vibrating parts. Single crystals of Ni-base superalloys are strongly anisotropic, which means that the observed properties are orientation dependent. Tensor algebra is then required to mathematically formulate the elastic properties and their relations to the crystal orientation. Hence, this chapter first summarizes some basic definitions and calculation rules for Rotation matrices, including the definition of the Euler angles, which are most commonly used to define the relative orientations of the crystal and the component. Parts of this chapter closely follow the lines of the excellent exposition of the topic by Olschewski.
Water-stable metal−organic frameworks (MOFs) with proton-conducting behavior have attracted great attention as promising materials for proton-exchange membrane fuel cells. Herein, we report the mechanochemical gram-scale synthesis of three new mixed-ligand phosphonate-based MOFs, {Co(H2PhDPA)(4,4′-bipy)H2O)·2H2O}n (BAM-1), {Fe(H2PhDPA)(4,4′-bipy) (H2O)·2H2O}n (BAM-2), and {Cu(H2PhDPA)(dpe)2(H2O)2·2H2O}n (BAM-3) [where H2PhDPA = phenylene diphosphonate, 4,4′-bipy = 4,4′-bipyridine, and dpe = 1,2-di(4-pyridyl)ethylene]. Single-crystal X-ray diffraction measurements revealed that BAM-1 and BAM-2 are isostructural and possess a three-dimensional (3D) network structure comprising one-dimensional (1D) channels filled with guest water molecules. Instead, BAM-3 displays a 1D network structure extended into a 3D supramolecular structure through hydrogenbonding and π−π interactions. In all three structures, guest water molecules are interconnected with the uncoordinated acidic hydroxyl groups of the phosphonate moieties and coordinated water molecules by means of extended hydrogen-bonding interactions. BAM-1 and BAM-2 showed a gradual increase in proton conductivity with increasing temperature and reached 4.9 × 10−5 and 4.4 × 10−5 S cm−1 at 90 °C and 98% relative humidity (RH). The highest proton conductivity recorded for BAM-3 was 1.4 × 10−5 S cm−1 at 50 °C and 98% RH. Upon further heating, BAM-3 undergoes dehydration followed by a phase transition to another crystalline form which largely affects its performance. All compounds exhibited a proton hopping (Grotthuss model) mechanism, as suggested by their low activation energy.
Lithium and boron are trace components of magmas, released during exsolution of a gas phase during volcanic activity. In this study, we determine the difusivity and isotopic fractionation of Li and B in hydrous silicate melts. Two glasses were synthesized with the same rhyolitic composition (4.2 wt% water), having diferent Li and B contents; these were studied in difusion-couple experiments that were performed using an internally heated pressure vessel, operated at 300 MPa in the temperature range 700–1250 °C for durations from 0 s to 24 h. From this we determined activation energies for Li and B difusion of 57±4 kJ/mol and 152±15 kJ/mol with pre-exponential factors of 1.53 × 10–7 m2/s and 3.80× 10–8 m2 /s, respectively. Lithium isotopic fractionation during difusion gave β values between 0.15 and 0.20, whereas B showed no clear isotopic fractionation. Our Li difusivities and isotopic fractionation results difer somewhat from earlier published values, but overall confrm that Li difusivity increases with water content. Our results on B difusion show that similarly to Li, B mobility increases in the presence of water. By applying the Eyring relation, we confrm that B difusivity is limited by viscous fow in silicate melts. Our results on Li and B difusion present a new tool for understanding degassing-related processes, ofering a potential geospeedometer to measure volcanic ascent rates.
The development of methodologies to sense glyphosate has gained momentum due to its toxicological and ecotoxicological effects. In this work, a red-emitting and polymerizable guanidinium benzoxadiazole probe was developed for the fluorescence detection of glyphosate. The interaction of the fluorescent probe and the tetrabutylammonium salt of glyphosate was studied via UV/vis absorption and fluorescence spectroscopy in chloroform and acetonitrile. The selective recognition of glyphosate was achieved by preparing molecularly imprinted polymers, able to discriminate against other common herbicides such as 2,4-dichlorophenoxyacetic acid (2,4-D) and 3,6-dichloro-2-methoxybenzoic acid (dicamba), as thin layers on submicron silica particles. The limits of detection of 4.8 µM and 0.6 µM were obtained for the sensing of glyphosate in chloroform and acetonitrile, respectively. The reported system shows promise for future application in the sensing of glyphosate through further optimization of the dye and the implementation of a biphasic assay with water/organic solvent mixtures for sensing in aqueous environmental samples.
Kunststoff- und Kunststoffrasenflächen kommt bei intensiv genutzten Flächen als Allwetterbeläge eine große Bedeutung zu. Sie leisten einen wichtigen Beitrag zur Absicherung eines ganzjähriger Sportangebote.
Gerade Kunststoffrasen ist aber in den letzten Jahren häufig in die Kritik geraten, insbesondere durch gefährliche Inhaltsstoffe und andere negative Einflüsse auf die Umwelt. Dies hat bei Bauherren zu einer Verunsicherung geführt und Fragen aufgeworfen, die erst teilweise beantwortet sind. Die Diskussionen rund um diesen Allwetterbelag haben bereits dazu geführt, dass von Seiten der Industrie viel verändert wurde und neue innovative Lösungen gefunden werden.
Der Fachbericht stellt eine Handreichung für Fachleute und interessierte Laien dar, um mehr Klarheit besonders hinsichtlich der Umweltanforderungen zu erzielen.
Antimicrobial resistance (AMR) is a global health problem with the environment being an important compartment for the evolution and transmission of AMR. Previous studies showed that de-novo mutagenesis and horizontal gene transfer (HGT) by conjugation or transformation – important processes underlying resistance evolution and spread - are affected by antibiotics, metals and pesticides. However, natural microbial communities are also frequently exposed to biocides used as material preservatives, but it is unknown if these substances induce mutagenesis and HGT. Here, we show that active substances used in material preservatives can increase rates of mutation and conjugation in a species- and substance-dependent manner, while rates of transformation are not increased. The bisbiguanide chlorhexidine digluconate, the quaternary ammonium compound didecyldimethylammonium chloride, the metal copper, the pyrethroid-insecticide permethrin, and the azole-fungicide propiconazole increase mutation rates in Escherichia coli, whereas no increases were identified for Bacillus subtilis and Acinetobacter baylyi.
Benzalkonium chloride, chlorhexidine and permethrin increased conjugation in E. coli. Moreover, our results show a connection between the RpoS-mediated general stress and the RecA-linked SOS response with increased rates of mutation and conjugation, but not for all biocides. Taken together, our data show the importance of assessing the contribution of material preservatives on AMR evolution and spread.
Es werden Methoden zur sicherheitstechnischen Bewertung des mechanischen Verhaltens von Brennstabhüllrohren entwickelt, um sprödes Versagen in Belastungsszenarien nach längerfristiger trockener Zwischenlagerung zu verhindern. Unbestrahlte Brennstabhüllrohrsegmente aus der Zirkoniumlegierung ZIRLO® wurden hydriert und thermomechanischen Behandlungen unterzogen, um Hüllrohrmaterial durch Ausscheidung radialer Hydride zu verspröden. Die Proben mit radialen Hydriden wurden im Ring Compression Test (RCT) bei Raumtemperatur untersucht. Bereits bei kleinen Probenverformungen wurden abrupte Kraftabfälle mit instabiler Rissausbreitung durch das Netzwerk radialer Hydride beobachtet. Die Risslängen erreichten in einigen Fällen bis zu 90 % der Wanddicke. Der mikromechanische Versagensmechanismus ist Quasi-Spaltbruch in den Hydriden und Porenbildung, -wachstum und -vereinigung in der Zirkoniummatrix an den duktilen Brücken zwischen benachbarten Hydriden. Es wurde ein Finite-Elemente-Modell des Ring Compression Tests erstellt, um das Versagensverhalten zirkoniumbasierter Legierungen mit radialen Hydriden im RCT zu analysieren. Die Fließkurve für das elastisch-plastische Materialmodell des Matrixmaterials wurde durch eine inverse Finite-Elemente-Analyse ermittelt. Kohäsivzonenmodelle wurden benutzt, um die plötzlichen Kraftabfälle zu reproduzieren. Es wurde ein mikromechanisches Modell mit statistisch generierten Matrix-Hydrid-Verteilungen entwickelt, das zwischen sprödem Versagen entlang der Hydride und duktilem Versagen der Zirkoniummatrix in der Kohäsivzone unterscheidet. Für das jeweilige Materialverhalten wird ein lokales zweiparametriges Versagenskriterium auf Grundlage der Kohäsionsfestigkeit und der Separationsenergie bei einer festgelegten Form des Kohäsivgesetzes vorgeschlagen. Geeignete Kohäsivparameter lassen sich mit einer inversen Finite-Elemente-Analyse des Versagensverhaltens von hydrierten Proben im Ring Compression Test bestimmen. In den Simulationen lag der Schwerpunkt auf dem ersten Kraftabfall. Die Berechnungsergebnisse stimmen gut mit den RCT-Ergebnissen überein. Es konnte gezeigt werden, dass die Rissinitiierung und -ausbreitung stark von der speziellen Anordnung der radialen Hydride und Matrixbrücken in der Bruchzone abhängt. Die numerische Modellbildung wurde an Versuchen mit bestrahlten Proben aus der Zirkoniumlegierung M5® validiert.
The large number of TEM investigations and the regular microstructure
of single-crystal nickel-base superalloys has boosted the development of a number of physically motivated constitutive laws. In contrast to the more phenomenological models discussed in the next chapter, these models use dislocation densities as internal variables. Obvious advantages are that the computed densities can be compared to TEM observations and the Deformation mechanisms can be easier translated into mathematical equations.
Considering the availability of serological and molecular biological methods, the bioassay has been paled into insignificance, although it is the only experimental method that can be used to demonstrate the infectivity of a virus. We compared goodness-of-fit and predictability power of five models for the quantification of tomato brown rugose fruit virus (ToBRFV) based on local lesion assays: the Kleczkowski model, Furumoto and Mickey models I and II, the Gokhale and Bald model (growth curve model), and the modified Poisson model. For this purpose, mechanical inoculations onto Nicotiana tabacum L. cv. Xanthi nc and N. glutionosa L. with defined virus concentrations were first performed with half-leaf randomization in a Latin square design. Subsequently, models were implemented using Python software and fitted to the number of local lesions. All models could fit to the data for quantifying ToBRFV based on local lesions, among which the modified Poisson model had the best prediction of virus concentration in spike samples based on local lesions, although data of individual indicator plants showed variations. More accurate modeling was obtained from the test plant N. glutinosa than from N. tabacum cv. Xanthi nc. The position of the half-leaves on the test plants had no significant effect on the number of local lesions.
Mechanically stable structures with interconnected hierarchical porosity combine the benefits of both small
and large pores, such as high surface area, pore volume, and good mass transport capabilities. Hence, lightweight micro-/meso-/macroporous monoliths are prepared from ordered mesoporous silica COK-12 by means of spark plasma sintering (SPS, S-sintering) and compared to conventionally (C-) sintered monoliths. A multi-scale model is developed to fit the small angle X-ray scattering data and obtain information on the hexagonal lattice parameters, pore sizes from the macro to the micro range, as well as the dimensions of the silica population. For both sintering techniques, the overall mesoporosity, hexagonal pore ordering, and amorphous character are preserved. The monoliths' porosity (77–49%), mesopore size (6.2–5.2 nm), pore volume (0.50–0.22 g cm-3
), and specific surface area (451–180 m2 g-1) decrease with increasing processing temperature and pressure. While the difference in porosity is enhanced, the
structural parameters between the C-and S-sintered monoliths are largely converging at 900 C, except for the mesopore size and lattice parameter, whose dimensions are more extensively preserved in the
S-sintered monoliths, however, coming along with larger deviations from the theoretical lattice. Their higher mechanical properties (biaxial strength up to 49 MPa, 724 MPa HV 9.807 N) at comparable porosities and ability to withstand ultrasonic treatment and dead-end filtration up to 7 bar allow S-sintered monoliths to reach a high permeance (2634 L m-2 h-1 bar-1), permeability (1.25 x 10^-14 m2), and ability to reduce the chemical oxygen demand by 90% during filtration of a surfactant-stabilized oil in water emulsion, while indicating reasonable resistance towards fouling.
In this work, molecular imprinting was combined with direct fluorescence detection of the pesticide Glyphosate (GPS). Firstly, the solubility of highly polar GPS in organic solvents was improved by using lipophilic tetrabutylammonium (TBA+) and tetrahexylammonium (THA+) counterions. Secondly, to achieve fluorescence detection, a fluorescent crosslinker containing urea-binding motifs was used as a probe for GPS-TBA and GPS-THA salts in chloroform, generating stable complexes through hydrogen bond formation. The GPS/fluorescent dye complexes were imprinted into 2–3 nm fluorescent molecularly imprinted polymer (MIP) shells on the surface of sub-micron silica particles using chloroform as porogen. Thus, the MIP binding behavior could be easily evaluated by fluorescence titrations in suspension to monitor the spectral changes upon addition of the GPS analytes. While MIPs prepared with GPS-TBA and GPS-THA both displayed satisfactory imprinting following titration with the corresponding analytes in chloroform, GPS-THA MIPs displayed better selectivity against competing molecules. Moreover, the THA+ counterion was found to be a more powerful phase transfer agent than TBA+ in a biphasic assay, enabling the direct fluorescence detection and quantification of GPS in water. A limit of detection of 1.45 μM and a linear range of 5–55 μM were obtained, which match well with WHO guidelines for the acceptable daily intake of GPS in water (5.32 μM).
One of the challenges of high-temperature polymer electrolyte membrane fuel cells is the poisoning of the Pt catalyst with H3PO4. H3PO4 is imbibed into the routinely used polybenzimidazole-based membranes, which facilitate proton conductivity in the temperature range of 120−200 °C. However, when leached out of the membrane by water produced during operation, H3PO4 adsorbs on the Pt catalyst surface, blocking the active sites and hindering the oxygen reduction reaction (ORR).
The reduction of H3PO4 to H3PO3, which occurs at the anode due to a combination of a low potential and the presence of gaseous H2, has been investigated as an additional important contributing factor to the observed poisoning effect. H3PO3 has an affinity toward adsorption on Pt surfaces even greater than that of H2PO4 −. In this work, we investigated the poisoning effect of both H3PO3 and H3PO4 using a half-cell setup with a gas diffusion electrode under ambient conditions. By means of in situ X-ray absorption spectroscopy, it was possible to follow the signature of different species adsorbed on the Pt nanoparticle catalyst (H, O, H2PO4 −, and H3PO3) at different potentials under ORR conditions in various electrolytes (HClO4, H3PO4, and H3PO3). It was found that H3PO3 adsorbs in a pyramidal configuration P(OH)3 through a Pt−P bond. The competition between H3PO4 and H3PO3 adsorption was studied, which should allow for a better understanding of the catalyst poisoning mechanism and thus assist in the development of strategies to mitigate this phenomenon in the future by minimizing H3PO3 generation by, for example, improved catalyst design or adapted operation conditions or changes in the electrolyte composition.
Black microcolonial fungi (Ascomycetes from Arthonio-, Dothideo-, and Eurotiomycetes) are stress-tolerant and persistent dwellers of natural and anthropogenic extreme habitats. They exhibit slow yeast-like or meristematic growth, do not form specialized reproduction structures and accumulate the black pigment 1,8-dihydroxynaphthalene (DHN) melanin in the multilayered cell walls. To understand how black fungi live, survive, colonize mineral substrates, and interact with phototrophs genetic methods are needed to test these functions and interactions. We chose the rock inhabitant Knufia petricola of the Chaetothyriales as a model for developing methods for genetic manipulation. Here, we report on the expansion of the genetic toolkit by more efficient multiplex CRISPR/Cas9 using a plasmid-based system for expression of Cas9 and multiple sgRNAs and the implementation of the three resistance selection markers genR (geneticin/nptII), baR (glufosinate/bar), and suR (chlorimuron ethyl/sur). The targeted integration of expression constructs by replacement of essential genes for pigment synthesis allows for an additional color screening of the transformants. The black-pink screening due to the elimination of pks1 (melanin) was applied for promoter studies using GFP fluorescence as reporter. The black-white screening due to the concurrent elimination of pks1 and phs1 (carotenoids) allows to identify transformants that contain the two expression constructs for co-localization or bimolecular fluorescence complementation (BiFC) studies. The co-localization and interaction of the two K. petricola White Collar orthologs were demonstrated. Two intergenic regions (igr1, igr2) were identified in which expression constructs can be inserted without causing obvious phenotypes. Plasmids of the pNXR-XXX series and new compatible entry plasmids were used for fast and easy generation of expression constructs and are suitable for a broad implementation in other fungi. This variety of genetic tools is opening a completely new perspective for mechanistic and very detailed study of expression, functioning and regulation of the genes/proteins encoded by the genomes of black fungi.
Im Verbundprojekt RUSEKU wurde die Probenahme von Wasserproben entscheidend weiterentwickelt. Wichtig ist hierbei zu gewährleisten, dass genügend Merkmalsträger in jeder Probe untersucht werden. Es muss daher eine für den Probenahmeort repräsentative Beprobung hinsichtlich des Wasservolumens in Abhängigkeit der Partikelanzahl gewährleistet sein.
Das Hauptaugenmerk lag im vorliegenden Projekt auf einer praxisnahen Beprobungsstrategie. Es wurden verschiedene Konzepte ausprobiert.
• Grundsätzlich hat sich gezeigt, dass eine Stichprobe eine Momentaufnahme des MP-Massengehaltes zeigt. Es wird eine hohe Statistik, also eine Vielzahl an Messungen am gleichen Probenahmeort, benötigt, um eine valide Aussage über den MP-Gehalt zu machen.
• Es zeigt sich, dass eine integrale Probenahme über mehrere Wochen mit dem SK routinemäßig möglich ist. Die erfassten MP-Massen sind reproduzierbar und robust.
• Die DFZ ist für Stichproben geeignet. Partikel < 50 µm werden eventuell unterschätzt
• Die fraktionierte Filtration kann für Stich- und Mischproben direkt im Feld genutzt werden. Fraktionen von 10 und 5 µm werden später im Labor Vakuum filtriert. Es erfolgt eine Fraktionierung der Probe mit Siebmaschenweiten von 1000, 500, 100, 50, 10 und 5 µm.
• Die fraktionierte Filtration kann auch anschließend an die Beprobung mit dem SK zur Anwendung kommen. Wird die mit dem SK gewonnene Wasserprobe fraktioniert filtriert, kann neben einem MP-Gesamtgehalt auch eine Einschätzung über die Partikelgrößen gewonnen werden.
• Für Wässer mit geringen Partikelzahlen wurde ein Messfiltertiegel entwickelt. Dieser hat eine Maschenweite von 6 µm. Seine Anwendung kann mögliche Verluste beim Transferieren vom Probenahmetool zum Messgefäß und mögliche Kontaminationen reduzieren.
Die Optimierung der Probenahmestrategie wurde durch Modellversuche und Simulationen unterstützt. Modellversuche zum Sinkverhalten und Simulationen von MP in realen Gewässern verdeutlichten das komplexe Verhalten der Partikel. Es konnte gezeigt werden, dass Partikel ab einer bestimmten Größe (und kleiner) bei genügend starker Turbulenz sich in der Wassersäule unabhängig von ihrer Dichte verhalten und so auch MP mit kleiner Dichte (z.B. PE) in der gesamten Wassersäule zu finden sind. Es konnte mit dem TEM die Existenz von NP gezeigt werden.
Ein wesentlicher Aspekt des RUSEKU Projektes war die Beprobung realer Kompartimente. Beprobt wurde neben Oberflächengewässern, das urbane Abwassersystem der Stadt Kaiserslautern, Waschmaschinenabwasser und Flaschenwasser.
• In Oberflächengewässern wurde hauptsächlich PE gefunden. Je nach Probe und Gewässer konnten auch PP, PS, PET, PA, SBR und Acrylate nachgewiesen werden.
• Im urbanen Abwassersystem der Stadt Kaiserslautern konnte an allen Probenahmestandorten MP nachgewiesen werden. Es wurde hauptsächlich PE, neben geringeren Mengen an PP, PS und SBR gefunden. Nach einem Regenereignis war der SBR Anteil deutlich erhöht.
• Die Beprobung eines realen Wäschepostens, bestehend aus T-Shirts und Hemden mit PA/CO oder PES/CO Mischgewebe, zeigte einen PA- und PES-Austrag im Waschwasser. Der überwiegende Teil der detektierten Fasern ist aber auf Baumwolle zurückzuführen. Reine gravimetrische Messungen zur Detektion von MP führen zu einer starken Überschätzung.
• In Flaschenwasser (PET-Flaschen) konnte MP detektiert werden. PET wurde nur im stillen Mineralwasser, nicht in Mineralwasser mit Kohlensäure gefunden werden. Teilweise wurde auch das MP-Material des Verschlusses im Wasser detektiert.
• Für Luftproben konnte ein Aufbau zur größenselektiven Beprobung getestet werden.
Neben der Probenahme hat das Projekt auch gezeigt, dass die TED-GC/MS geeignet für die MP-Detektion im Routinebetrieb ist. Die TED-GC/MS konnte weiter optimiert werden. Es wurden MP-Massen bestimmt.
Im Projekt wurden erste realitätsnahe Referenzmaterialien für die MP Detektion hergestellt. Die Herstellung von realitätsnahen Polymeren in ausreichender Homogenität und Menge hat sich als große Herausforderung herausgestellt.
Rock weathering is a key process in global elemental cycling. Life participates in this process with tangible consequences observed from the mineral interface to the planetary scale. Multiple lines of evidence show that microorganisms may play a pivotal—yet overlooked—role in weathering. This topic is reviewed here with an emphasis on the following questions that remain unanswered: What is the quantitative contribution of bacteria and fungi to weathering? What are the associated mechanisms and do they leave characteristic imprints on mineral surfaces or in the geological record? Does biogenic weathering fulfill an ecological function, or does it occur as a side effect of unrelated metabolic functions and biological processes? An overview of efforts to integrate the contribution of living organisms into reactive transport models is provided. We also highlight prospective opportunities to harness microbial weathering in order to support sustainable agroforestry practices and mining activities, soil remediation, and carbon sequestration.
Rapid solidification leads to unique microstructural features, where a less studied topic is the formation of various crystalline defects, including high dislocation densities, as well as gradients and splitting of the crystalline orientation. As these defects critically affect the material’s mechanical properties and performance features, it is important to understand the defect formation mechanisms, and how they depend on the solidification conditions and alloying. To illuminate the formation mechanisms of the rapid solidification induced crystalline defects, we conduct a multiscale modelling analysis consisting of bond-order potential-based molecular dynamics (MD), phase field crystal-based amplitude expansion simulations, and sequentially coupled phase field–crystal plasticity simulations. The resulting dislocation densities are quantified and compared to past experiments. The atomistic approaches (MD, PFC) can be used to calibrate continuum level crystal plasticity models, and the framework adds mechanistic insights arising from the multiscale analysis.
This article is part of the theme issue ‘Transport phenomena in complex systems (part 2)’.
Investigation of the Thermal Stability of Proteinase K for the Melt Processing of Poly(L‑lactide)
(2022)
The enzymatic degradation of aliphatic polyesters offers unique opportunities for various use cases in materials science. Although evidently desirable, the implementation of enzymes in technical applications of polyesters is generally challenging due to the thermal lability of enzymes. To prospectively overcome this intrinsic limitation, we here explored the thermal stability of proteinase K at conditions applicable for polymer melt processing, given that this hydrolytic enzyme is well established for its ability to degrade poly(L-lactide) (PLLA). Using assorted spectroscopic methods and enzymatic assays, we investigated the effects of high temperatures on the structure and specific activity of proteinase K. Whereas in solution, irreversible unfolding occurred at temperatures above 75−80 °C, in the dry, bulk state, proteinase K withstood prolonged incubation at elevated temperatures. Unexpectedly little activity loss occurred during incubation at up to 130 °C, and intermediate levels of catalytic activity were preserved at up to 150 °C. The resistance of bulk proteinase K to thermal treatment was slightly enhanced by absorption into polyacrylamide (PAM) particles. Under these conditions, after 5 min at a temperature of 200 °C, which is required for the melt processing of PLLA, proteinase K was not completely denatured but retained around 2% enzymatic activity. Our findings reveal that the thermal processing of proteinase K in the dry state is principally feasible, but equally, they also identify needs and prospects for improvement. The experimental pipeline we establish for proteinase K analysis stands to benefit efforts directed to this end. More broadly, our work sheds light on enzymatically degradable polymers and the thermal processing of enzymes, which are of increasing economical and societal relevance.
In this work, two X-ray refraction based imaging methods, namely, synchrotron X-ray refraction radiography (SXRR) and synchrotron X-ray refraction computed tomography (SXRCT), are applied to analyze quantitatively cracks and porosity in metallic materials.
SXRR and SXRCT make use of the refraction of X-rays at inner surfaces of the material, e.g., the surfaces of cracks and pores, for image contrast. Both methods are, therefore, sensitive to smaller defects than their absorption based counterparts X-ray radiography and computed tomography. They can detect defects of nanometric size.
So far the methods have been applied to the analysis of ceramic materials and fiber reinforced plastics. The analysis of metallic materials requires higher photon energies to achieve sufficient X-ray transmission due to their higher density. This causes smaller refraction angles and, thus, lower image contrast because the refraction index depends on the photon energy. Here, for the first time, a conclusive study is presented exploring the possibility to apply SXRR and SXRCT to metallic materials. It is shown that both methods can be optimized to overcome the reduced contrast due to smaller refraction angles. Hence, the only remaining limitation is the achievable X-ray Transmission which is common to all X-ray imaging methods. Further, a model for the quantitative analysis of the inner surfaces is presented and verified.
For this purpose four case studies are conducted each posing a specific challenge to the imaging task. Case study A investigates cracks in a coupon taken from an aluminum weld seam. This case study primarily serves to verify the model for quantitative analysis and prove the sensitivity to sub-resolution features. In case study B, the
damage evolution in an aluminum-based particle reinforced metal-matrix composite is analyzed. Here, the accuracy and repeatability of subsequent SXRR measurements is investigated showing that measurement errors of less than 3% can be achieved. Further, case study B marks the fist application of SXRR in combination with in-situ tensile loading. Case study C is out of the highly topical field of additive manufacturing. Here, porosity in additively manufactured Ti-Al6-V4 is analyzed with a special interest in the pore morphology. A classification scheme based on SXRR measurements is devised which allows to distinguish binding defects from keyhole pores even if the defects cannot be spatially resolved. In case study D, SXRCT is applied to the analysis of hydrogen assisted cracking in steel. Due to the high X-ray attenuation of steel a comparatively high photonenergy of 50 keV is required here. This causes increased noise and lower contrast in the data compared to the other case studies. However, despite the lower data quality a quantitative analysis of the occurance of cracks in dependence of hydrogen content and applied mechanical load is possible.
Advanced peptide-based nanomaterials composed of self-assembling peptides (SAPs) are of emerging interest in pharmaceutical and biomedical applications. The introduction of fluorine into peptides, in fact, offers unique opportunities to tune their biophysical properties and intermolecular interactions. In particular, the degree of fluorination plays a crucial role in peptide engineering as it can be used to control the characteristics of fluorine-specific interactions and, thus, peptide conformation and self-assembly. Here, we designed and explored a series of amphipathic peptides by incorporating the fluorinated amino acids (2S)-4-monofluoroethylglycine (MfeGly), (2S)-4,4-difluoroethylglycine (DfeGly) and (2S)-4,4,4-trifluoroethylglycine (TfeGly) as hydrophobic components. This approach enabled studying the impact of fluorination on secondary structure formation and peptide self-assembly on a systematic basis. We show that the interplay between polarity and hydrophobicity, both induced differentially by varying degrees of side chain fluorination, does affect peptide folding significantly. A greater degree of fluorination promotes peptide fibrillation and subsequent formation of physical hydrogels in physiological conditions. Molecular simulations revealed the key role played by electrostatically driven intra-chain and inter-chain contact pairs that are modulated by side chain fluorination and give insights into the different self-organization behaviour of selected peptides. Our study provides a systematic report about the distinct features of fluorinated oligomeric peptides with potential applications as peptide-based biomaterials.
Die Publikation befasst sich mit einer einzigartigen Sammlung mexikanischer und südamerikanischer Handschriften, die zu Beginn des 19. Jahrhunderts ins Leben gerufen wurde, als Alexander von Humboldt der Königlichen Bibliothek zu Berlin Fragmente indigener mexikanischer Bilderhandschriften aus dem 16. Jahrhundert schenkte. Sie sind heute auch unter der Bezeichnung Humboldt-Fragmente bekannt und stellen den bedeutendsten Teil der Sammlung dar, die im Laufe der Zeit durch den Ankauf verschiedener Arten von Handschriften aus Mittelamerika, vorwiegend in indigenen Sprachen und lateinischer Schrift, erweitert wurde.
In den zwei Jahren von April 2017 bis März 2019 verfolgten die Staatsbibliothek zu Berlin – Preußischer Kulturbesitz (SBB-PK) und die Bundesanstalt für Materialforschung und -prüfung (BAM) ein gemeinsames, von der Deutschen Forschungsgemeinschaft (DFG) großzügig gefördertes wissenschaftliches Projekt: Materialanalysen und kulturgeschichtliche Untersuchungen mexikanischer Handschriften aus der Kolonialzeit in Berlin und Krakau.
Die Hauptziele des Projekts bestanden darin, die Provenienz der Manuscripta americana zu ermitteln und, da sie einen hohen Grad an Fragmentierung aufweisen, festzustellen, wie sie untereinander und mit Objekten außerhalb der Sammlung in Beziehung stehen. Zu diesem Zweck wurden ethno-kulturhistorische und naturwissenschaftliche Methoden kombiniert. Dank einer guten Zusammenarbeit mit der Jagiellonen-Bibliothek konnten wir die Manuscripta americana sowohl in Berlin als auch in Krakau sehen und studieren und sie wissenschaftlich vermessen.
Die Klassik-Stiftung Weimar besitzt eine umfangreiche Sammlung niederländischer und flämischer Zeichnungen vom 15. bis 19. Jahrhundert. Im Rahmen des Forschungsprojektes »Kennerschaft heute« wurde der Bestand der über 1.500 Zeichnungen erstmals wissenschaftlich erschlossen. Das Handbuch führt anhand bedeutender Werkgruppen, darunter Zeichnungen von Lucas van Leyden, Dirck Vellert, Roelant Savery und Rembrandt, den Reichtum der Weimarer Sammlung vor Augen, die zum großen Teil auf die Sammelleidenschaft von Johann Wolfgang Goethe zurückgeht. Im Zentrum des Buches steht aber die Zusammenarbeit von traditioneller Stilkritik und naturwissenschaftlicher Materialanalyse. In zwölf Fallbeispielen wird die Notwendigkeit einer methodischen Neuausrichtung der Kennerschaft darlegt. Einen Schwerpunkt der Untersuchungen bildet hierbei das große Konvolut an Zeichnungen von Rembrandt und seinen Schülern, das erstmals systematisch auf die verwendeten Zeichenmaterialien und Papiere untersucht wird.
What is meant by ‘Micro Non-Destructive Testing and Evaluation’? This was the central subject of debate in this Special Issue.
At present, sub-millimeter-size components or even assemblies are pervading the industrial and scientific world. Classic examples are electronic devices and watches (as well as parts thereof), but recent examples encompass additively manufactured lattice structures, stents, or other microparts. Moreover, most assemblies contain micro-components. Testing such components or their miniaturized parts would fit well within the topic of micro non-destructive testing and evaluation.
In all cases, performance and integrity testing, quality control, and dimensional tolerances need to be measured at the sub-millimeter level (ideally with a spatial resolution of about a micron); most of the time, such features and components are embedded in much larger assemblies, which also need to be taken into account. The solution to this dilemma (i.e. measuring large parts with high resolution) depends on the part and on the problem under consideration.
Another possible definition of micro non-destructive testing and evaluation can relate to the characterization of micro-features (e.g., the microstructure) in much larger specimens, such as damage in concrete cores or porosity in additively manufactured components. A further aspect is the use of microscopic probes to evaluate macroscopic properties. This is the case, for instance but not at all exclusively, in the use of diffraction techniques to determine macroscopic stress.
The splits between testing and characterization at the micro-level (or of micro parts) from one side and handling of macroscopic assemblies on the other represent a great challenge for many fields of materials characterization. On top of that, including the use of microscopic methods to test integrity would add a further level of complexity.
Imaging, mechanical testing, non-destructive testing, measurement of properties, structural health monitoring, and dimensional metrology all need to be re-defined if we want to cope with the multi-faceted topic of micro non-destructive testing and evaluation.
The challenge has already been accepted by the scientific and engineering communities for a while but is still far from being universally tackled. This Special Issue yields an interesting answer to the questions posed above. It presents the progress made and the different aspects of the challenge as well as at indicates the paths for the future of NDT&E.