Wissenschaftliche Artikel der BAM
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High temperature oxidation of 9–12% Cr ferritic/martensitic steels under dual-environment conditions
(2017)
In normal operations, the opposite surfaces of the power plant components are exposed to two different environments, i.e. air/flue gas on the one side and steam on the other side. Exposure under such dual-environment can lead to accelerated corrosion of the components on the air side. The oxidation behaviour of ferritic/martensitic steel T92 was investigated under dual-environment in a specially designed test equipment. The samples were exposed to dry oxyfuel flue gas (CO2–27%N2–2%O2–1%SO2) on one side and to steam on the other side up to 1000 h at 650°C. The formation of oxide scales was characterised by optical microscopy and scanning electron microscopy with attached energy-dispersive spectroscopy. Oxidation rate of specimens under dual-Environment condition was almost three times higher than that in single-environment condition. This is explained based on hydrogen transport through the bulk alloy from the steam side to the flue gas side.
For the application of the time-temperature superposition principle a suitable relation is needed to describe the time-temperature shift factor α. Therefore, the Arrhenius equation is widely used due to its simple form and often leads to suitable results. Where, the Arrhenius equation presents a linear relation for the temperature-dependent shift factor in logarithmic scale ln(α) with the absolute inverse temperature (1/ϑ). However, in cases with a large temperature range which eventually include more complex reaction processes, the functional relation between ln(α) and (1/ϑ) is nonlinear in the ‘Arrhenius plot’. In those cases, the monotone change of the nonlinear range in the ‘Arrhenius plot’ can be interpreted as a transient range between two approximately linear or constant regions. An extended application of the modified Arrhenius equation from Nakamura (1989) is presented in this study for this transient range. The introduced method was applied to describe the time-temperature equivalence in the relaxation analysis of restoring seal force of metal seals, which are used in lid-systems of transport and interim storage casks for radioactive materials. But, the method is widely valid and can be used for different objectives which are characterized by thermorheologically simple behavior with nonlinear sensitivity to inverse temperature.
Corrosion fatigue (CF) of duplex stainless steel (DSS) X2CrNiMoN22-5-3 was investigated in in-situ geothermal conditions of the Northern German Basin (NGB). The influence of the load type on CF behavior of the alloy was examined by applying push/pull and rotating bending cyclic load to failure. The hour-glass shaped specimens with both polished and precisely turned surface finish were tested in corrosion chambers allowing for the permanent circulation of Northern German Basin electrolyte heated to 369 K. Additionally, the influence of a protective cathodic potential on the CF life expectancy was investigated by employing a potentiostat. The rotating bending cyclic load led to a higher CF life expectancy, which decreased with increasing duration of the experiment due to a higher deterioration rate of the material. The application of a cathodic potential caused a significant increase of the CF lifespan from 4.7 x 105 (open-circuit potential (OCP)) to 107 cycles (preset threshold cycle number) for the potential range from USHE = – 450 to – 900 mV. Microstructural analysis of the CF damage revealed horizontal grain attack within corrosion pit cavities, multiple fatigue cracks and preferable deterioration of the austenitic phase.
Cell-to-cell variation and specialization in sugar metabolism in clonal bacterial populations
(2017)
While we have good understanding of bacterial metabolism at the population level, we know little about the metabolic behavior of individual cells: do single cells in clonal populations sometimes specialize on different metabolic pathways? Such metabolic specialization could be driven by stochastic gene expression and could provide individual cells with growth benefits of specialization. We measured the degree of phenotypic specialization in two parallel metabolic pathways, the assimilation of glucose and arabinose. We grew Escherichia coli in chemostats, and used isotope-labeled sugars in combination with nanometer-scale secondary ion mass spectrometry and mathematical modeling to quantify sugar assimilation at the single-cell level. We found large variation in metabolic activities between single cells, both in absolute assimilation and in the degree to which individual cells specialize in the assimilation of different sugars. Analysis of transcriptional reporters indicated that this variation was at least partially based on cell-to-cell variation in gene expression. Metabolic differences between cells in clonal populations could potentially reduce metabolic incompatibilities between different pathways, and increase the rate at which parallel reactions can be performed.
The work aims at addressing the modelling and implementation of criteria for multiple crack propagation, including interaction and coalescence, for a more reliable fracture mechanics-based prediction of stress-life curves for weldments.
A large experimental work is presented in which micro-cracks have been made visible by heat-tinting at successive stages of fatigue life of the welded specimens. Here the correlation between the number of initiation sites and the applied stress level has been also investigated.
The criteria have been implemented in in-house software, which allows multiple fatigue crack propagation, and validated against selected experimental tests. The results have shown that the modelling of multiple crack propagation and interaction is crucial for the prediction of the fatigue strength of weldments, both in finite and infinite life regime.
The additive manufacturing technology of Selective Laser Melting (SLM) experiences a rapid development within an increasing marked of quite different application fields. The properties of SLM materials and structures are influenced by a number of tech-nological parameters such as the metal powder (particle size, homogeneity, cleanliness), the laser tool (power, beam diameter, pulse lengths), the scanning operation (speed, sequence and orientation of melting paths), parameters of the over-all equipment (design and preheating of the base plate, currents and turbulence in the protective gas atmosphere) and, last not least, the hatching strategy including the build-up direction of the structure with respect to the loading direction of the component.
For the perspective use of SLM structures as load carrying, safety-relevant components the knowledge of their mechanical properties is necessary. It is essential to understand these in the context of the manufacturing-related features and at the back-ground of the basic characteristics of metallic materials: crystal lattice, microstructure and material defects. The paper provides an overview on factors which affect the mechanical parameters stiffness, strength, ductility, toughness, fatigue crack propagation and fatigue strength in the context of selective laser melting.
The paper provides an overview on the results of a German cluster project on the use of fracture mechanics to the determination of the fatigue strength of weldments with fatigue cracks originating at the weld toes. The approach includes (a) a concept for short crack propagation for which the common ΔK concept is not applicable and the crack closure effects are still being gradually build-up, (b) a method for determining fatigue life relevant initial crack sizes as they are needed in any fracture mechanics analysis and (c) multiple cracking and crack coalescence at load levels higher than the endurance limit. The analyses are stochastically performed. Both, the endurance limit and the finite life branch of the S-N curve are determined.
Besides a brief introduction into the approach, validation examples are presented. These comprise different weldment types (butt welds, cross joints and longitudinal stiffened plates), two steels (S355NL and S960QL) of quite different strengths, different weld geometries due to different welding techniques (WIG, MAG), as-welded and stress relieved welds and different stress ratios varying from R = -1 to R = 0.5.
Fracture mechanics based component design requires appropriate fracture mechanics toughness data with respect to both, loading rate as well as test temperature. Taking high-rate loading into account such as with accidental scenarios, different standards such as ASTM E 1820 or BS 7448-3 provide some information on dynamic fracture mechanics testing. Nevertheless, the designations differ so that a validation of the own material specific test method used for dynamic R-curve determination is mandatory. In order to address this for ductile cast iron materials an experimental method for the reliable determination of dynamic J-integral crack resistance curves at -40 °C following the multiple specimen approach has been established and validated. The experimental concept offers some additional valuable features. Single values of dynamic crack initiation toughness can be determined using a single specimen technique based on crack sensors. Furthermore, an experimentally independent method is provided according to which CTOD δ5 R-curves can be established. The focus of the present paper is on the validation of the experimental low blow technique using a drop tower test system.
A drop tower test system was developed and set up to perform low blow tests at temperatures down to -40 °C. The system allows for a variation of the impact mass and height and was optimized for testing of ductile cast iron at stress intensity rates from approximately 5∙10⁴ to 3∙10⁵ MPa√ms⁻¹. This range of loading rate is characteristic for instance with crash scenarios of heavy sectioned DCI casks for radioactive materials. In order to address characteristic challenges of impact tests (test duration of microseconds up to milliseconds, inertial effects, signal oscillations), an appropriate full bridge strain gage method for the measurement of force directly on the specimen as well as a non-contact measurement of load line displacement using an optical extensometer have been developed and validated.
The low blow test requires either to prevent bouncing strikes of the hammer by using the stop block technique or to catch the hammer after its first strike. Both options are not part of the experimental concept and setup which have been realized here. The paper describes investigations which have been performed in order to make sure that bouncing strikes of the hammer do not cause additional crack extension in the specimen. This is necessary to ensure a unique relation between the work done and the achieved crack extension. The investigations covered the analysis of limit loads of the specimen with respect to the measured force. The measured stiffness of the specimen was assessed and signals of crack sensors were analyzed. Furthermore, an analysis of the mechanical behavior of the loading system and the specimen by optical observation was performed. Corresponding results are discussed in the paper. It had finally been proven that additional crack extension in the specimen due to bouncing strikes of the hammer is not to be expected under the given conditions of test setup, material and loading. It can be seen as a major experimental advantage that the striker does not have to be catched after the low blow test.
A finite element tearing and interconnecting (FETI) approach for phase-field models and Gradient enhanced damage models is presented. These diffusive crack models can solve fracture mechanics problems by integrating a set of partial differential equations and thus avoid the explicit treatment of discontinuities. However, they require a fine discretization in the vicinity of the crack. FETI methods distribute the computational cost among multiple processors and thus speed up the computation.
Damage caused by stress concentrations in the complex mesoscopic geometry of concrete leads to continuous stress redistribution over the material’s life time. The presented fatigue damage model
captures this by resolving each load cycle in a cycle-by-cycle time integration. The model extends a static damage model to failure caused by the (time dependent) strain amplitudes and, thus, allows calibrating the majority of the material’s parameters in static experiments.
The heterogeneous mesostructure of concreted causes local stress concentrations. Stress dependent phenomena like damage and creep as well as their interactions are effected by those stress
concentrations. Therefore a material model’s macroscopic behavior will differ whether the mesoscale structure is considered or not. The differences between the mesoscale approach and an homogeneous approach will be presented. The results are discussed with focus on the true materials behavior.
A coupled thermomechanical mesoscale model for concrete under heating is presented. When considering the heterogeneous structure under coupled loads, complex macroscopic material properties can be modelled using simple constitutive relations. For instance, damage evolution is directly driven by the incompatibility of thermal strains between matrix and aggregates. Without prescribing
fc = f(T), a decline in compressive strength with rising temperatures will be shown.
For in-service inspections on wheelset axles with a hollow drilling, mechanized ultrasound inspection systems with single element probes are typically used. The ultrasonic testing in the zones close to the external surface of the railway axles can be realized from the inside of the bore hole, without demounting the wheelset and without dismantling the wheels and the brake discs. The testing system must be able to find flaws in the external surface of the hollow shafts, whose surface lies in the radial-radial plane, these are called transversal flaw. Presently testing systems are used, where scanning is realized in the circumferential direction by mechanical rotation of the probe system in the actual drilling. The phased array probe system, which is presented here, can carry out the rotation scan electronically. The scan can be carried out by simply moving the system forward and backwards through the drilling without mechanical rotation. Manipulation becomes simpler and the inspection time can be shortened considerably. The ultrasonic beam can be inclined exactly and be focused in the plane vertical to the specimen axis.
The probe is designed with help of indispensable simulations using especially designed software developed by BAM. The feasibility and the alignment between the simulated and experimental results were shown in earlier projects reported by Boehm et al. (2006) and Völz et al. (2012). The main task here is to optimize a probe for bore holes with a diameter of 65 mm with an increase in sensitivity and a high spatial resolution. This development will be carried out by use of extensive simulations and result in certain changes of the relevant probe parameters.
Fourteen hollow and one cast anthropomorphic and zoomorphic figurines produced in Incan times for ritual offerings from the Ethnologisches Museum in Berlin were selected to investigate the technologies and alloys used for their fabrication with portable optical microscopy and non-destructive XRF elemental analysis. This group of gold and silver figurines includes typical specimens of the Inca production, such as the four silver figurines from the Island Coati in Lake Titicaca and the two gold figurines from Pachacamac, as well as specimens that are seldom present in collections, which makes them atypical. In addition to the tall figurines with atypical hair or standing pose, one bicolour figurine half silver, half gold) and another with coloured inlays were included in this study for comparison. The large majority of the silver specimens are made from very high quality alloys and the gold figurines are made from alloys containing low copper contents and silver ranging from 30wt% to 52wt%.
Melanised cell walls and extracellular polymeric matrices protect rock-inhabiting microcolonial fungi from hostile environmental conditions. How extracellular polymeric substances (EPS) perform this protective role was investigated by following development of the model microcolonial black fungus Knufia petricola A95 grown as a sub-aerial biofilm. Extracellular substances were extracted with NaOH/formaldehyde and the structures of two excreted polymers studied by methylation as well as NMR analyses. The main polysaccharide (~ 80%) was pullulan, also known as α-1,4-; α-1,6-glucan, with different degrees of polymerisation. Αlpha-(1,4)-linked-Glcp and α-(1,6)-linked-Glcp were present in the molar ratios of 2:1. A branched galactofuromannan with an α-(1,2)-linked Manp main chain and a β-(1,6)-linked Galf side chain formed a minor fraction (~ 20%). To further understand the roles of EPS in the weathering of minerals and rocks, viscosity along with corrosive properties were studied using atomic force microscopy (AFM). The kinetic viscosity of extracellular K. petricola A95 polysaccharides (≈ 0.97 × 10-6 m2 s-1) ranged from the equivalent of 2% (w/v) to 5% glycerine, and could thus profoundly affect diffusion-dominated processes. The corrosive nature of rock-inhabiting fungal EPS was also demonstrated by its effects on the aluminium coating of the AFM cantilever and the silicon layer below.
Magnetic iron oxide nanoparticle clusters (mnpc) coated with organic stabilizers were investigated using scanning transmission x-ray microscopy (STXM). Simultaneous surface and bulk sensitive Fe L3 edge absorption spectra, obtained using a photomultiplier tube and a channeltron, were used to detect subtle changes in the oxidation state in the surface and bulk of Iron Oxide mnpc.
The effectiveness of this mode of STXM operation is demonstrated for These nanoparticle clusters.
The sonication process is commonly used for de-agglomerating and dispersing nanomaterials in aqueous based media, necessary to improve homogeneity and stability of the suspension. In this study, a systematic step-wise approach is carried out to identify optimal sonication conditions in order to achieve a stable dispersion. This approach has been adopted and shown to be suitable for several nanomaterials (cerium oxide, zinc oxide, and carbon nanotubes) dispersed in deionized (DI) water. However, with any change in either the nanomaterial type or dispersing medium, there needs to be optimization of the basic protocol by adjusting various factors such as sonication time, power, and sonicator type as well as temperature rise during the process. The approach records the dispersion process in detail. This is necessary to identify the time Points as well as other above-mentioned conditions during the sonication process in which there may be undesirable changes, such as damage to the particle surface thus affecting surface properties. Our goal is to offer a harmonized approach that can control the Quality of the final, produced dispersion. Such a guideline is instrumental in ensuring dispersion quality repeatability in the nanoscience community, particularly in the field of nanotoxicology.
Currently, research in chemical manufacturing moves towards flexible plug-and-play approaches focusing on modular plants, capable of producing small scales on-demand with short down-times between individual campaigns. This approach allows for efficient use of hardware, a faster optimization of the process conditions, and thus, an accelerated introduction of new products to the market. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably straightforward and robust analysis techniques.
Here we report on a fast and reliable calibration-free online high field NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement with a time interval of 20 s per spectrum, and a robust, automated algorithm to interpret the obtained data. All spectra were acquired using a 500 MHz NMR spectrometer (Varian) with a dual band flow probe having a 1/16-inch polymer tubing working as a flow cell. Single scan 1H NMR spectra were recorded with an acquisition time of 5 s, relaxation delay of 15 s. As a proof-of-concept, the thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was conducted in non-deuterated solvents while its time-resolved behaviour was characterised with step tracer experiments.
Through the application of spectral modeling the signal area for each reactant can be deconvoluted in the online spectra and thus converted to the respective concentrations or molar ratios. The signals which were suitable for direct integration were used herein for comparison purposes of both methods.
Validation report on NMR
(2017)
The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug and play integration, even though they may appear to be more complex at first sight. Smart sensors enable concepts like self-diagnostics, self-calibration, and self-configuration/ parameterization whenever our current automation landscape allows it.
Here we summarize the currently discussed general requirements for process sensors 4.0 and introduce a smart online NMR sensor module as example, which was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (www.consensspire.eu).
Our current projects focus on the material analysis of the writing materials
kept in the Taylor-Schechter Collection at Cambridge University Library,
which houses the largest collection of Cairo Geniza fragments, about 190,000.
Although Geniza manuscripts have attracted a great deal of scholarly attention,
the material aspects of these documents seem to have been largely neglected.
The current study aims to obtain information on the composition of the writing
supports and the inks that were used, the production of the original manuscripts
and the history of their degradation. The collected data should supplement the
description based on Hebrew palaeography and codicology. Moreover, a characterisation
of the writing materials would provide insights on trade, local production
techniques and social structures. The tabulated results have the potential to
be used as geo-chronological markers if sufficient data is collected.
For our study, we chose Hebrew legal documents and letters from three communities
that co-existed in Fustat (today Cairo) in the 11th century: the Jerusalemite
(or ‘Palestinian’) community, the Babylonian community and the Karaites, three
different communities with different scribal traditions. In addition to this, we
studied non-biblical scrolls attributed to the Palestinian and Babylonian communities.
The question we addressed was whether we can correlate the use of a
specific type of ink to an objective criterion.
For our analysis at Cambridge University Library, we used a number of protocols
developed at BAM (Bundesanstalt für Materialforschung und -prüfung) in
Berlin and at the Centre for Study of Manuscript Cultures, University of Hamburg
(CSMC). These include reflectographic examination followed by non-destructive
X-ray fluorescence (XRF) analysis using transportable instruments so that the
analysis can be carried out in situ.
We have illustrated our approach here by providing two examples. The first one
describes our investigation of the leather fragment containing a portion of the
Babylonian Talmud on its hair side (TS Misc.26.53.17). The second example illustrates
our ability to compare iron-gall inks using the XRF method. In this case,
we explored the question of the codicological attribution of three fragments (TS
F17.4, TS 12.755 and TS 12.756) to the same Talmud manuscript.
As part of the Qumran project conducted at the Federal Institute for Materials Research and Testing (BAM) in Berlin between 2007 and 2010, my colleagues and I developed a new, integrated methodology for determining the original and acquired properties of highly heterogeneous Dead Sea Scrolls. The purpose of this methodology is to help scholars determine the provenance of fragments of the scrolls and sort and compare them more easily than in the past. Since our measurements allowed us to differentiate between the minerals originating from the production processes and the sediments accrued during storage in the caves in Qumran, we were able to reconstruct the treatment of hides and discovered that at least two distinct parchmentproduction techniques co-existed at the beginning of the common era.
The reconstruction of workmanship on animal hides in Antiquity raised doubts about the validity of the current definition of parchment, which is based on a production technique known from the Middle Ages. We hope that our current work will also help researchers understand the characteristic properties of gewil, qelaf and dukhsustos better.¹
The evolution and socio-geographic distribution of writing inks in late Antiquity and the early Middle Ages are the second focus of our investigative work at BAM.
We use X-ray fluorescence analysis (XRF) to determine the chemical composition of inks and NIR reflectography for their typology. We are amply assisted in our ambitious enterprise by codicologists and palaeographers who have adopted our methodology and conduct field studies of their own.
Two novel species of the fungal genus Ochroconis, O. lascauxensis and O. anomala have been isolated from the walls of the Lascaux Cave, France. The interest in these fungi and their melanins lies in the formation of black stains on the walls and rock art which threatens the integrity of the paintings. Here we report solid-state cross polarization magic-angle spinning 13C and 15N nuclear magnetic resonance (NMR) spectroscopy and surface-enhanced Raman spectroscopy (SERS) of the melanins extracted from the mycelia of O. lascauxensis and O. anomala in order to known their chemical structure. The melanins from these two species were compared with those from other fungi. The melanins from the Ochroconis species have similar SERS and 13C and 15N NMR spectra. Their chemical structures as suggested by the data are not related to 3,4-dihydroxyphenylalanine, 5,6-dihydroxyindole or 1,8-dihydroxynaphthalene precursors and likely the building blocks from the melanins have to be based on other phenols that react with the N-terminal amino acid of proteins. The analytical pyrolysis of the acid hydrolysed melanin from O. lascauxensis supports this assumption.
The development of alkali‐activated materials (AAMs) as an alternative to Portland cement (PC) has seen significant progress in the past decades. However, there still remains significant uncertainty regarding their long term performance when used in steel‐reinforced structures. The durability of AAMs in such applications depends strongly on the corrosion behaviour of the embedded steel reinforcement, and the experimental data in the literature are limited and in some cases inconsistent. This letter elucidates the role of the chemistry of AAMs on the mechanisms governing passivation and chloride‐induced corrosion of the steel reinforcement, to bring a better understanding of the durability of AAM structures exposed to chloride. The corrosion of the steel reinforcement in AAMs differs significantly from observations in PC; the onset of pitting (or the chloride ‘threshold’ value) depends strongly on the alkalinity, and the redox environment, of these binders. Classifications or standards used to assess the severity of steel corrosion in PC appear not to be directly applicable to AAMs due to important differences in pore solution chemistry and phase assemblage.
This paper presents a novel non-destructive testing and health monitoring system using a network of tactile transducers and accelerometers for the condition assessment and damage classification of foundation piles and utility poles. While in traditional pile integrity testing an impact hammer with broadband frequency excitation is typically used, the proposed testing system utilizes an innovative excitation system based on a network of tactile transducers to induce controlled narrow-band frequency stress waves. Thereby, the simultaneous excitation of multiple stress wave types and modes is avoided (or at least reduced), and targeted wave forms can be generated. The new testing system enables the testing and monitoring of foundation piles and utility poles where the top is inaccessible, making the new testing system suitable, for example, for the condition assessment of pile structures with obstructed heads and of poles with live wires. For system validation, the new system was experimentally tested on nine timber and concrete poles that were inflicted with several types of damage. The tactile transducers were excited with continuous sine wave signals of 1 kHz frequency. Support vector machines were employed together with advanced signal processing algorithms to distinguish recorded stress wave signals from pole structures with different types of damage. The results show that using fast Fourier transform signals, combined with principal component analysis as the input feature vector for support vector machine (SVM) classifiers with different kernel functions, can achieve damage classification with accuracies of 92.5% ± 7.5%.
Non-destructive testing (NDT) helps to find material defects without having an influence on the material itself. It is applied as a method of quality control, for online structural health monitoring, and for inspection of safety related components. Due to the ability of automation and a simple test setup ultrasonic testing is one major NDT technique next to several existing options. Whereas contact technique allows the use of higher frequencies of some MHz and phased array focusing, air-coupled ultrasonic testing (ACUT) shows different advantages. Most significant for ACUT is the absence of any coupling fluid and an economical test procedure respective time and costs. Both contact technique and ACUT have been improved and enhanced during the past years. One important enhancement is the development of airborne transducers based on ferroelectrets, like charged cellular polypropylene (cpp), which makes the application of any matching layers being mandatory in conventional piezoelectric transducers unnecessary. In this contribution we show ultrasonic inspection results of specimens made of carbon- and glass-fibre-reinforced plastic. These specimens include defects represented by drill holes and artificial delaminations of various size and depth. We compare inspection results achieved by using contact technique to those achieved by ACUT. For ACUT, conventional piezoelectric transducers and transducers based on cpp were used, both focused as well as non-focused types. Contact inspections were performed with a multi-channel matrix array probe. Once the inspection data is recorded it can be analysed in order to detect and evaluate defects in the specimen. We present different analysing strategies and compare these regarding detection rate and sizing of defects.
Detection of the electronic structure of iron-(III)-oxo oligomers forming in aqueous solutions
(2017)
The nature of the small iron-oxo oligomers in iron-(III) aqueous solutions has a determining effect on the chemical processes that govern the formation of nanoparticles in aqueous phase. Here we report on a liquid-Jet photoelectron-spectroscopy experiment for the investigation of the electronic structure of the occurring iron-oxo oligomers in FeCl3 aqueous solutions. The only iron species in the as-prepared 0.75 M solution are Fe3+ monomers. Addition of NaOH initiates Fe3+ hydrolysis which is followed by the formation of iron-oxo oligomers. At small enough NaOH concentrations, corresponding to approximately [OH]/[Fe] = 0.2–0.25 ratio, the iron oligomers can be stabilized for several hours without engaging in further aggregation. Here, we apply a combination of non-resonant as well as iron 2p and Oxygen 1s resonant photoelectron spectroscopy from a liquid microjet to detect the electronic structure of the occurring species. Specifically, the oxygen 1s partial electron yield X-ray absorption (PEY-XA) spectra are found to exhibit a peak well below the onset of liquid water and OH (aq) absorption. The iron 2p absorption gives rise to signal centered between the main absorption bands typical for aqueous Fe3+. Absorption bands in both PEY-XA spectra are found to correlate with an enhanced photoelectron Peak near 20 eV binding energy, which demonstrates the sensitivity of resonant photoelectron (RPE) spectroscopy to mixing between iron and ligand orbitals. These various signals from the iron-oxo oligomers exhibit Maximum intensity at [OH]/[Fe] = 0.25 ratio. For the same ratio, we observe changes in the pH as well as in complementary Raman spectra, which can be assigned to the Transition from monomeric to oligomeric species. At approximately [OH]/[Fe] = 0.3 we begin to observe particles larger than 1 nm in radius, detected by small-angle X-ray scattering.
Although the concept of structural water that is bound inside hydrophobic pockets and helps to stabilize protein structures is well established, water has rarely found a similar role in supramolecular polymers. Water is often used as a solvent for supramolecular polymerization, however without taking the role of a comonomer for the supramolecular polymer structure. We report a low–molecular weight monomer whose supramolecular polymerization is triggered by the incorporation of water. The presence of water molecules as comonomers is essential to the polymerization process. The supramolecular polymeric material exhibits strong adhesion to surfaces, such as glass and paper. It can be used as a water-activated glue, which can be released at higher temperatures and reused many times without losing its performance.
Data correction is probably the least favourite activity amongst users experimenting with small-angle X-ray scattering: if it is not done sufficiently well, this may become evident only during the data analysis stage, necessitating the repetition of the data corrections from scratch. A recommended comprehensive sequence of elementary data correction steps is presented here to alleviate the difficulties associated with data correction, both in the laboratory and at the synchrotron. When applied in the proposed order to the raw signals, the resulting absolute scattering cross section will provide a high degree of accuracy for a very wide range of samples, with its values accompanied by uncertainty estimates. The method can be applied without modification to any pinhole-collimated instruments with photon-counting direct-detection area detectors.
Efficiency Evaluation of Extraction Methods for Analysis of OCPs and PCBs in Soils of Varying TOC
(2017)
Organochlorine pesticides and polychlorinated biphenyls are toxic, carcinogenic, and have a high potential for bioaccumulation. Due to their stability, they are still considered an environmental problem even though the use of most of them has been phased out several decades ago. Soil is a matrix which can retain these contaminants to a great extent. This ability is often associated with the total organic carbon content (TOC). In order to judge the pollution status of soil and to make monitoring data more easily comparable a simple, yet robust extraction method is needed. Agitation solid-liquid-extraction is well suited for this purpose. However, the influence of TOC on the analyte recovery has to be known. For the presented study, 12 organochlorine pesticides and 7 polychlorinated biphenyls were spiked into four model soils with organic carbon contents between 1.6% - 13.3%. The matrices were extracted using solid-liquid extraction between 45 minutes and 16 hours. For comparison, all soils were also extracted using pressurised liquid extraction and Soxhlet extraction. After clean-up the extracts were measured using a gas chromatography-mass spectrometry (GC-MS) system. Statistical analysis of the results implied that the TOC content of the soils did not have significant influence on the extraction efficiency. A longer solid-liquid extraction time did not necessarily increase analyte recovery: Extraction for one hour resulted in 88% recovery while 16 hour extraction led to 89%. Thus, the efficiency of all the methods was comparable for all model soils. Additional investigations regarding GC liner performance highlighted the need for isotopically labelled standards during the analysis of thermolabile pesticides.
A simple batch test leaching procedure is used in many countries, as a compliance test, to evaluate the leaching of mainly inorganic substances from soil. However, agitating certain types of soil and then passing the solution through a membrane filter with 0.45-µm pores yields filtrates that have been colored by the colloidal particles. These colloids might affect the results of the inorganic substances obtained in the batch tests. In this study, we evaluated the effects of colloidal particles on the results and the reproducibility of batch tests on contaminated soil using different agitation methods and membrane filters with different pore sizes. The leaching behaviors of As, Pb, Se, F and Cl from three types of soil were studied. The As and Pb concentrations in the leachates of some types of soil were clearly affected by the amount of colloidal particles with a diameter of 0.10–0.45 µm and by the agitation method used. This was probably because As and Pb were present mainly in the particulate form in the leachate that had been passed through a membrane filter with 0.45-µm pores. This is not the case for every type of soil. The results of batch leaching tests showed that not only dissolved but also colloidal forms with a diameter of 0.10–0.45 µm might be included and that the existence of colloidal particles in the leachate decreases the batch leaching test reproducibility.
In the present study, we applied a regularized inversion method to extract the particle size, magnetic moment and relaxation-time distribution of magnetic nanoparticles from small-angle x-ray scattering (SAXS), DC magnetization (DCM) and AC susceptibility (ACS) measurements. For the measurements the particles were colloidally dispersed in water. At first approximation the particles could be assumed to be spherically shaped and homogeneously magnetized single-domain particles. As model functions for the inversion, we used the particle form factor of a sphere (SAXS), the Langevin function (DCM) and the Debye model (ACS). The extracted distributions exhibited features/peaks that could be distinctly attributed to the individually dispersed and non-interacting nanoparticles. Further analysis of these peaks enabled, in combination with a prior characterization of the particle ensemble by electron microscopy and dynamic light scattering, a detailed structural and magnetic characterization of the particles. Additionally, all three extracted distributions featured peaks, which indicated deviations of the scattering (SAXS), magnetization (DCM) or relaxation (ACS) behavior from the one expected for individually dispersed, homogeneously magnetized nanoparticles. These deviations could be mainly attributed to partial agglomeration (SAXS, DCM, ACS), uncorrelated surface spins (DCM) and/or intra-well relaxation processes (ACS). The main advantage of the numerical inversion method is that no ad hoc assumptions regarding the line shape of the extracted distribution functions are required, which enabled the detection of these contributions. We highlighted this by comparing the results with the results obtained by standard model fits, where the functional form of the distributions was a priori assumed to be log-normal shaped.
Virulence determines the impact a pathogen has on the fitness of its host, yet current understanding of the evolutionary origins and causes of virulence of many pathogens is surprisingly incomplete. Here, we explore the evolution of Marek’s disease virus (MDV), a herpesvirus commonly afflicting chickens and rarely other avian species. The history of MDV in the 20th century represents an important case study in the evolution of virulence. The severity of MDV infection in chickens has been rising steadily since the adoption of intensive farming techniques and vaccination programs in the 1950s and 1970s, respectively. It has remained uncertain, however, which of these factors is causally more responsible for the observed increase in virulence of circulating viruses. We conducted a phylogenomic study to understand the evolution of MDV in the context of dramatic changes to poultry farming and disease control. Our analysis reveals evidence of geographical structuring of MDV strains, with reconstructions supporting the emergence of virulent viruses independently in North America and Eurasia. Of note, the emergence of virulent viruses appears to coincide approximately with the introduction of comprehensive vaccination on both continents. The time-dated phylogeny also indicated that MDV has a mean evolutionary rate of ~1.6 × 10−5 substitutions per site per year. An examination of gene-linked mutations did not identify a strong association between mutational variation and virulence phenotypes, indicating that MDV may evolve readily and rapidly under strong selective pressures and that multiple genotypic pathways may underlie virulence adaptation in MDV.
Classical film radiography is a well-established NDT technique and it is most commonly used for testing weld seams and corroded pipes e.g. in oil and gas industry or in nuclear power plants. In the course of digitization, digital detector arrays (DDA) are finding their way into industrial applications and are replacing film radiography step by step. This study deals with the latest generation of DDAs, the photon counting and energy resolving detectors (PCD), and their characteristics compared to charge integrating detectors (CID). No matter which technology to use, radiography still lacks a general issue: A three-dimensional object is projected onto a two dimensional image. Of course, advanced computed tomography (CT) algorithms exist since many years, but if the object to investigate is too large to fit into the manipulation system or its shape is not appropriate, CT is not feasible or sensible to be applied. To overcome this limitation, numerous laminographic algorithms have been developed in the past. In this study, photon counting detectors are used in combination with co-planar translational laminography to gain reconstructed three-dimensional volumes. Both laminographic testing and PCDs require a serious knowledge of many parameters that can influence the image quality in the resulting datasets. These are e.g. the detector efficiency and calibration procedure, setting of energy thresholds, exposure data, number of projections, beam length correction and spatial resolution. The use of PCDs yields more variables to be considered compared to CIDs. The most important parameters in laminographic testing and in the use of PCDs are described in this study and limits are discussed.
Ancient papyri are a written heritage of culture that flourished more than 3000 years ago in Egypt. One of the most significant collections in the world is housed in the Egyptian Museum and Papyrus Collection in Berlin, from where the samples for our investigation come. The papyrologists, curators and conservators of such collections search intensely for the analytical detail that would allow ancient papyri to be distinguished from modern fabrications, in order to detect possible forgeries, assess papyrus deterioration state, and improve the design of storage conditions and conservation methods. This has become the aim of our investigation. The samples were studied by a number of methods, including spectroscopic (FTIR, fluorescent-FS, Raman) diffractional (XRD) and chromatographic (size exclusion chromatography-SEC), selected in order to determine degradation parameters: overall oxidation of lignocellulosic material, degree of polymerization and crystallinity of cellulose. The results were correlated with those obtained from carefully selected model samples including modern papyri and paper of different composition aged at elevated temperature in humid air. The methods were classified in the order SEC > FS > FTIR > XRD, based on their effectiveness in discriminating the state of papyri degradation. However, the most trustworthy evaluation of the age of papyri samples should rely on several methods.
Environmental and sustainable economical concerns are generating a growing interest in biofuels predominantly produced from biomass. It would be ideal if an energy conversion device could directly extract energy from a sustainable energy resource such as biomass. Unfortunately, up to now, such a direct conversion device produces insufficient power to meet the demand of practical applications. To realize the future of biofuel-fed fuel cells as a green energy conversion device, efforts have been devoted to the development of carbon-based nanomaterials with tunable electronic and surface characteristics to act as efficient metal-free electrocatalysts and/or as supporting matrix for metal-based electrocatalysts. We present here a mini review on the recent advances in carbon-based catalysts for each type of biofuel-fed/biofuel cells that directly/indirectly extract energy from biomass resources, and discuss the challenges and perspectives in this developing field
Ectoine plays an important role in protecting biomolecules and entire cells against environmental stressors such as salinity, freezing, drying and high temperatures. Recent studies revealed that ectoine also provides effective protection for human skin cells from damage caused by UV-A radiation. These protective properties make ectoine a valuable compound and it is applied as an active ingredient in numerous pharmaceutical devices and cosmetics. Interestingly, the underlying mechanism resulting in protecting cells from radiation is not yet fully understood. Here we present a study on ectoine and its protective influence on DNA during electron irradiation. Applying gel electrophoresis and atomic force microscopy, we demonstrate for the first time that ectoine prevents DNA strand breaks caused by ionizing electron radiation. The results presented here point to future applications of ectoine for instance in cancer radiation therapy.
Miniaturized pacemakers with a surface consisting of a Ti alloy may have to be removed after several years from their implantation site in the heart and shall, therefore, not be completely overgrown by cells or tissue. A method to avoid this may be to create at the surface by laser-ablation self-organized sharp conical spikes, which provide too little surface for cells (i.e., fibroblasts) to grow on. For this purpose, Ti-alloy substrates were irradiated in the air by 790 nm Ti:sapphire femtosecond laser pulses at fluences above the ablation threshold. The laser irradiation resulted in pronounced microstructure formation with hierarchical surface morphologies. Murine fibroblasts were seeded onto the laser-patterned surface and the coverage by cells was evaluated after 3–21 days of cultivation by means of scanning electron microscopy. Compared to flat surfaces, the cell density on the microstructures was significantly lower, the coverage was incomplete, and the cells had a clearly different morphology. The best results regarding suppression of cell growth were obtained on spike structures which were additionally electrochemically oxidized under acidic conditions. Cell cultivation with additional shear stress could reduce further the number of adherent cells.
Predictable Peptide Conjugation Ratios by Activation of Proteins with Succinimidyl Iodoacetate (SIA)
(2017)
The small heterobifunctional linker succinimidyl iodoacetate (SIA) was examined for the preparation of peptide–protein bioconjugates with predicable conjugation ratios. For many conjugation protocols, the protein is either treated with a reductant to cleave disulfide bonds or is reacted with thiolation chemicals, such as Traut’s reagent. Both approaches are difficult to control, need individual optimization and often lead to unsatisfactory results. In another popular approach, a heterobifunctional linker with a N-hydroxysuccinimide (NHS) and a maleimide functionality is applied to the protein. After the activation of some lysine ε-amino groups with the NHS ester functionality, a cysteine-containing peptide is attached to the activated carrier protein via maleimide. Particularly, the maleimide reaction leads to some unwanted byproducts or even cleavage of the linker. Many protocols end up with conjugates with unpredictable and irreproducible conjugation ratios. In addition, the maleimide-thiol addition product should be assumed immunogenic in vivo. To avoid these and other disadvantages of the maleimide approach, we examined the known linker succinimidyl iodoacetate (SIA) in more detail and developed two protocols, which lead to peptide–protein conjugates with predefined average conjugation ratios. This holds potential to eliminate tedious and expensive optimization steps for the synthesis of a bioconjugate of optimal composition.
Decision makers for waste management are confronted with the problem of selecting the most economic, environmental, and socially acceptable waste treatment process. This paper elucidates evaluation methods for waste treatment processes for the comparison of ecological and economic aspects such as material flow analysis, statistical entropy analysis, energetic and exergetic assessment, cumulative energy demand, and life cycle assessment.The work is based on the VDI guideline 3925. A comparison of two thermal waste treatment plants with different process designs and energy recovery systems was performed with the described evaluation methods. The results are mainly influenced by the type of energy recovery, where the waste-to-energy plant providing district heat and process steam emerged to be beneficial in most aspects. Material recovery options from waste incineration were evaluated according to sustainability targets, such as saving of resources and environmental protection.
In 2011, the Association of German Engineers (VDI) started working on a set of guidelines
towards increased resource efficiency. These guidelines represent a framework that defines resource efficiency and outlines considerations for the producing industry. A special guideline for SMEs is included as well as guidelines on methodologies for evaluating resource use
indicators, such as the cumulative raw material demand of products and production systems.
Resource efficiency, defined here as the relationship between a specific benefit or use and the natural resources that need to be spent or consumed to attain this benefit or use. It can be
evaluated by defining a function which expresses the specific benefit and quantifies the resource requirements through a set of indicators (use of raw materials, energy, water, land
and ecosystem services including sinks). The results from this also depend on the system boundary parameters and the allocation rules for by-products and waste treatment options. Optimising resource use is possible at all stages of a product’s or production system’s life cycle chain (raw material extraction, production and manufacturing, use and consumption, and the
end-of-life stage).
VDI guidelines are widely accepted across Germany’s industrial sector and therefore represent an important means of mainstreaming resource efficiency in this target area. As well as providing a methodological framework, the guidelines describe strategies and measures towards increasing resource efficiency, and they enable industrial producers and service providers to identify potential areas of improvement. The full article presents an overview of
the methodology and contents of these guidelines and discusses their impact in achieving absolute reductions in the industrial use of natural resources.
Approximation of the crack driving force for cracks at notches under static and cyclic loading
(2017)
The work deals with the efficient calculation of the elastic-plastic crack driving force (J-integral for monotonic loading andΔJ-integral under cyclic loading) for short cracks at notches as essential parameter for the reliable static and fatigue assessment of notched structures. The J- or ΔJ-integral is calculated based on analytical solutions for stress intensity factors, estimated by means of well-known weight function solutions in the case of cracks under power-law stress distributions. A plasticity-correction function is applied to the stress intensity factors to obtain the final expression of the crack driving force. The comparison between analytical solutions and finite element calculations in case of cracks at the weld toe in welded joints shows good agreement.
The mechanochemical Knoevenagel condensation of malononitrile with p-nitrobenzaldehyde was studied in situ using a tandem approach. X-ray diffraction and Raman spectroscopy were combined to yield time-resolved information on the milling process. Under solvent-free conditions, the reaction leads to a quantitative conversion to p-nitrobenzylidenemalononitrile within 50 minutes. The in situ data indicate that the process is fast and proceeds under a direct conversion. After stopping the milling process, the reaction continues until complete conversion. The continuous and the stopped milling process both result in crystalline products suitable for single crystal X-ray diffraction.
Mobility particle size spectrometers (MPSS) belong to the essential instruments in aerosol science that determine the particle number size distribution (PNSD)in the submicrometer size range. Following calibration procedures and target uncertainties against standards and reference instruments are suggested for a complete MPSS quality assurance program: a) calibration of the CPC counting efficiency curve (within 5% for the plateau counting efficiency; within 1 nm for the 50% detection efficiency diameter), b) sizing calibration of the MPSS, using a certified polystyrene latex (PSL) particle size standard at 203 nm (within 3%), c) intercomparison of the PNSD of the MPSS (within 10% and 20% of the dN/dlogDP concentration for the particle size range 20 – 200 nm and 200 to 800 nm, respectively), and d) intercomparison of the integral PNC of the MPSS (within 10%). Furthermore, following measurement uncertainties have been investigated: a) PSL particle size standards in the range from 100-500nm match within 1% after sizing calibration at 203 nm. b) Bipolar diffusion chargers based on the radioactive nuclides Kr85, Am241 and Ni63 and a new ionizer based on corona discharge follow the recommended bipolar charge distribution, while soft X-ray-based charges may alter faster than expected. c) The use of a positive high voltage supply show a 10% better performance than a negative one. d) The intercomparison of the integral PNC of an MPSS against the total number concentration is still within the target uncertainty at an ambient pressure of approximately 500 hPa.
Discoloration Effects of High-Dose gamma-Irradiation and Long-Term Thermal Aging of (U) HMW-PE
(2017)
Two polyethylene types with ultra-high (UHMWPE) and high molecular weight (HMW-PE) used as neutron radiation shielding materials in casks for radioactive waste were irradiated with doses up to 600 kGy using a 60Co gammasource. Subsequently, thermal aging at 125∘C was applied for up to one year. Degradation effects in the materials were characterized using colorimetry, UV-Visspectroscopy, IR spectroscopy, and DSC. Both materials exhibited a yellowing upon irradiation.The discoloration of UHMW-PE disappeared again after thermal aging.Therefore, the yellowing is assumed to originate fromannealable color centers in the formof free radicals that are trapped in the crystalline regions of the polymer and recombine at elevated temperatures. For the antioxidantcontaining HMWPE, yellowing was observed after both irradiation and thermal aging. The color change was correlated mainly to decomposition products of the antioxidant in addition to trapped radicals as in UHMW-PE. Additionally, black spots appeared after thermal aging of HMW-PE.
A wide range of aspects concerning microscope slides, their preparation, long-time storage, curatorial measures in collections, deterioration, restoration, and study is summarized based on our own data and by analyzing more than 600 references from the 19th century until 2016, 15 patents, and about 100 Materials Safety Data Sheets. Information from systematic zoology, conservation sciences, chemistry, forensic sciences, pathology, paleopathology, applied sciences like food industry, and most recent advances in digital imaging are put together in order to obtain a better understanding of which and possibly why mounting media and coverslip seals deteriorate, how slides can be salvaged, which studies may be necessary to identify a range of ideal mounting media, and how microscope studies can benefit from improvements in developmental biology and related fields. We also elaborate on confusing usage of concepts like that of maceration and of clearing.
The chemical ingredients of a range of mounting media and coverslip seals are identified as much as possible from published data, but this information suffers in so far as the composition of a medium is often proprietary of the manufacturer and may vary over time. Advantages, disadvantages, and signs of deterioration are documented extensively for these media both from references and from our own observations. It turns out that many media degrade within a few years, or decades at the latest, except Canada balsam with a documented life-time of 150 years, Euparal with a documented life-time of 50 years, and glycerol-paraffin mounts sealed with Glyceel, which represents almost the only non-deteriorating and easily reversible mount. Deterioration reveals itself as a yellowing in natural resins and as cracking, crystallization, shrinkage on drying or possibly on loss of a plasticizer, detachment of the coverslip, segregation of the ingredients in synthetic polymers, as well as continued maceration of a specimen to a degree that the specimen virtually disappears. Confusingly, decay does not always appear equally within a collection of slides mounted at the same time in the same medium. The reasons for the deteriorative processes have been discussed but are controversial especially for gum-chloral media. Comparing data from conservation sciences, chemical handbooks, and documented ingredients, we discuss here how far chemical and physical deterioration probably are inherent to many media and are caused by the chemical and physical properties of their components and by chemicals dragged along from previous preparation steps like fixation, chemical maceration, and physical clearing. Some recipes even contain a macerating agent, which proceeds with its destructive work. We provide permeability data for oxygen and water vapor of several polymers contained in mounting media and coverslip seals. Calculation of the penetration rate of moisture in one example reveals that water molecules reach a specimen within a few days up to about a month; this lays to rest extensive discussions about the permanent protection of a mounted specimen by a mounting medium and a coverslip seal.
Based on the ever growing evidence of the unsuitable composition and application of many, and possibly almost all, mounting media, we strongly encourage changing the perspective on microscope slides from immediate usability and convenience of preparation towards durability and reversibility, concepts taken from conservation sciences. Such a change has already been suggested by Upton (1993) more than 20 years ago for gum-chloral media, but these media are still encouraged nowadays by scientists. Without a new perspective, taxonomic biology will certainly lose a large amount of its specimen basis for its research within the next few decades. Modern non-invasive techniques like Raman spectroscopy may help to identify mounting media and coverslip seals on a given slide as well as to understand ageing of the media. An outlook is given on potential future studies.
In order to improve the situation of existing collections of microscope slides, we transfer concepts as per the Smithsonian Collections Standards and Profiling System, developed for insect collections more than 25 years ago, to collections of slides. We describe historical and current properties and usage of glass slides, coverslips, labels, and adhesives under conservational aspects. In addition, we summarize and argue from published and our own experimental information about restorative procedures, including re-hydration of dried-up specimens previously mounted in a fluid medium. Alternatives to microscope slides are considered. We also extract practical suggestions from the literature concerning microscope equipment, cleaning of optical surfaces, health risks of immersion oil, and recent improvements of temporary observation media especially in connection with new developments in digital software.
This paper presents the first worldwide inter-laboratory comparison of small-angle X-ray scattering (SAXS) for nanoparticle sizing. The measurands in this comparison are the mean particle radius, the width of the size distribution and the particle concentration. The investigated sample consists of dispersed silver nanoparticles, surrounded by a stabilizing polymeric shell of poly(acrylic acid). The silver cores dominate the X-ray scattering pattern, leading to the determination of their radius size distribution using (i) the generalized indirect Fourier transformation method, (ii) classical model fitting using SASfit and (iii) a Monte Carlo fitting approach using McSAS. The application of these three methods to the collected data sets from the various laboratories produces consistent mean number- and volume-weighted core radii of Rn = 2.76 (6) nm and Rv = 3.20 (4) nm, respectively. The corresponding widths of the lognormal radius distribution of the particles were σn = 0.65 (1) nm and σv = 0.71 (1) nm. The particle concentration determined using this method was 3.0 (4) g l−1 or 4.2 (7) × 10−6 mol l−1. These results are affected slightly by the choice of data evaluation procedure, but not by the instruments: the participating laboratories at synchrotron SAXS beamlines, commercial and in-house-designed instruments were all able to provide highly consistent data. This demonstrates that SAXS is a suitable method for revealing particle size distributions in the sub-20 nm region (at minimum), out of reach for most other analytical methods.
The Cambrian explosion, the rapid appearance of most animal phyla in the geological record, occurred concurrently with bottom seawater oxygenation. Whether this oxygenation Event was triggered through enhanced nutrient supply and organic carbon burial forced by increased continental weathering, or by species engaging in ecosystem engineering, remains a fundamental yet unresolved question. Here we provide evidence for several simultaneous developments that took place over the Ediacaran–Cambrian transition: expansion of siliceous sponges, decrease of the dissolved organic carbon pool, enhanced organic carbon burial, increased phosphorus removal and seawater oxygenation. This evidence is based on Silicon and carbon stable isotopes, Ge/Si ratios, REE-geochemistry and redox-sensitive elements in a chert-shale succession from the Yangtze Platform, China. According to this reconstruction, sponges have initiated seawater oxygenation by redistributing organic carbon oxidation through filtering suspended organic matter from seawater. The resulting increase in dissolved oxygen levels potentially triggered the diversification of eumetazoans.
We analyse the signal formation process for scanning electron microscopic imaging applications on crystalline specimens. In accordance with previous investigations, we find nontrivial effects of incident beam diffraction on the backscattered electron distribution in energy and momentum. Specifically, incident beam diffraction causes angular changes of the backscattered electron distribution which we identify as the dominant mechanism underlying pseudocolour orientation imaging using multiple, angle-resolving detectors. Consequently, diffraction effects of the incident beam and their impact on the subsequent coherent and incoherent electron transport need to be taken into account for an in-depth theoretical modelling of the energy- and momentum distribution of electrons backscattered from crystalline sample regions. Our findings have implications for the level of theoretical detail that can be necessary for the interpretation of complex imaging modalities such as electron channelling contrast imaging (ECCI) of defects in crystals. If the solid angle of detection is limited to specific regions of the backscattered electron momentum distribution, the image contrast that is observed in ECCI and similar applications can be strongly affected by incident beam diffraction and topographic effects from the sample surface. As an application, we demonstrate characteristic changes in the resulting images if different properties of the backscattered electron distribution are used for the analysis of a GaN thin film sample containing dislocations.
Periodic self-organization of matter beyond the diffraction limit is a puzzling phenomenon, typical both for surface and bulk ultrashort laser processing. Here we compare the mechanisms of periodic nanostructure formation on the surface and in the bulk of fused silica. We show that volume nanogratings and surface nanoripples having subwavelength periodicity and oriented perpendicular to the laser polarization share the same electromagnetic origin. The nanostructure orientation is defined by the near-field local enhancement in the vicinity of the inhomogeneous scattering centers. The periodicity is attributed to the coherent superposition of the waves scattered at inhomogeneities. Numerical calculations also support the multipulse accumulation nature of nanogratings formation on the surface and inside fused silica. Laser surface processing by multiple laser pulses promotes the transition from the high spatial frequency perpendicularly oriented nanoripples to the low spatial frequency ripples, parallel or perpendicular to the laser polarization. The latter structures also share the electromagnetic origin, but are related to the incident field interference with the scattered far-field of rough non-metallic or transiently metallic surfaces. The characteristic ripple appearances are predicted by combined electromagnetic and thermo-mechanical approaches and supported by SEM images of the final surface morphology and by time-resolved pump-probe diffraction measurements.
Measurements of downburst wind loading acting on an overhead transmission line in Northern Germany
(2017)
Along an overhead transmission line in Northern Germany, a unique instrumentation of anemometers and force measurements is installed. Details of this test line with wind measurements along a horizontal axis are given. A recent event of a presumable downburst wind event is analyzed by means of available data and precedent works on thunderstorm analysis. The measured response of the conductors at the suspension tower is investigated and compared with time domain simulation of a finite element model.