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Paper des Monats
- ja (71)
Selective Electron Beam Melting (SEBM) is a promising powder bed Additive Manufacturing technique for near-net-shape manufacture of high-value titanium components. However without post-manufacture HIPing the fatigue life of SEBM parts is currently dominated by the presence of porosity. In this study, the size, volume fraction, and spatial distribution of the pores in model samples have been characterised in 3D, using X-ray Computed Tomography, and correlated to the process variables. The average volume fraction of the pores (b0.2%) was measured to be lower than that usually observed in competing processes, such as selective laser melting, but a strong relationship was found with the differentbeamstrategies used to contour ,and infill by hatching, a part section. The majority of pores were found to be small spherical gas pores, concentrated in the infill hatched region; this was attributed to the lower energy density and less focused beam used in the infill strategy allowing less opportunity for gas bubbles to escape the melt pool. Overall, increasing the energy density or focus of the beam was found to correlate strongly to a reduction in the level of gas porosity. Rarer irregular shaped pores were mostly located in the contour region and have been attributed to a lack of fusion between powder particles.
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.consens-spire.eu).
The vast experience with the automated, ultrasonic system for the inspection of hollow railway axles used by Deutsche Bahn shows that much smaller flaws are detectable than required. This results in a number of false calls. False calls lead to unnecessary demounting and disassembling of wheelsets, which generates unnecessary additional costs. In order to adjust the sensitivity of the inspection system to reduce the number of false calls without compromising safety, the capability of the system to detect cracks needs to be comprehensively established. This capability can be quantified by using probability of detection (POD) curves for the system. The multi-parameter POD model makes it possible to include several factors that influence the crack detection in the analysis. The analysis presented in this paper shows that crack position, orientation, depth extension, and shape as well as the geometry of the axle all have influence on the ultrasonic response amplitude. For future work, calculation of the POD using multi-parameter POD model with these parameters is planned.
The use of novel multi-scale correlative methods, which involve the coordinated characterisation of matter across a range of length scales, are becoming of increasing value to materials scientists. Here, we describe for the first time how a multi-scale correlative approach can be used to investigate the nature of ductile fracture in metals. Specimens of a nuclear pressure vessel steel, SA508 Grade 3, are examined following ductile fracture using medium and high-resolution 3D X-ray computed tomography (CT) analyses, and a site-specific analysis using a dual beam plasma focused ion beam scanning electron microscope (PFIB-SEM). The methods are employed sequentially to characterise damage by void nucleation and growth in one volume of interest, allowing for the imaging of voids that ranged in size from less than 100 nm to over 100 mm. This enables the examination of voids initiated at carbide particles to be detected, as well as the large voids initiated at inclusions. We demonstrate that this multi-scale correlative approach is a powerful tool, which not only enhances our understanding of ductile failure through detailed characterisation of microstructure, but also provides quantitative information about the size, volume fractions and spatial distributions of voids that can be used to inform models of failure. It isfound that the vast majority of large voids nucleated at MnS inclusions, and that the volume of a void varied according to the volume of its initiating inclusion raised to the power 3/2. The most severe voiding was concentrated within 500 mm of the fracture surface, but measurable damage was found to extend to a depth of at least 3 mm. Microvoids associated with carbides (carbide-initiated voids) were found to be concentrated around larger inclusion-initiated voids at depths of at least 400 mm. Methods for quantifying X-ray CT void data are discussed, and a procedure for using this data to calibrate parameters in the Gurson-Tvergaard Needleman (GTN) model for ductile failure is also introduced.
X-ray tomography characterisation of lattice structures processed by selective electron beam melting
(2017)
Metallic lattice structures intentionally contain open porosity; however, they can also contain unwanted closed porosity within the structural members. The entrained porosity and defects within three different geometries of Ti-6Al-4V lattices, fabricated by Selective Electron Beam Melting (SEBM), is assessed from X-ray computed tomography (CT) scans. The results suggest that horizontal struts that are built upon loose powder show particularly high (~20 x 10⁻³ vol %) levels of pores, as do nodes at which many (in our case 24) struts meet. On the other hand, for struts more closely aligned (0° to 54°) to the build direction, the fraction of porosity appears to be much lower (~0.17 x 10⁻³%) arising mainly from pores contained within the original atomised powder particles.
Strand breaks and conformational changes of DNA have consequences for the physiological role of DNA. The natural protecting molecule ectoine is beneficial to entire bacterial cells and biomolecules such as proteins by mitigating detrimental effects of environmental stresses. It was postulated that ectoine-like molecules bind to negatively charged spheres that mimic DNA surfaces. We investigated the effect of ectoine on DNA and whether ectoine is able to protect DNA from damages caused by ultraviolet radiation (UV-A). In order to determine different isoforms of DNA, agarose gel electrophoresis and atomic force microscopy experiments were carried out with plasmid pUC19 DNA. Our quantitative results revealed that a prolonged incubation of DNA with ectoine leads to an increase in transitions from supercoiled (undamaged) to open circular (single-strand break) conformation at pH 6.6. The effect is pH dependent and no significant changes were observed at physiological pH of 7.5. After UV-A irradiation in ectoine solution, changes in DNA conformation were even more pronounced and this effect was pH dependent. We hypothesize that ectoine is attracted to the negatively charge surface of DNA at lower pH and therefore fails to act as a stabilizing agent for DNA in our in vitro experiments.
Avoiding aerial microfibre contamination of environmental samples is essential for reliable analyses when it comes to the detection of ubiquitous microplastics. Almost all laboratories have contamination problems which are largely unavoidable without investments in clean-air devices. Therefore, our study supplies an approach to assess background microfibre contamination of samples in the laboratory under particle-free air conditions. We tested aerial contamination of samples indoor, in a mobile laboratory, within a laboratory fume hood and on a clean bench with particles filtration during the examining process of a fish. The used clean bench reduced aerial microfibre contamination in our laboratory by 96.5%. This highlights the value of suitable clean-air devices for valid microplastic pollution data. Our results indicate, that pollution levels by microfibres have been overestimated and actual pollution levels may be many times lower. Accordingly, such clean-air devices are recommended for microplastic laboratory applications in future research work to significantly lower error rate
Scattering on scattering
(2017)
Erosion of soils affects both natural landscapes and engineering constructions as embankment dams or levees. Improving the safety of such earthen structures requires in particular finding out more about the elementary mechanisms involved in soil erosion. Towards this end, an experimental work was undertaken in three steps. First, several model materials were developed, made of grains (mostly glass beads) with solid bridges at particle contacts whose mechanical yield strength can be continuously varied. Furthermore, for most of them, we succeeded in obtaining a translucent system for the purpose of direct visualization. Second, these materials were tested against surface erosion by an impinging jet to determine a critical shear stress and a kinetic coefficient. Note that an adapted device based on optical techniques (combination of Refractive Index Matching and Planar Laser Induced Fluorescence) was used specifically for the transparent media. Third, some specifically developed mechanical tests, and particularly traction tests, were implemented to estimate the mechanical strength of the solid bridges both at micro-scale (single contact) and at macro-scale (sample) and to investigate a supposed relationship with soil resistance to erosion.
We focus here on the major and still relevant issue of soil erosion by fluid flows, and more specifically on the determination of both a critical threshold for erosion occurrence and a kinetics that specifies the rate of eroded matter entrainment. A state-of-the-art is first proposed with a critical view on the most commonly used methods and erosion models. It is then discussed an alternative strategy, promoting the use of model materials that allow systematic parametric investigations with the purpose of identifying more precisely the local mechanisms responsible for soil particle erosion and ultimately quantifying both critical onsets and kinetics, possibly through existing or novel empirical erosion laws. Finally, we present and discuss several examples following this methodology, implemented either by means of experiments or numerical simulations, and coupling erosion tests in several particular hydrodynamical configurations with wisely selected mechanical tests.
Here we investigate the physical mechanisms behind the surface erosion of a cohesive granular soil induced by an impinging jet by means of numerical simulations coupling fluid and grains at the microscale. The 2D numerical model combines the Discrete Element and Lattice Boltzmann methods (DEM-LBM) and accounts for the granular cohesion with a contact model featuring a paraboloidal yield surface. Here we review first the hydrodynamical conditions imposed by the fluid jet on a solid granular packing, turning then the attention to the impact of cohesion on the erosion kinetics. Finally, the use of an additional subcritical debonding damage model based on the work of Silvani and co-workers provides a novel insight into the internal solicitation of the cohesive granular sample by the impinging jet.
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 choice of a pure cohesive or a pure frictional viscoplastic model to represent the rheological behaviour of a flowslide is of paramount importance in order to obtain accurate results for real cases. The principal Goal of the present work is to clarify the influence of the type of viscous model—pure cohesive versus pure frictional—with the numerical reproduction of two different real flowslides that occurred in 1966: the Aberfan flowslide and the Gypsum tailings impoundment flowslide. In the present work, a depth-integrated model based on the v-pw Biot–Zienkiewicz formulation, enhanced with a diffusion-like equation to account for the pore pressure Evolution within the soil mass, is applied to both 1966 cases. For the Aberfan flowslide, a frictional viscous model based on Perzyna viscoplasticity is considered, while a pure cohesive viscous model (Bingham model) is considered for the case of the Gypsum flowslide. The numerical approach followed is the SPH method, which has been enriched by adding a 1D finite difference grid to each SPH node in order to improve the description of the pore water evolution in the propagating mixture. The results obtained by the performed simulations are in agreement with the documentation obtained through the UK National Archive (Aberfan flowslide) and the International Commission of large Dams (Gypsum flowslide).
Bees are considered to be threatened globally, with severe overwinter losses of the most important commercial pollinator, the Western honeybee, a major concern in the Northern Hemisphere. Emerging infectious diseases have risen to prominence due to their temporal correlation with colony losses. Among these is Deformed wing virus (DWV), which has been frequently linked to colony mortality. We now provide evidence of a strong statistical association between overwintering colony decline in the field and the presence of DWV genotype-B (DWV-B), a genetic variant of DWV that has recently been shown to be more virulent than the original DWV genotype-A. We link the prevalence of DWV-B directly to a quantitative measure of overwinter decline (workforce mortality) of honeybee colonies in the field. We demonstrate that increased prevalence of virus infection in individual bees is associated with higher overwinter mortality. We also observed a substantial reduction of infected colonies in the spring, suggesting that virus-infected individuals had died during the winter. Our findings demonstrate that DWV-B, plus possible A/B recombinants exhibiting DWV-B at PCR primer binding sites, may be a major cause of elevated overwinter honeybee loss. Its potential emergence in naïve populations of bees may have far-reaching ecological and economic impacts.
Unity in defence: honeybee workers exhibit conserved molecular responses to diverse pathogens
(2017)
Background: Organisms typically face infection by diverse pathogens, and hosts are thought to have developed specific responses to each type of pathogen they encounter. The advent of transcriptomics now makes it possible to test this hypothesis and compare host gene expression responses to multiple pathogens at a genome-wide scale. Here, we performed a meta-analysis of multiple published and new transcriptomes using a newly developed bioinformatics approach that filters genes based on their expression profile across datasets. Thereby, we identified common and unique molecular responses of a model host species, the honey bee (Apis mellifera), to its major pathogens and parasites: the Microsporidia Nosema apis and Nosema ceranae, RNA viruses, and the ectoparasitic mite Varroa destructor, which transmits viruses.
Results: We identified a common suite of genes and conserved molecular pathways that respond to all investigated pathogens, a result that suggests a commonality in response mechanisms to diverse pathogens. We found that genes differentially expressed after infection exhibit a higher evolutionary rate than non-differentially expressed genes. Using our new bioinformatics approach, we unveiled additional pathogen-specific responses of honey bees; we found that apoptosis appeared to be an important response following microsporidian infection, while genes from the immune signalling pathways, Toll and Imd, were differentially expressed after Varroa/virus infection. Finally, we applied our bioinformatics approach and generated a gene co-expression network to identify highly connected (hub) genes that may represent important mediators and regulators of anti-pathogen responses.
Conclusions: Our meta-analysis generated a comprehensive overview of the host metabolic and other biological processes that mediate interactions between insects and their pathogens. We identified key host genes and pathways that respond to phylogenetically diverse pathogens, representing an important source for future functional studies as well as offering new routes to identify or generate pathogen resilient honey bee stocks. The statistical and bioinformatics approaches that were developed for this study are broadly applicable to synthesize information across transcriptomic datasets. These approaches will likely have utility in addressing a variety of biological questions.
A complex measuring campaign has been performed including the simultaneous measurement of vehicle, track, and soil vibrations during train runs at 16, 25, 40, 63, 80, 100, 125, 140, 160 km/h, and impulse measurements of the passenger car, three track sections and the soil. A ballast track on the soil surface and on a concrete bridge have been investigated as well as a slab track in a tunnel. The evaluation and comparison of all these data shows a generally good agreement for all components if the strong low- and high-frequency cut-off characteristics of the layered and damped soil are incorporated. There is a strong causal correlation between the vehicle and the soil by the dynamic excitation forces and a weak relation between the track and the soil by the axle-sequence spectrum of the train. However, the similarity between the axle-impulse spectrum observed at the track and the spectra of the ground vibration lead to the special excitation component of “scattered axle impulses” which is pre-dominant at the far-field points of the soil.
The objective of this work is to report the improvement obtained in the discrimination of complex aroma and taste with subtle differences in odor and flavor, by the use of fast suitable procedures for the cases of measurements in the field demanding decision-making in real time. The proposed electronic sensing systems, formed by an E-nose and VE-tongue, were used to discriminate cumin cultivars from different geographical origins, as well as to quantify the cumin adulteration percentages by using unsupervised and supervised chemometric tools. Thus, the results obtained are sufficiently encouraging as a starting point for the development of new electronic sensing systems with more improvement such the reliability of the sensors’ performance as well as the chemometric tools in order to deal with a complex dataset.
The order Chaetothyriales (Pezizomycotina, Ascomycetes) harbours obligatorily melanised fungi and includes numerous etiologic agents of chromoblastomycosis, phaeohyphomycosis and other diseases of vertebrate hosts. Diseases range from mild cutaneous to fatal cerebral or disseminated infections and affect humans and cold-blooded animals globally. In addition, Chaetothyriales comprise species with aquatic, rock-inhabiting, ant-associated, and mycoparasitic life-styles, as well as species that tolerate toxic compounds, suggesting a high degree of versatile extremotolerance. To understand their biology and divergent niche occupation, we sequenced and annotated a set of 23 genomes of main the human opportunists within the Chaetothyriales as well as related environmental species. Our analyses included fungi with diverse life-styles, namely opportunistic pathogens and closely related saprobes, to identify genomic adaptations related to pathogenesis. Furthermore, ecological preferences of Chaetothyriales were analysed, in conjuncture with the order-level phylogeny based on conserved ribosomal genes. General characteristics, phylogenomic relationships, transposable elements, sex-related genes, protein family evolution, genes related to protein degradation (MEROPS), carbohydrate-active enzymes (CAZymes), melanin synthesis and secondary metabolism were investigated and compared between species. Genome assemblies varied from 25.81 Mb (Capronia coronata) to 43.03 Mb (Cladophialophora immunda). The bantiana-clade contained the highest number of predicted genes (12 817 on average) as well as larger genomes. We found a low content of mobile elements, with DNA transposons from Tc1/Mariner superfamily being the most abundant across analysed species. Additionally, we identified a reduction of carbohydrate degrading enzymes, specifically many of the Glycosyl Hydrolase (GH) class, while most of the Pectin Lyase (PL) genes were lost in etiological agents of chromoblastomycosis and phaeohyphomycosis. An expansion was found in protein degrading peptidase enzyme families S12 (serine-type D-Ala-D-Ala carboxypeptidases) and M38 (isoaspartyl dipeptidases). Based on genomic information, a wide range of abilities of melanin biosynthesis was revealed; genes related to metabolically distinct DHN, DOPA and pyomelanin pathways were identified. The MAT (MAting Type) locus and other sexrelated genes were recognized in all 23 black fungi. Members of the asexual genera Fonsecaea and Cladophialophora appear to be heterothallic with a single copy of either MAT-1-1 or MAT-1-2 in each individual. All Capronia species are homothallic as both MAT1-1 and MAT1-2 genes were found in each single genome. The genomic synteny of the MAT-locus flanking genes (SLA2-APN2-COX13) is not conserved in black fungi as is commonly observed in Eurotiomycetes, indicating a unique genomic context for MAT in those species. The heterokaryon (het) genes expansion associated with the low selective pressure at the MAT-locus suggests that a parasexual cycle may play an important role in generating diversity among those fungi.
Seabird excrements (guano) have been preserved in the arid climate of Northern Chile since at least the Pliocene. The deposits of marine organic material in coastal areas potentially open a window into the present and past composition of the coastal ocean and its food web. We use the stable isotope composition of nitrogen and carbon as well as element contents to compare the principal prey of the birds, the Peruvian anchovy, with the composition of modern guano. We also investigate the impact of diagenetic changes on the isotopic composition and elemental contents of the pure ornithogenic sediments, starting with modern stratified deposits and extending to fossil guano. Where possible, 14C systematics is used for age information. The nitrogen and carbon isotopic composition of the marine prey (Peruvian anchovy) of the birds is complex as it shows strong systematic variations with latitude. The detailed study of a modern profile that represents a few years of guano deposition up to present reveals systematic changes in nitrogen and carbon isotopic composition towards heavier values that increase with age, i.e. depth. Only the uppermost, youngest layers of modern guano show compositional affinity to the prey of the birds. In the profile, the simultaneous loss of nitrogen and carbon occurs by degassing, and non-volatile elements like phosphorous and calcium are passively enriched in the residual guano. Fossil guano deposits are very low in nitrogen and low in carbon contents, and show very heavy nitrogen isotopic compositions. One result of the study is that the use of guano for tracing nitrogen and carbon isotopic and elemental composition in the marine food web of the birds is restricted to fresh material. Despite systematic changes during diagenesis, there is little promise to retrieve reliable values of marine nitrogen and carbon signatures from older guano. However, the changes in isotopic composition from primary marine nitrogen isotopic signatures towards very heavy values generate a compositionally unique material. These compositions trace the presence of guano in natural ecosystems and its use as fertilizer in present and past agriculture.
Artificial light harvesting complexes find applications in artificial photosynthesis, photovoltaics and light harvesting chemical sensors. They are used to enhance the absorption of light of a reaction center which is often represented by a single acceptor. Here, we present different light harvesting systems on DNA origami structures and analyze systematically the light harvesting efficiency. By changing the number and arrangement of different fluorophores (FAM as donor, Cy3 as transmitter and Cy5 as acceptor molecules) the light harvesting efficiency is optimized to create a broadband absorption and to improve the antenna effect 1 (including two energy transfer steps) from 0.02 to 1.58, and the antenna effect 2 (including a single energy transfer step) from 0.04 to 8.7, i.e. the fluorescence emission of the acceptor is significantly higher when the light-harvesting antenna is excited at lower wavelength compared to direct excitation of the acceptor. The channeling of photo energy to the acceptor proceeds by Förster Resonance Energy Transfer (FRET) and we carefully analyze also the FRET efficiency of the different light harvesting systems. Accordingly, the antenna effect can be tuned by modifying the stoichiometry of donor, transmitter and acceptor dyes, whereas the FRET efficiency is mainly governed by the spectroscopic properties of dyes and their distances.
Recently, there has been a rise in freshwater harmful algal blooms (HABs) globally, as well as increasing aquaculture practices. HABs can produce cyanotoxins, many of which are hepatotoxins. An ultra-performance liquid chromatography tandem mass spectrometry method was developed and validated for nine cyanotoxins across three classes including six microcystins, nodularin, cylindrospermopsin and anatoxin-a. The method was used to analyse free cyanotoxin(s) in muscle (n = 34), liver (n = 17) and egg (n = 9) tissue samples of 34 fish sourced from aquaculture farms in Southeast Asia. Conjugated microcystin was analysed by Lemieux oxidation to ascertain the total amount of microcystin present in muscle. Some tilapia accumulated free microcystin-LR in the muscle tissue at a mean of 15.45 μg/kg dry weight (dw), with total microcystin levels detected at a mean level of 110.1 μg/kg dw, indicating that the amount of conjugated or masked microcystin present in the fish muscle accounted for 85% of the total. Higher levels of cyanotoxin were detected in the livers, with approximately 60% of those tested being positive for microcystin-LR and microcystin-LF, along with cylindrospermopsin. Two fish from one of the aquaculture farms contained cylindrospermopsin in the eggs; the first time this has been reported. The estimated daily intake for free and total microcystins in fish muscle tissue was 2 and 14 times higher, respectively, than the tolerable daily intake value. This survey presents the requirement for further monitoring of cyanotoxins, including masked microcystins, in aquaculture farming in these regions and beyond, along with the implementation of guidelines to safeguard human health.
Air pollution and climate change are potential drivers for the increasing burden of allergic diseases. The molecular mechanisms by which air pollutants and climate parameters may influence allergic diseases, however, are complex and elusive. This article provides an overview of physical, chemical and biological interactions between air pollution, climate change, allergens, adjuvants and the immune system, addressing how these interactions may promote the development of allergies. We reviewed and synthesized key findings from atmospheric, climate, and biomedical research. The current state of knowledge, open questions, and future research perspectives are outlined and discussed. The Anthropocene, as the present era of globally pervasive anthropogenic influence on planet Earth and, thus, on the human environment, is characterized by a strong increase of carbon dioxide, ozone, nitrogen oxides, and combustion- or traffic-related particulate matter in the atmosphere. These environmental factors can enhance the abundance and induce chemical modifications of allergens, increase oxidative stress in the human body, and skew the immune system toward allergic reactions. In particular, air pollutants can act as adjuvants and alter the immunogenicity of allergenic proteins, while climate change affects the atmospheric abundance and human exposure to bioaerosols and aeroallergens. To fully understand and effectively mitigate the adverse effects of air pollution and climate change on allergic diseases, several challenges remain to be resolved. Among these are the identification and quantification of immunochemical reaction pathways involving allergens and adjuvants under relevant environmental and physiological conditions.
The determination of the microscopic dose-damage relationship for DNA in an aqueous environment is of a fundamental interest for dosimetry and applications in radiation therapy and protection. We combine geant4 particle-scattering simulations in water with calculations concerning the movement of biomolecules to obtain the energy deposit in the biologically relevant nanoscopic volume. We juxtaposition these results to the experimentally determined damage to obtain the dose-damage relationship at a molecular level. This approach is tested for an experimentally challenging system concerning the direct irradiation of plasmid DNA (pUC19) in water with electrons as primary particles. Here a microscopic target model for the plasmid DNA based on the relation of lineal energy and radiation quality is used to calculate the effective target volume. It was found that on average fewer than two ionizations within a 7.5-nm radius around the sugar-phosphate backbone are sufficient to cause a single strand break, with a corresponding median lethal energy deposit being E1/2=6±4 eV. The presented method is applicable for ionizing radiation (e.g., γ rays, x rays, and electrons) and a variety of targets, such as DNA, proteins, or cells.
The report on the results of an in vitro digestion study of silver nanoparticles in presence and absenceof food. The particles were poly(acrylic acid) stabilized ultra-small silver nanoparticles with a radius of 3.1 nm and a relative size distribution width of 0.2. As food components oil, starch, skimmed milk powderand a mixture thereof were chosen. Aggregation of the particles was quantified with small-angle X-rayscattering in terms of log-normal radii distributions. Complete aggregation of the primary particles wasdetermined in the absence of food. In contrast, the presence of oil and starch initiates a disaggregationin the intestine. Only small aggregates of 6 nm radii and aggregation numbers of 7 were found in thepresence of milk powder. It prevents primary particles from etching in the gastric and intestinal juice.Our results indicate that the silver nanoparticles can pass the digestion process in a nanoscale form butundergo a strong and food-dependent transformation in their state of aggregation.
Structural Health Monitoring (SHM) is an important part of buildings surveillance and maintenance to detect material failure as early as possible and to contribute in protection of structures and their users.
The implementation of Radio Frequency Identification (RFID) sensor systems without cable connection and battery into building components offers innovative possibilities to enable long-term in-situ SHM of addressed structures, bridges. The objectives of the presented study are complete embedding of RFID sensors systems in concrete, full passive communication with the systems, at best for the whole life span of structures. One challenge for this task is the highly alkaline environment in concrete, which requires non-degrading and robust encapsulation. Further Requirements are passive communication and energy supply, appropriate antenna design, placement and fixation in concrete, and the selection and implementation of sensors and connections. The concept is to develop and optimize a simple and robust system, which meets the requirements, as well as comprehensive validation in concrete specimen and real world applications. Two different systems were developed (HF and UHF RFID, respectively).
First tasks were the implementation of analog sensors using the superposition principle for the signal adaption. Investigation of suitable materials for robust encapsulation and sensor protection against basic environments.
Four materials were investigated in pH 13 solution for 14 days
- 3D-Printer-Polymer was completely resolved
- PVC has no noticeable decrease in weight
- (VitaPro) glass filter for the sensor protector, has weight loss 2.7 %
- The epoxy resin has increased by 1.8 % due to moisture expansion
Different concrete samples were prepared for the validation of the systems.
RFID sensors were embedded in different integration depths. Investigate the energy- and data transfer through concrete, also with varying moisture content. Additionally, signal strength data was used to optimize and validate the antenna characteristics in concrete. Next steps are to guarantee a sufficient energy supply for UHF RFID systems embedded in different concrete mixtures and further embedding the HF and UHF RFID systems in real bridges and buildings to validate the long term monitoring.
The genome of the Halomonas elongata type strain DSM 2581, an industrial producer, was reevaluated using the Illumina HiSeq2500 technology. To resolve duplication-associated ambiguities, PCR products were generated and sequenced. Outside of duplications, 72 sequence corrections were required, of which 24 were point mutations and 48 were indels of one or few bases. Most of these were associated with polynucleotide stretches (poly-T stretch overestimated in 19 cases, poly-C underestimated in 15 cases). These problems may be attributed to using 454 technology for original Genome sequencing. On average, the original genome sequence had only one error in 56 kb. There were 23 frameshift error corrections in the 29 protein-coding genes affected by sequence revision. The genome has been subjected to major reannotation in order to substantially increase the annotation quality.
Radiation induced attenuation in perfluorinated polymer optical fibres for dosimetry applications
(2016)
Real-time measurement of radiation-induced attenuation (RIA) in a commercial perfluorinated polymer optical fibre (PF-POF) is performed with regard to on-line Radiation monitoring purposes. Spectral character and dose dependence of fibre’s RIA is measured in 450-900 nm spectral region. Fibre exhibited high radiation sensitivity in the visible region with strong increase towards the UV wavelengths. Good linearity and high sensitivity reaching up to 130 dBm-1/kGy was demonstrated in the VIS region for a low-dose range. This of-the-shelf PF-POF could be therefore interesting for on-line remote dosimetry applications.
Impact of gamma radiation on transmission of a commercial Cytop polymer optical fibre (Lucina, Asahi Glass Company) is investigated. Spectral dependence of radiation induced attenuation in the investigated fibre is measured in the VIS-NIR spectral region. Besides attenuation increase, radiation is found to increase fibre susceptibility to water as well. While pristine Cytop fibre is rather humidity insensitive, strong humidity related absorption in the NIR region is observed after fibre irradiation. Selective irradiation of separate fibre sections is proposed as a way of fibre humidity sensitization and quasi-distributed water detection is demonstrated using optical time domain reflectometry at 1310 nm.
Novel MnS nanoclusters were synthesized on nickel foam (NF) using a successive ionic layer adsorption and reaction (SILAR) method. MnS nanoclusters with different sizes were obtained by varying the number of deposition cycles. The crystal structure, chemical composition, and surface microstructure of the electrodes were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, field Emission scanning electron microscopy, and high-resolution transmission electron microscopy. The electrochemical behavior of the MnS nanoclusters was examined by cyclic voltammetry, galvanostatic charge–discharge, cycling test, and electrochemical impedance spectroscopy. The MnS nanoclusters prepared with 90 SILAR cycles showed the best supercapacitance in a 6 M KOH aqueous electrolyte with a specific capacitance of 828 F/g at a scan rate of 5 mV/s and cycling stability of 85.2 % after 5000 charge–discharge cycles.
Moreover, an asymmetric supercapacitor (ASC) was assembled with the as-prepared MnS electrode on NF as the positive electrode, hydrothermally prepared reduced graphene oxide (rGO) on NF as the negative electrode, and PVA–KOH gel as the electrolyte. The MnS@NF//rGO@NF ASC showed excellent electrochemical performance with maximum energy and power densities of 34.1 Wh/kg and 12.8 kW/kg, respectively. The ASC also showed a capacitive retention of 86.5 % after 2000 charge–discharge cycles, highlighting its practical application for energy storage.
Photocatalysis is a promising technique to reduce volatile organic compounds indoors. Titanium dioxide (TiO2) is a frequently-used UV active photocatalyst. Because of the lack of UV light indoors, TiO2 has to be modified to get its working range shifted into the visible light spectrum. In this study, the photocatalytic degradation of toluene, butyl acetate and limonene was investigated under UV LED light and blue LED light in emission test chambers with catalysts either made of pure TiO2 or TiO2 modified with graphene oxide (GO). TiO2 coated with different GO amounts (0.75%–14%) were investigated to find an optimum ratio for the photocatalytic degradation of VOC in real indoor air concentrations. Most experiments were performed at a relative humidity of 0% in 20 L emission test chambers. Experiments at 40% relative humidity were done in a 1 m³ emission test chamber to determine potential byproducts. Degradation under UV LED light could be achieved for all three compounds with almost all tested catalyst samples up to more than 95%. Limonene had the highest degradation of the three selected volatile organic compounds under blue LED light with all investigated catalyst samples.
Methane dry reforming (DRM) was investigated over highly active Ni catalysts with low metal content (2.5wt%) supported on Mg-Al mixed oxide. The aim was to minimize carbon Deposition and metal sites agglomeration on the working catalyst which are known to cause catalyst deactivation.
The solids were characterized using N2 adsorption, X-ray diffraction, temperature-programmed reduction, X-ray photoelectron spectroscopy, and UV-Vis diffuse reflectance spectroscopy. The results showed that MgO-Al2O3 solid solution phases are obtained when calcining Mg-Al hydrotalcite precursor in the temperature range of 550–800 °C. Such phases contribute to the high activity of catalysts with low Ni content even at low temperature (500 °C). Modifying the catalyst preparation with citric acid significantly slows the coking rate and reduces the size of large octahedrally coordinated NiO-like domains, which may easily agglomerate on the surface during DRM. The most effective Ni catalyst shows a stable DRM course over 60 h at high weight hourly space velocity with very low coke deposition. This is a promising result for considering such catalyst systems for further development of an industrial DRM technology.
Phosphorus-based flame retardants were incorporated into different, easily preparable matrices, such as polymeric thermoset resins and paraffin as a proposed model for polyolefins and investigated for their flame retardancy performance. The favored mode of action of each flame retardant was identified in each respective system and at each respective concentration. Thermogravimetric analysis was used in combination with infrared spectroscopy of the evolved gas to determine the pyrolysis behavior, residue formation and the release of phosphorus species. Forced flaming tests in the cone calorimeter provided insight into burning behavior and macroscopic residue effects. The results were put into relation to the phosphorus content to reveal correlations between phosphorus concentration in the gas phase and flame inhibition performance, as well as phosphorus concentration in the residue and condensed phase activity. Total heat evolved (fire load) and peak heat release rate were calculated based on changes in the effective heat of combustion and residue, and then compared with the measured values to address the modes of action of the flame retardants quantitatively. The quantification of flame inhibition, charring, and the protective layer effect measure the non-linear flame retardancy effects as functions of the phosphorus concentration. Overall, this screening approach using easily preparable polymer systems provides great insight into the effect of phosphorus in different flame retarded polymers, with regard to polymer structure, phosphorus concentration, and phosphorus species.
A first pilot study on the sorption of environmental pollutants on various microplastic materials
(2017)
With the drastic increase in plastic production, the input of plastic particles into the environment has become a recognised problem.
Xenobiotics are able to sorb to polymer materials, and this process is further enhanced where they Encounter microplastics (plastic fragments <5 mm). In this work we studied the sorption of metformin, a type-2 diabetes drug, and difenoconazole, a fungicide, onto the virgin polymer materials polyamide (PA), polypropylene (PP), and polystyrene (PS). Additionally, PP was cryo-milled and PA was treated with acid to investigate the influence of an increase in surface area and chemical modification. The material properties were also studied by dynamic scanning calorimetry (DSC), gel permeation chromatography (GPC) and Fourier transform infrared spectroscopy (FTIR). Sorption experiments were performed on the basis of a full factorial design examining the effect of agitation, pH value, and salinity. Experimental results showed that difenoconazole sorbs readily to all microplastics, whereas the more polar analyte metformin did not show any affinity to the materials used. For difenoconazole the governing factor in all cases is agitation, while both pH and salinity exhibited only a slight influence. The modification of polymers leads to enhanced sorption, indicating that an increase in surface area (cryo-milled PP) or inner volume (acid-treated PA) strongly favours adsorption. Moreover, long-term experiments demonstrated that the time until equilibrium is reached depends strongly on the particle size.
Vibration-based model updating and identification of multiple axial forces in truss structures
(2017)
Safety assessment of existing iron and steel truss structures requires the determination of the axial Forces and corresponding stresses in truss structural members. The results of the axial force determination can be integrated as part of a structural health Monitoring scheme for existing trusses. In this work, a methodology is proposed to identify multiple axial forces in members of a truss structure based on the modal parameters. Vibration test allows the identification of the natural frequencies and mode shapes, globally of the truss structure as well as locally of the individual bars. The method calibrates the numerical model of the truss structure using a genetic algorithm and strategic validation criteria. The validation criteria are based on the identified natural frequencies and global mode shapes of the truss structure as well as information of the axial forces in the individual bars of the truss, which are estimated from the natural frequencies and five amplitudes of the corresponding local mode shapes of the single bars based on an analytical-based algorithm. The calibration allows the identification of the axial forces in all bars of the truss structure. For mode pairing strategy, a technique makes use of the enhanced modal assurance criteria with the calculation of the modal strain energies.
Moreover, the modal strain energies are also used to select the relevant local mode shape of the individual bars. The feasibility and accuracy of the proposed methodology is verified by laboratory experiments on several truss structures. In situ tests on existing trusses are intended. The results from one of the laboratory tested structures, i.e. a two-bar system, are included in this paper.
The structural and magnetic properties of magnetic multi-core particles were determined by numerical inversion of small angle scattering and isothermal magnetisation data. The investigated particles consist of iron oxide nanoparticle cores (9 nm) embedded in poly(styrene) spheres (160 nm). A thorough physical characterisation of the particles included transmission electron microscopy, X-ray diffraction and asymmetrical flow field-flow fractionation. Their structure was ultimately disclosed by an indirect Fourier transform of static light scattering, small angle X-ray scattering and small angle neutron scattering data of the colloidal dispersion. The extracted pair distance distribution functions clearly indicated that the cores were mostly accumulated in the outer surface layers of the poly(styrene) spheres. To investigate the magnetic properties, the isothermal magnetisation curves of the multi-core particles (immobilised and dispersed in water) were analysed. The study stands out by applying the same numerical approach to extract the apparent moment distributions of the particles as for the indirect Fourier transform. It could be shown that the main peak of the apparent moment distributions correlated to the expected intrinsic moment distribution of the cores. Additional peaks were observed which signaled deviations of the isothermal magnetisation behavior from the non-interacting case, indicating weak dipolar interactions.
Hydroxyapatite (HA) is a bioceramic material with excellent biological properties. However, these properties are strongly dependent of ist crystallinity degree, with high values of crystallinity associated to poor resorption rates and bioactivity. This work evaluates the properties of HA samples produced by two different free-forming conformation methods, CNC machining and 3D printing. In both cases, porous gypsum samples were produced and subsequently converted into HA in a reaction with di-ammonium hydrogen phosphate at 100°C and pH 8. A total conversion of the samples was achieved after 36 h independently of the conformation method used. The microstructure, however, before and after the conversion is showed to be dependent on the method used. After conversion the machined samples achieved a Maximum compressive strength of 3.5 MPaforporosities of circa 80%, while 3D printed samples achieved a tensile strength of 2.0 MPa by porosities of 61%.
Quantification of nanoparticle (NP) uptake in cells or tissues is very important for safety assessment. Often, electron microscopy based approaches are used for this purpose, which allow imaging at very high resolution. However, precise quantification of NP numbers in cells and tissues remains challenging. The aim of this study was to present a novel approach, that combines precise quantification of NPs in individual cells together with high resolution imaging of their intracellular distribution based on focused ion beam/ scanning electron microscopy (FIB/SEM) slice and view approaches.
The VSSA approach has the important advantage over classifying, imaging and counting techniques that it does not involve dispersion protocols. Further, the BET technique as the basis for VSSA determination it is in widespread use, generates low costs and is specified for many commercial materials. Finally, the same equipment allows for a deeper analysis by full isotherm evaluation.
The present deliverable assesses all NanoDefine powders, supplemented by further real-world materials (in total 26 powders), and quantitatively compares the relationship between the median size (by Electron Microscopy – considered as benchmark for the EC nanomaterial definition) vs. the size derived from VSSA. The VSSA method mitigates the challenges of EM to assess the thickness of platelets, but worked as well on fibbers and particles of irregular shapes. A screening strategy is proposed. If applied to the further data from real-world materials as validation set, this screening does achieve a correct classification, leaving only borderline materials for tier 2 assessment.
Hydroxyl radical-induced oxidation of proteins and peptides can lead to the cleavage of the peptide, leading to a release of fragments. Here, we used high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) and pre-column online ortho-phthalaldehyde (OPA) derivatization-based amino acid analysis by HPLC with diode array detection and fluorescence detection to identify and quantify free amino acids released upon oxidation of proteins and peptides by hydroxyl radicals. Bovine serum albumin (BSA), ovalbumin (OVA) as model proteins, and synthetic tripeptides (comprised of varying compositions of the amino acids Gly, Ala, Ser, and Met) were used for reactions with hydroxyl radicals, which were generated by the Fenton reaction of iron ions and hydrogen peroxide. The molar yields of free glycine, aspartic acid, asparagine, and alanine per peptide or protein varied between 4 and 55%. For protein oxidation reactions, the molar yields of Gly (∼32-55% for BSA, ∼10-21% for OVA) were substantially higher than those for the other identified amino acids (∼5-12% for BSA, ∼4-6% for OVA). Upon oxidation of tripeptides with Gly in C-terminal, mid-chain, or N-terminal positions, Gly was preferentially released when it was located at the C-terminal site. Overall, we observe evidence for a site-selective formation of free amino acids in the OH radical-induced oxidation of peptides and proteins, which may be due to a reaction pathway involving nitrogen-centered radicals.
Magura Cave, north-western Bulgaria, possesses valuable rock-art paintings made with bat guano and dated from the period between the Eneolithic and Bronze Ages. Since 2008, the Art Gallery is closed to the general public in order to protect the paintings from vandalism, microclimatic changes caused by visitors and artificial illumination, and the consequent growth of fungi and phototrophs. Nevertheless, some tourist visits are allowed under the supervision of cave managers. This study provides the first scientific report on cultivable fungal assemblages dwelling different substrata in the Art Gallery. A total of 78 strains, belonging to 37 OTUs (Ascomycota 81%, Zygomycota 13%, Basidiomycota 5%), were isolated in the study. This fungal diversity was clearly dominated by Penicillium (50% of strains) and Aspergillus (13%). The most relevant visible fungal colonies were detected in sediments rich in bat guano, where, besides Penicillium, other guanophilic fungi such as Mucor, Mortierella, Trichosporon and Trichoderma were dominant. Conversely, scarce fungi were detected on rock surface of painted walls. Based on the biocide susceptibility assay, octylisothiazolinone (OIT) and benzalkonium chloride (BAC) were effective inhibiting the in vitro growth of dominant fungal species in Magura Cave, when applied at concentrations ranged from 100 to 1,000 mg/L. These data provide a valuable knowledge about Magura fungi, and exemplify a type of preliminary test that may be conducted before planning any biocide treatment. However, considering the irreversible effects of biocides on the ecological balance in caves, and the low fungal contamination in painted walls of Magura Cave, there is no reason to use conventional biocides in this cave. Further studies, monitoring microbial communities and microclimatic parameters, should be conducted to improve the knowledge on microbial ecology in Magura Cave and possible human impacts, as well as to allow the early detection of potential microbial outbreaks.
A facile method to probe the vascular permeability of nanoparticles in nanomedicine applications
(2017)
The effectiveness of nanoparticles (NP) in nanomedicine depends on their ability to extravasate from vasculature towards the target tissue. This is determined by their permeability across the endothelial barrier. Unfortunately, a quantitative study of the diffusion permeability coefficients (Pd) of NPs is difficult with in vivo models. Here, we utilize a relevant model of vascular-tissue interface with tunable endothelial permeability in vitro based on microfluidics. Human umbilical vein endothelial cells (HUVECs) grown in microfluidic devices were treated with Angiopoietin 1 and cyclic adenosine monophosphate (cAMP) to vary the Pd of the HUVECs monolayer towards fluorescent polystyrene NPs (pNPs) of different sizes, which was determined from image analysis of their fluorescence intensity when diffusing across the monolayer. Using 70 kDa dextran as a probe, untreated HUVECs yielded a Pd that approximated tumor vasculature while HUVECs treated with 25 μg/mL cAMP had Pd that approximated healthy vasculature in vivo. As the size of pNPs increased, its Pd decreased in tumor vasculature, but remained largely unchanged in healthy vasculature, demonstrating a trend similar to tumor selectivity for smaller NPs. This microfluidic model of vascular-tissue interface can be used in any laboratory to perform quantitative assessment of the tumor selectivity of nanomedicine-based systems.
Development of theranostic concepts that include inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS (LA-ICP-MS) imaging can be hindered by the lack of a direct comparison to more standardly used methods for in vitro and in vivo evaluation; e.g. fluorescence or nuclear medicine. In this study a bimodal (or rather, hybrid) tracer that contains both a fluorescent dye and a chelate was used to evaluate the existence of a direct link between mass spectrometry (MS) and in vitro and in vivo molecular imaging findings using fluorescence and radioisotopes. At the same time, the hybrid label was used to determine whether the use of a single isotope label would allow for MS-based diagnostics.
The excitation of localized surface plasmons in noble metal nanoparticles (NPs) results in different nanoscale effects such as electric field enhancement, the generation of hot electrons and a temperature increase close to the NP surface. These effects are typically exploited in diverse fields such as surface-enhanced Raman scattering (SERS), NP catalysis and photothermal therapy (PTT). Halogenated nucleobases are applied as radiosensitizers in conventional radiation cancer therapy due to their high reactivity towards secondary electrons. Here, we use SERS to study the transformation of 8-bromoadenine (8BrA) into adenine on the surface of Au and AgNPs upon irradiation with a low-power continuous wave laser at 532, 633 and 785 nm, respectively. The dissociation of 8BrA is ascribed to a hot-electron transfer reaction and the underlying kinetics are carefully explored. The reaction proceeds within seconds or even milliseconds. Similar dissociation reactions might also occur with other electrophilic molecules, which must be considered in the interpretation of respective SERS spectra. Furthermore, we suggest that hot-electron transfer induced dissociation of radiosensitizers such as 8BrA can be applied in the future in PTT to enhance the damage of tumor tissue upon irradiation.
Distributed measurement of humidity is a sought-after capability for various fields of application, especially in the civil engineering and structural health monitoring sectors. This article presents a method for distributed humidity sensing along polymethyl methacrylate (PMMA) polymer optical fibers (POFs) by analyzing wavelength-dependent Rayleigh backscattering and attenuation characteristics at 500 nm and 650 nm wavelengths. Spatially resolved humidity sensing is obtained from backscatter traces of a dual-wavelength optical time domain reflectometer (OTDR). Backscatter dependence, attenuation dependence as well as the fiber length change are characterized as functions of relative humidity. Cross-sensitivity effects are discussed and quantified. The evaluation of the humidity-dependent backscatter effects at the two wavelength measurements allows for distributed and unambiguous measurement of relative humidity. The technique can be readily employed with low-cost standard polymer optical fibers and commercial OTDR devices.
This article reports on the characterization of four superparamagnetic iron oxide nanoparticles stabilized with dimercaptosuccinic acid, which are suitable candidates for reference materials for magnetic properties. Particles p1 and p2 are single-core particles, while p3 and p4 are multi-core particles. Small-angle X-ray scattering analysis reveals a lognormal type of size distribution for the iron oxide cores of the particles. Their mean radii are 6.9 nm (p1), 10.6 nm (p2), 5.5 nm (p3) and 4.1 nm (p4), with narrow relative distribution widths of 0.08, 0.13, 0.08 and 0.12. The cores are arranged as a clustered network in the form of dense mass fractals with a fractal dimension of 2.9 in the multi-core particles p3 and p4, but the cores are well separated from each other by a protecting organic shell. The radii of gyration of the mass fractals are 48 and 44 nm, and each network contains 117 and 186 primary particles, respectively. The radius distributions of the primary particle were confirmed with transmission electron microscopy. All particles contain purely maghemite, as shown by X-ray absorption fine structure spectroscopy
Ti-6Al-4V bridges were additively fabricated by selective laser melting (SLM) under different scanning speed conditions, to compare the effect of process energy density on the residual stress state. Subsurface lattice strain characterization was conducted by means of synchrotron diffraction in energy dispersive mode. High tensile strain gradients were found at the frontal surface for samples in an as-built condition. The geometry of the samples promotes increasing strains towards the pillar of the bridges. We observed that the higher the laser energy density during fabrication, the lower the lattice strains. A relief of lattice strains takes place after heat treatment.
In granular soils, long-term cyclically loaded structures can lead to an accumulation of irreversible strain by forming closed convective cells in the upper layer of the bedding. The size of the convective cell, its formation and grain migration inside this closed volume have been studied with reference to different stiffness of the embedded structure and different maximum force amplitudes applied at the head of the structure.
This relation was experimentally investigated by applying a cyclic lateral force to a scaled flexible vertical element embedded in a dry granular soil. The model was monitored with a camera in order to derive the displacement field by means of the PIV technique. Furthermore, the ratcheting convective cell was also simulated with DEM with the aim of extracting some micromechanical information. The main results regarded the different development, shape and size of the convection cell and the surface settlements.
A controlled, reproducible, gram-scale method is reported for the covalent functionalization of graphene Sheets by a one-pot nitrene [2+1] cycloaddition reaction under mild conditions. The reaction between commercially available 2,4,6-trichloro-1,3,5-triazine and sodium azide with thermally reduced graphene oxide (TRGO) results in defined dichlorotriazine-functionalized sheets. The different reactivities of the chlorine substituents on the functionalized graphene allow stepwise post-modification by manipulating the temperature.
This new method provides unique access to defined bifunctional 2D nanomaterials, as exemplified by chiral surfaces and multifunctional hybrid architectures.
The duplex stainless steel 1.4062 (X2CrNiN22-2) is used as alternative material to austenitic stainless steels in the construction industry. The corrosion resistance of welded seams is influenced by the base material, the weld filler material, the welding process and also by the final surface treatment. The scale layer next to the weld seam can be removed by grinding, pickling, electro-polished or blasting depending on the application and the requested corrosion resistance. Blasted surfaces are often used in industrial practice due to the easier and cheaper manufacturing process compared to pickled or electro-polished surfaces. Furthermore blasting with corundum-grain is more effective than blasting with glass-beads which also lower the process costs. In recent years, stainless steel surfaces showed an unusually high susceptibility to pitting corrosion after grinding with corundum. For this reason, it is now also questioned critically whether the corrosion resistance is influenced by the applied blasting agent. This question was specifically investigated by comparing grinded, pickled, corundum-grain- and glass-bead-blasted welding seams. Results of the SEM analyses of the blasting agents and the blasted surfaces will be presented and correlated with the different performed corrosion tests (potential measurement, KorroPad-test and pitting potential) on welding seams with different surface treatments.
The novel heat treatment concept, “quenching and partitioning” (Q&P) has been developed for high strength steels with enhanced formability. This heat treatment involves quenching of austenite to a temperature between martensite start and finish, to receive a several amount of retained austenite. During the subsequent annealing treatment, the so called partitioning, the retained austenite is stabilized due to carbon diffusion, which results in enhanced formability and strength regarding strain induced austenite to martensite transformation. In this study a Q&P heat treatment was applied to a Fe-0.45C-0.65Mn-0.34Si-13.95Cr stainless martensite. Thereby the initial quench end temperature and the partitioning time were varied to characterize their influence on microstructural evolution. The microstructural changes were analysed by dilatometer measurements, X-ray diffraction and scanning electron microscopy, including electron backscatter diffraction. Compression testing was made to examine the mechanical behaviour. It was found that an increasing partitioning time up to 30 min leads to an enhanced formability without loss in strength due to a higher amount of stabilized retained and reversed austenite as well as precipitation hardening.
Water and aqueous reagents are essential in any biological process or system. But apart from a few special low vapor-pressure cases, liquids have not been accessible to any technique requiring UHV conditions. EnviroESCA opens up this exciting field of applications.
In this paper first results from water based samples are presented as a proof of concept to demonstrate the special capabilities of EnviroESCA analyzing liquid samples. The following solutions were investigated under near ambient pressure conditions: i.) water, ii.) brine, iii.) an oil in water dispersion, iv.) aqueous iron(II) sulfate heptahydrate, and v.) a suspension of nano silver particles in water.
An UCST-type copolymer of acrylamide (AAm) and acrylonitrile (AN) (poly(AAm-co-AN)) was prepared by reversible addition fragmentation chain transfer (RAFT) polymerization and its temperature-induced phase transition and aggregation behaviour studied by turbidimetry, static and dynamic light scattering, small angle neutron scattering (SANS) and cryo-transmission electron microscopy (cryo-TEM) measurements. The phase transition temperature was found to increase with increasing AN content in the copolymer, concentration of the solutions and copolymer chain length. A significant effect was observed onto the phase transition temperature by addition of different electrolytes into the copolymer solution. The copolymer chains were aggregated below the phase transition temperature and disaggregated above it. The size of the aggregates increases with increasing AN contents and concentration of the copolymer solutions below the phase transition temperature. The copolymer chains were expanded and weekly associated in solution above the phase transition temperature. A model is proposed to explain such association–aggregation behaviour of poly(AAm-co-AN) copolymers depending on AN contents and concentration of the copolymer solutions as a function of temperature.
The paper presents a new method for the determination and evaluation of tafel factors using gel-type electrolytes and electrochemical frequency modulation technique (EFM). This relatively new electrochemical method offers the possibility to determine both polarization resistances and tafel factors within one measurement and in short measuring intervals. Starting from a comprehensive parameter study it is shown that a direct relationship between the two values exists that can be described mathematically. This contribution presents the determined tafel factors for the system gel-type electrolyte/zinc and discusses their applicability and their limits.
The CCQM-K123 key comparison was organized by the Inorganic Analysis Working Group (IAWG) of CCQM to assess and document the capabilities of the national metrology institutes (NMIs) or the designated institutes (DIs) to measure the mass fractions of sodium, calcium, potassium, magnesium phosphorous and sulfur in biodiesel fuel (BDF). The National Metrology Institute of Japan (NMIJ) and National Institute of Standards and Technology (NIST) acted as the coordinating laboratories.
Results were submitted by 11 NMIs and DIs. The participants used different measurement methods, though most of them used inductively coupled plasma-mass spectrometry (ICP-MS), isotope dilution technique with ICP-MS and inductively coupled plasma-optical emission spectrometry (ICP-OES) with microwave acid digestion.
The material was quite challenging and a number of questions were raised at the IAWG meeting. Concerning S, the variation in S results between participants, particularly those using IDMS methods was discussed at the IAWG meeting. BAM, NIST and NMIJ reviewed their experimental conditions, results and/or uncertainty calculations for IDMS. According to the additional evaluation and investigation, the variances between the revised results became smaller than the original one, the revised results were overlapping between IDMS measurements of S content at the k=2 level. It is not possible to calculate a KCRV with values being modified after submission. It was concluded that this KC does not support S measurements.
Accounting for relative expanded uncertainty, comparability of measurement results for each of Na, Ca, K, Mg and P was successfully demonstrated by the participating NMIs or DIs. It is expected that sodium, calcium, potassium, magnesium and phosphorus at mass fractions greater than approximately 0.1 mg/kg, 0.1 mg/kg, 0.05 mg/kg, 0.05 mg/kg and 0.1 mg/kg respectively in biodiesel fuel and similar matrices (fuels and oils etc.) can be determined by each participant using the same technique(s) employed for this key comparison to achieve similar uncertainties mentioned in the present report. Furthermore, the results of this key comparison can be utilized along with the IAWG core capability approach.
This work demonstrates that phase-segregated poly(ester urethane) (PEU) with switching segments of crystallizable poly(1,4-butylene adipate) (PBA) can be programmed to generate two separate stress recovery events upon heating under constant strain conditions. For programming, two elongations are applied at different temperatures, followed by unloading and cooling. During the adjacent heating, two-step stress recovery is triggered. The results indicate that the magnitude of the stress recovery signals corresponds to the recovery of the two deformation stresses in reverse order. As demonstrated by further experiments, twofold stress recovery can be detected as long as the elongation at higher temperature exceeds the strain level of the deformation at lower temperature. Another finding includes that varying the lower deformation temperature enables a control over the stress recovery temperature and thus the implementation of so-called “temperature-memory effects”. Moreover, exerting only one elongation during programming enables a heating-initiated one-step stress recovery close to the deformation temperature. Based on these findings, such polymers may offer new technological opportunities in the fields of active assembly when used as fastening elements and in functional clothing when utilized for compression stockings.
Referee Report 06 March 2017
(2017)
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 possessing short set-up times. Here, we report on a fast and reliable calibration-free online NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement of 1H spectra with a time interval of 20 s per spectrum, and a robust, fully automated algorithm to interpret the obtained data. As a proof-of-concept, the thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was conducted in a variety of non-deuterated solvents while its time-resolved behaviour was characterized with step tracer experiments. Overlapping signals in online spectra during thiol-ene coupling could be deconvoluted with a spectral model using indirect hard modeling and were subsequently converted to either molar ratios (using a calibrationfree approach) or absolute concentrations (using 1-point calibration). For various solvents the kinetic constant k for pseudo-first order reaction was estimated to be 3.9 h-1 at 25 °C. The obtained results were compared with direct integration of non-overlapping signals and showed good agreement with the implemented mass balance.
Structural relaxation phenomena in binary and multicomponent lithium silicate glasses were studied upon irradiation with femtosecond (fs) laser pulses (800 nm central wavelength, 130 fs pulse duration) and subsequent thermal annealing experiments. Depending on the annealing temperature, micro-Raman spectroscopy analyses evidenced different relaxation behaviours, associated to bridging and non-bridging oxygen structures present in the glass network. The results indicate that the mobility of lithium ions is an important factor during the glass modification with fs-laser pulses. Quantitative phase contrast imaging (spatial light interference microscopy) revealed that these fs-laser induced structural modifications are closely related to local changes in the refractive index of the material. The results establish a promising strategy for tailoring fs-laser sensitivity of glasses through structural mobility.
Matrix-assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF MS) is a well-implemented analytical technique for the investigation of complex biological samples. In MS, the sample preparation strategy is decisive for the success of the measurements. Here, sample preparation processes and target materials for the investigation of different pollen grains are compared. A reduced and optimized sample preparation process prior to MALDI-TOF measurement is presented using conductive carbon tape as target. The application of conductive tape yields in enhanced absolute signal intensities and mass spectral pattern information, which leads to a clear separation in subsequent pattern analysis. The results will be used to improve the taxonomic differentiation and identification, and might be useful for the development of a simple routine method to identify pollen based on mass spectrometry.
This author interview is by Dr Michael G. Weller, Head of Division 1.5 Protein Analysis at Federal Institute for Materials Research and Testing (BAM). BAM (www.bam.de/en) is a senior scientific and technical institute with responsibility to the German Federal Ministry for Economic Affairs and Energy. Dr Weller's review paper, Quality issues of research antibodies is available for download in Analytical Chemistry Insights.
Immunoassays are suitable tools for high-throughput screenings. The prerequisite for accurate determinations by these methods is the selection of an excellent antibody. The production and selection of monoclonal antibodies is usually a tedious process. In this study, new strategies for improving antibody production and characterization were applied. This includes the monitoring of the immunization progress in mice through antibodies extracted from feces, which allows a time-resolved and animal-friendly monitoring of the immune response. Additionally, fluorescence polarization immunoassay (FPIA) could be successfully applied for fast and easy examination of cell culture supernatants and the investigation of antibody/antigen interactions including kinetics and fluorescence properties. These methods simplify the selection of the optimal antibody. As a target analyte, carbamazepine was chosen. This is a widely used antiepileptic drug which also frequently occurs in the environment. The new antibody enables CBZ determination in the concentration range 0.66–110 µg L-1 within 10 min using a high-throughput microtiter plate-based FPIA, and between 1.4 and 79 µg L-1 within 5 min applying an automated cuvette-based FPIA instrument, and from 0.05–36 µg L-1 using ELISA. The measurements were performed at a non-equilibrium state which improved the sensitivity and selectivity of the assays. Due to low cross-reactivity especially towards the main CBZ metabolite and other pharmaceuticals (<1%), this antibody gives the opportunity for application in medical and environmental analyses.
This article provides an impression on potentials in applying nowadays welding simulation tools in construction design. This is carried out exemplary on plate girders from two structural steel grades. The calculated residual stresses are compared with measurements by sectioning method. It has been repeatedly stated that present Eurocode models fail to approximate the residual stresses. Especially for high strength steel (HSS) only limited information is available on realistic occurring residual stresses in typical I-girders. The investigations are aimed to give further guidance on these values. A few proposals on advanced models are discussed.
In the quest for finding the ideal synchrotron-radiation-induced imaging method for the investigation of trace element distributions in human bone samples, experiments were performed using both a scanning confocal synchrotron radiation micro X-ray fluorescence (SR-mXRF) (FLUO beamline at ANKA) setup and a full-field color X-ray camera (BAMline at BESSY-II) setup. As zinc is a trace element of special interest in bone, the setups were optimized for its detection. The setups were compared with respect to count rate, required measurement time and spatial resolution. It was demonstrated that the ideal method depends on the element of interest. Although for Ca (a major constituent of the bone with a low energy of 3.69 keV for its K alpha XRF line) the color X-ray camera provided a higher resolution in the plane, for Zn (a trace element in bone) only the confocal SR-µXRF setup was able to sufficiently image the distribution.
Investigation of manuscripts found in sites along the Silk Road shows the history of communication and exchange between Asia and the Mediterranean over the centuries. Different scripts and languages preserved on paper in certain styles provide information about traditions and provenance.
To get an idea of the cultural background of the highly developed painting techniques obvious in some illuminated manuscripts, the material used for writing and painting is analyzed. Singular Sogdian and Tocharian manuscripts from Turfan show text on one side with a colorful painting on the other side of the document. In comparison with other productions of different periods or usages from the site, special features are worked out to characterize cultural roots or influence in the network of relationships. Details analyzed in the most elaborated documents Show various influences led to the colorful masterpieces.
Designing artificial macromolecules with absolute sequence order represents a considerable challenge. Here we report an advanced light-induced avenue to monodisperse sequencedefined functional linear macromolecules up to decamers via a unique photochemical approach. The versatility of the synthetic strategy—combining sequential and modular concepts—enables the synthesis of perfect macromolecules varying in chemical constitution and topology. Specific functions are placed at arbitrary positions along the chain via the successive addition of monomer units and blocks, leading to a library of functional homopolymers, alternating copolymers and block copolymers. The in-depth characterization of each sequence-defined chain confirms the precision nature of the macromolecules. Decoding of the functional information contained in the molecular structure is achieved via tandem mass spectrometry without recourse to their synthetic history, showing that the sequence information can be read.We submit that the presented photochemical strategy is a viable and advanced concept for coding individual monomer units along a macromolecular chain.
Reliable nanomaterial classification of powders using the volume-specific surface area method
(2017)
The volume-specific surface area (VSSA) of a particulate material is one of two apparently very different metrics recommended by the European Commission for a definition of "nanomaterial" for regulatory purposes: specifically, the VSSA metric may classify nanomaterials and non-nanomaterials differently than the median size in number metrics, depending on the chemical composition, size, polydispersity, shape, porosity, and aggregation of the particles in the powder.
Here we evaluate the extent of agreement between classification by electron microscopy (EM) and classification by VSSA on a large set of diverse particulate substances that represent all the anticipated challenges except mixtures of different substances. EM and VSSA are determined in multiple labs to assess also the level of reproducibility. Based on the results obtained on highly characterized benchmark materials from the
NanoDefine EU FP7 project, we derive a tiered screening strategy for the purpose of implementing the definition of nanomaterials. We finally apply the Screening strategy to further industrial materials, which were classified correctly and left only borderline cases for EM.
On platelet-shaped nanomaterials, VSSA is essential to prevent false-negative classification by EM. On porous materials, approaches involving extended Adsorption isotherms prevent false positive classification by VSSA. We find no false negatives by VSSA, neither in Tier 1 nor in Tier 2, despite real-world industrial polydispersity and diverse composition, shape, and coatings. The VSSA screening strategy is recommended for inclusion in a technical guidance for the implementation of the definition.
Halophilic bacteria use a variety of osmoregulatory methods, such as the accumulation of one or more compatible solutes. The wide diversity of compounds that can act as compatible solute complicates the task of understanding the different strategies that halophilic bacteria use to cope with salt. This is specially challenging when attempting to go beyond the pathway that produces a certain compatible solute towards an understanding of how the metabolic network as a whole addresses the problem. Metabolic reconstruction based on genomic data together with Flux Balance Analysis (FBA) is a promising tool to gain insight into this problem. However, as more of these reconstructions become available, it becomes clear that processes predicted by genome annotation may not reflect the processes that are active in vivo. As a case in point, E. coli is unable to grow aerobically on citrate in spite of having all the necessary genes to do it. It has also been shown that the realization of this genetic potential into an actual capability to metabolize citrate is an extremely unlikely event under normal evolutionary conditions. Moreover, many marine bacteria seem to have the same pathways to metabolize glucose but each species uses a different one. In this work, a metabolic network inferred from genomic annotation of the halophilic bacterium Halomonas elongata and proteomic profiling experiments are used as a starting point to motivate targeted experiments in order to find out some of the defining features of the osmoregulatory strategies of this bacterium. This new information is then used to refine the network in order to describe the actual capabilities of H. elongata, rather than its genetic potential.
Electron Beam Melting (EBM) as a means of Additive Manufacturing (AM), is of interest for the fabrication of intricate geometries for cellular materials in areas where complex architectures are needed, e.g. biomedical implants. Most studies have focused on specific geometries and so the effect of the structure on mechanical performance is not well understood. Many kinds of micro- and macro-scale defects can arise in additively manufactured components, so assessment of their influence on properties is needed. In this work, lattices of Ti-6Al-4V having a cubic structure have been manufactured by EBM, and the effect of heat treatments above and below the β-transus temperature on microstructure and compression response have been investigated. The former modifies only slightly the α + β structure and mechanical performance whereas the latter leads to coarse alternating α and β lamellae packets and α at the prior grain boundaries with a 10% loss in yield strength. The variation in the compressive yield stress with strut diameter is in good accord with simple models based on compressive deformation rather than shearing or buckling. Internal pores for struts aligned with the build direction are found around the edges of the solid form, in regions which seem to be associated with the EB scan pattern. Struts normal to the build direction show more significant defects but their redundancy means that they do not compromise the compressive performance in the build direction. Using a particle size in the range 45–100 μm minimum weld-track sizes were experimentally and numerically identified to be 176 and 148 μm in depth respectively with a depth-to-width ratio of 0.55. This produced a beam pass of the order of 300 μm oversizing small features (struts of 0.4 and 0.6 mm nominal diameter) when a contour around the strut periphery was applied.
Experimental and phase field studies of age hardening response of a high purity Al‐4Cu‐1Li‐0.25Mn‐alloy (mass %) during isothermal aging are conducted. In the experiments, two hardening phases are identified: the tetragonal θ′ (Al₂Cu) phase and the hexagonal T1 (Al₂CuLi) phase. Both are plate shaped and of nm size. They are analyzed with respect to the development of their size, number density and volume fraction during aging by applying different analysis techniques in TEM in combination with quantitative microstructural analysis. 3D phase‐field simulations of formation and growth of θ′ phase are performed in which the full interfacial, chemical and elastic energy contributions are taken into account. 2D simulations of T1 phase are also investigated using multi‐component diffusion without elasticity. This is a first step toward a complex phase‐field study of T1 phase in the ternary alloy. The comparison between experimental and simulated data shows similar trends. The still unsaturated volume fraction indicates that the precipitates are in the growth stage and that the coarsening/ripening stage has not yet been reached.
Today’s efforts for lightweight design result in a growing application of high-strength structural steels from 960 MPa. In welded structures of these steels increased demands regarding component safety and a high elastic ratio should be considered. Hence, the prevention of an evolution of high weld-induced tensile residual stresses is required. Recent studies showed that component related restraint conditions of welds are able to elevate welding induced stresses to critical values, depending on material characteristics, the welding process and parameters. This work involves multi-axial welding loads as a consequence of the superposition of local residual stresses, global reaction stresses and moments, varying the welding parameters under different restraint conditions. The global welding loads are measured via GMA-weld tests in a special testing facility and via a DIC(Digital Image Correlation)-system in a slot weld. Local transverse residual stresses were analysed by means of X-ray diffraction. The application of a less amount of weld runs due to a modified welding parameters and welds seam configurations revealed as a beneficial approach to reduce welding loads in high-strength steels.
Welding is the most important joining technology. In the steel construction
industry, e.g. production of windmill sections, welding accounts for a
main part of the manufacturing costs and resource consumption. Moreover, social
issues attached to welding involve working in dangerous environments. This aspect
has unfortunately been neglected so far, in light of a predominant focus on economics
combined with a lack of suitable assessment methods. In this chapter,
exemplary welding processes are presented that reduce the environmental and
social impacts of thick metal plate welding. Social and environmental Life Cycle
Assessments for a thick metal plate joint are conducted for the purpose of
expressing and analysing the social and environmental impacts of welding.
Furthermore, it is shown that state-of-the-art technologies like Gas Metal Arc
Welding with modified spray arcs and Laser Arc-Hybrid Welding serve to increase
social and environmental performance in contrast to common technologies, and
therefore offer great potential for sustainable manufacturing.
We report on a study in which plasmid DNA in water was irradiated with 30 keV electrons generated by a scanning electron microscope and passed through a 100 nm thick Si3N4 membrane. The corresponding Monte Carlo simulations suggest that the kinetic energy spectrum of the electrons throughout the water is dominated by low energy electrons (<100 eV). The DNA radiation damage, single-strand breaks (SSB) and double-strand breaks (DSB), was determined by electrophoresis. The median lethal dose of D1/2 = 1.7 ± 0.3 Gy was found to be much smaller compared to partially or fully hydrated DNA irradiated under vacuum conditions. The ratio of DSB to SSB was found to be (1:12) as compared to 1:88) found for hydrated DNA. Our method enables quantitative measurements of radiation damage to biomolecules (DNA, proteins) in solutions under varying conditions (pH, salinity, cosolutes) for an electron energy range which is difficult to probe by standard methods.
We report on calibration standards of nanoparticles meeting the definition of a nanomaterial given by the European Commission (EU 2011) which are relevant for the characterisation methods applied in the NanoDefine project. We found that the Impact of nanoparticles is outstanding in the scientific literature. A number of 270.000 paper titles on nanoparticles are listed in the Web of Science data base. But surprisingly, the availability of suitable certified standard reference materials is scarce. Only a few sources were found. For example, BAM provides the database Nanoscaled Reference Materials at http://www.nano-refmat.bam.de/en/ in cooperation with the ISO/TC 229 Nanotechnologies. In addition, two publications from 2013 on nanoscale reference materials are available. Candidates of nano-(certified) reference materials from other ongoing or just finished FP6 and FP7 nano-metrology projects have been extracted from the Compendium of Projects in the European NanoSafety Cluster (Compendium NSC, 2013). Recommendations for selection of representative test materials and calibration standards for NanoDefine internal tasks, respectively, are also given.
The EU FP7 NanoDefine project was launched in November 2013 and will run until October 2017. The Project is dedicated to support the implementation of the EU Recommendation on the Definition of Nanomaterial
by the provision of the required analytical tools and respective guidance. Main goal is to develop a novel
tiered approach consisting of (i) rapid and cost-efficient screening methods and (ii) confirmatory measurement
methods. The "NanoDefiner" eTool will guide potential end-users, such as concerned industries and regulatory bodies as well as enforcement and contract laboratories, to reliably classify if a material is nano or not. To achieve this objective, a comprehensive inter-laboratory evaluation of the performance of current
characterisation techniques, instruments and software is performed. Instruments, software and methods are
further developed. Their capacity to reliably measure the size of particulates in the size range 1-100 nm and
above (according to the EU definition) is validated. Technical reports on project results are published to
reach out to relevant stakeholders, such as policy makers, regulators, industries and the wider scientific community, to present and discuss our goals and results, to ensure a continuous exchange of views,
needs and experiences obtained from different fields of expertise and application, and to finally integrate the resulting feedback into our ongoing work on the size-related classification of nanomaterials.
The content of the paper is the assessment of the performance of (conventional) measurement techniques (MTs)with respect to the classification of disperse materials according to the EC recommendation for a definition of nanomaterial. This performance essentially refers to the accurate assessment of the number weighted median of (the constituent) particles. All data and conclusions are based on the analytical study conducted as real-world performance testing.
It comprised different types of MTs (imaging, counting, fractionating, spectroscopic and integral) as well as different types of materials. Beside reference materials with well-defined size distribution the study also included several commercial powders (variation of particle composition, morphology, coating, size range and polydispersity). In order to ensure comparability of measurement results, the participants were guided to use uniform protocols in sample preparation, conducting measurements, data analysis and in reporting results. Corresponding documents have been made public, in order to support the reviewing process of the paper, respectively to ensure the reproducibility of data by other users under the same conditions.
The scientific paper relies on a comprehensive set of revised measurement data reported in uniform templates, completely describes the experimental procedures and discusses the MTs’ performance for selected materials in detail. Even more, the study is summarised and evaluated, which leads to recommendations for the use of MTs within a tiered approach of NM characterisation. In addition, the paper critically examines the factors that may affect the outcome of such a comparison among different MTs.
The current paper presents residual stress analyses of large scale LTT (Low Transformation Temperature) welds. LTT filler materials are specially designed for residual stress engineering by means of an adjusted martensite phase transformation. Controlling the level of mostly detrimental residual stresses already during the welding process would be highly attractive as time and cost consuming post processing may be prevented. In large scale welds the residual stress state is influenced by the heat control (e.g. interpass temperature) during welding. Therefore, welding residual stresses are studied here putting the focus on the influence of welding process parameters while joining heavy steel sections with a thickness of 25 mm. The residual stress state was determined at the top surface using X-ray diffraction as well as in the bulk by neutron diffraction. The results show that control of the interpass temperature is vital for the residual stresses present in the joints. This accounts for the top surface but is most pronounced for the bulk of the welds. While high interpass temperatures are appropriate to induce compressive residual stresses in the weld metal, low interpass temperatures favor unwanted tensile residual stresses instead.
This report is the result of a comprehensive study on the available CMs which come potentially in question for the reliable analysis of the number based size distribution of a nanomaterial according to the EC recommendation for a definition of nanomaterial. Based on the performance criteria already established in NanoDefine the potential CMs are evaluated according to studies available in the literature as well as following the expertise of the NanoDefine consortium partners. The specific advantages and disadvantages of each method with respect to its applicability to the scope of NanoDefine are particularly highlighted. An CM evaluation table is produced so that the mostly suited CMs with respect to the EC definition can be grouped and recommended to the corresponding NanoDefine work packages for further specific development (improvement and adaption), or for direct validation and standardisation, respectively. The actual evaluation report including the recommended CMs will be revised and, if necessary, eventually updated at the mid time of the project. The update will be jointly discussed in the NanoDefine consortium on the basis of the results of testing the methods on the NanoDefine real world materials.
We propose the use of alternating pulse wavelengths in a direct-detection coherent optical time domain reflectometry (C-OTDR) setup not only to measure strain and temperature changes but also to determine the correct algebraic sign of the change. The sign information is essential for the intended use in distributed mode shape analysis of civil engineering structures. Correlating relative backscatter signal shifts in the temporal/signal domain allows for measuring with correct magnitude and sign. This novel approach is simulated, experimentally implemented and demonstrated for temperature change measurement at a spatial resolution of 1 m.
Carbon arc-air gouging is a common technology when repairing defects in welded structures. Often this technique is applied in repeated cycles even on the same location of the joint. Due to the multiple heat input by gouging and subsequent re-welding, the residual stresses are strongly influenced. This can become crucial when microstructure and mechanical properties are adversely affected by multiple weld reparations. Knowledge about the relation of gouging and residual stresses is scarce but important when high strength steels, which are sensitive to residual stresses, are processed. The present study shows the effect of repair welding on a high strength steel structural element. The weld and the heat affected zone were subjected to multiple thermal cycles by gouging and subsequent repair welding. The residual stresses were determined by X-ray diffraction at different positions along the joint. The results showed that the residual stress level has increased by the repair cycles. This is most pronounced for the heat affected zone. Adapted welding procedures may prevent detrimental residual stress distributions.
The nonlinear analysis became a common tool to precisely assess the load-bearing behavior of steel beam and column members. The failure level is significantly influenced by different types of imperfections, among geometric also structural imperfections (residual stresses). Here are still gaps in the knowledge. Nowadays, 3-D welding simulation developed to a level where it could provide reliable estimation of weld-induced distortion and residual stresses. Nevertheless, modelling and computational effort are still in a less practicable range. In this study a simplified procedure to implement residual welding stresses in continuous large scale members is proposed and the influence on the ultimate limit state of slender members in compression is evaluated for two common structural steel grades. The results showed significant improvements in the utilization of load bearing capacity compared with simplified design methods. The comparatively general approach in this study offers
potential for future optimization.
Residual stresses and distortions in welded I-girders for steel construction are relevant when evaluating the stability of steel beams and column members. The application of high strength steels allows smaller wall thicknesses compared to conventional steels. Therefore, the risk of buckling has to be considered carefully. Due to the lack of knowledge concerning the residual stresses present after welding in high strength steel components conservative assumptions of their level and distribution is typically applied. In this study I-girders made of steels showing strengths of 355 MPa and 690 MPa were welded with varying heat input. Due to the dimension of the I-girders and the complex geometry the accessibility for residual stress measurement using X-ray diffraction was limited. Therefore, saw cutting accompanied by strain gauge measurement has been used to produce smaller sections appropriate to apply X-ray diffraction. The stress relaxation measured by strain gauges has been added to residual stresses determined by X-ray diffraction to obtain the original stress level and distribution before sectioning. The combination of both techniques can produce robust residual stress values. From practical point of view afford for strain gauge application can be limited to a number of measuring positions solely to record the global amount of stress relaxation. X-ray diffraction can be applied after sectioning to determine the residual stresses with sufficient spatial resolution.
The detection and characterization of surface cracks in steel specimens prior to damage is a technologically and economically highly significant task and is of utmost importance when it comes to safety-relevant structures. In steel production where steel billets at high temperatures have to be inspected while moving a number of well-established NDT methods cannot be applied. Laser thermography however is a promising candidate to serve as a fast, non-contact and remote tool in this case. We present a study that shows that the crack detection capabilities of laser thermography can be extended also to specimens at high temperature. A combination of inductive and laser heating allows to systematically study the contrast formation as well as the optimization of the important measurement parameters. The experiments are accompanied by FEM simulations that provide a better insight of the physical correlations and support the experimental developments. The aim of these studies is to develop a system with high inspection speed and detection performance to be in-line operated under the hostile environment of steel production lines.
In this study, the feasibility of using non-contact Infrared thermography as a potential tool to monitor the CMT welding process is explored. The presence of internal defects such as porosity, lack of filler material deposition and formation of improper weld bead produce perturbations in the surface temperature which can be identified using an Infrared thermography technique. We present recent results obtained from online monitoring of the the dissimilar joining using CMT weld brazing of Aluminum and Steel using a transmission mode measurement approach. The effect of loss of zinc coating on the weldability of the cold metal transfer joining of aluminum to galvanised steel was investigated. A correlation between measured online thermal indications with the weld anomalies is successfully attempted and the results are compared with the conventional post-weld NDT inspection methods.
A permanent-magnet synchronous motor (PMSM) servo drive for lightweight robotic platforms that have a high torque demand at low rotational speeds has been developed. First, a current-independent torque controller is derived and cascaded with a speed and position controller, while merely an encoder is used as a sensor device in combination with a speed estimator. Finally, the speed estimator output is compared to gyroscope measurements and the overall functioning is verified on a real system.
A phosphaphenanthrene and triazinetrione group containing flame retardant (TAD) is combined with organically modified montmorillonite (OMMT) in epoxy resin thermosets (EP) to improve the performance of the flame-retardant system. When only 1 wt% OMMT/4 wt% TAD is introduced into the EP, the limited oxygen index (LOI) rises from 26% to 36.9% and a V-0 rating is achieved in a UL 94 test. The decomposition and pyrolysis products in the gas phase and condensed phase were characterized using thermogravimetry-Fourier transform infrared spectroscopy (TG-FTIR). The influence on the decomposition of EP, such as the increase in char yield, is limited with the incorporation of OMMT; a large amount of the phosphorus is released into the gas phase. The flame-retardant effect evaluation based on cone calorimeter data testified that OMMT improves the protective-barrier effect of the fire residue of OMMT/TAD/EP on the macroscopic scale, while TAD mainly causes flame inhibition. The fire residues showed a corresponding macroscopic appearance (digital photo) and microstructure (scanning electron microscope [SEM] results). The protective barrier effect of OMMT and the flame-inhibition effect of TAD combined to exert a superior flame-retardant effect, resulting in sufficient flame-retardant performance of OMMT/TAD/EP
A high-performance fiber Bragg grating-based (FBG) sensor device has been developed for the detection of small magnetic fields. Based on a smart multilayer jacket around the fibre over the physical length of the FBG, magnetic fields generated by rotating machine parts, power generators or power cable can be easily detected, analysed and evaluated. Consequently, this innovative, on-line and non-contact inspection method results in an increase in quality and reliability of high-performing machine parts, devices and cables. The basic physical principle is based on a magnetostrictive multilayer system that strains the high-resolution FBG element in presence of magnetic fields. Subsequently, a fixed relationship between induced magnetic field and wavelength change of the FBG element describes the characteristic sensitivity curve. Intensive tests regarding characterisation of this magnetic field FBG sensor have been carried out and its performance has been evaluated.
IND15 JRP SurfChem: Traceable quantitative surface chemical analysis for industrial applications
(2016)
The SurfChem project has made a significant contribution to traceable quantitative surface chemical analysis for industrial applications by delivering new certified reference materials and test samples for specific technical applications. Regular performance tests of instruments, metrological methodology for the detection of (bio)organic surface species, ambient and non-destructive surface chemical analysis for in-line process control and new in situ characterisation techniques of catalytically active surfaces have been achieved.
Materials and chemical producers require detailed knowledge of surface chemistry for research into new products. One way to understand a surface without damaging it is to bombard it with an electron beam, causing its atoms to emit characteristic X-rays enabling identification. The measurement of these must be precise as many elements emissions are close in energy – traceable reference materials will ensure instruments using this technique are stable and accurate.
Ultrasonic imaging systems usually require an array of ultrasonic transducers for data acquisition on a wide area on top of an object under investigation. The goal of an imaging algorithm is the use of reflected ultrasound data to form a recognizable image. Conventional algorithms like SAFT are based on an inverse Huygens' principle and need therefore a dense measurement grid. This requires a big effort in data capturing. For simple and inexpensive measurement different strategies of imaging with reduced amount of data and examples with a manual scanning device on concrete elements are presented.
Online monitoring and process control requires fast and noninvasive analytical methods, which are able to monitor the concentration of reactants in multicomponent mixtures with parts-per-million resolution. Online NMR spectros-copy can meet these demands when flow probes are directly coupled to reactors, since this method features a high linearity between absolute signal area and sample concentration, which makes it an absolute analytical com-parison method being independent on the matrix. Due to improved magnet design and field shimming strategies portable and robust instruments have been introduced to the market by several manufacturers during the last few years. First studies with this technology showed promising results to monitor chemical reaction in the laboratory.
In this work, fullerene has been functionalized with cyanuric Chloride at room temperature by a nitrene mediated [2 + 1] cycloaddition reaction. The adduct after functionalization is inherently in the form of azafulleroid and shows broad UV absorption in the wavelength range of 200–800 nm, as well as photothermal conversion and fluorescence with a high quantum yield.
A novel photoswitchable rotaxane was synthesised and its switching behaviour in solution was analysed with NMR and UV-Vis. A monolayer of rotaxanes was deposited on glass surfaces and the on-surface photoswitching was investigated. Angle-resolved NEXAFS spectra revealed a preferential orientation that reversibly changes upon switching.
Healable materials could play an important role in reducing the environmental footprint of our
modern technological society through extending the life cycles of consumer products and constructions. However, as most healing processes are carried out by heat alone, the ability to heal damage generally kills the parent material’s thermal and mechanical properties. Here we
present a dynamic covalent polymer network whose thermal healing ability can be switched ‘on’ and ‘off’ on demand by light, thereby providing local control over repair while retaining the advantageous macroscopic properties of static polymer networks. We employ a photoswitchable furan-based crosslinker, which reacts with short and mobile maleimidesubstituted poly(lauryl methacrylate) chains forming strong covalent bonds while simultaneously allowing the reversible, spatiotemporally resolved control over thermally induced de- and re-crosslinking. We reason that our system can be adapted to more complex materials and has the potential to impact applications in responsive coatings, photolithography and microfabrication.
Immuno imaging by the use of Laser Ablation Inductively Coupled Mass Spectrometry (LA-ICP-MS) is a growing research field in life sciences such as biology and biomedicine. Various element labeling strategies for antibodies have been developed for the application of multiplex immunoassays analyzed by the use of LA-ICP-MS. High multiplexing capabilities, a wide linear dynamic range and the possibility of absolute quantification are the main advantages of ICP-MS. But in the context of immuno imaging by the use of LA-ICP-MS, quantification of analytes is limited due to non-controllable antibody labeling chemistry. In the presented proof-of-principle a novel antibody labeling technique has been investigated which results in a controlled labeling degree. A small affinity protein based on the C2 domain of protein G was modified with conventional metal coded tags (MeCAT) after introducing a cysteine into the C-terminus of the protein. The modified C2 domain photo-crosslinks to the Fc or Fab region of the IgG and allows specific and covalent labeling of antibodies for multiplex immunoassay analysis by the use of LA-ICP-MS. In combination with a house-made calibration membrane the amount of labeled antibody–antigen complexes in a multiplex western blot immunoassay was determined by LA-ICP-MS.
Boehmite nanoparticles show great potential in improving mechanical properties of fiber reinforced polymers. In order to predict the properties of nanocomposites, knowledge about the material parameters of the constituent phases, including the boehmite particles, is crucial. In this study, the mechanical behavior of boehmite is investigated using Atomic Force Microscopy (AFM) experiments and Molecular Dynamic Finite Element Method (MDFEM) simulations. Young’s modulus of the perfect crystalline boehmite nanoparticles is derived from numerical AFM simulations. Results of AFM experiments on boehmite nanoparticles deviate significantly. Possible causes are identified by experiments on complementary types of boehmite, that is, geological and hydrothermally synthesized samples, and further simulations of imperfect crystals and combined boehmite/epoxy models. Under certain circumstances, the mechanical behavior of boehmite was found to be dominated by inelastic effects that are discussed in detail in the present work.The studies are substantiated with accompanying X-ray diffraction and Raman experiments.
The crystal structures and syntheses of four different copper(II) phenylphosphonates, the monophenylphosphonates α-, β-, and γ-Cu(O3PC6H5)·H2O (α-CuPhPmH (1) β-CuPhPmH (2) and γ-CuPhPmH (3)), and the diphosphonate Cu(HO3PC6H5)2·H2O (CuPhP2mH (4)), are presented. The compounds were synthesized from solution at room temperature, at elevated temperature, under hydrothermal conditions, and mechanochemical conditions. The structures of α-CuPhPmH (1) and CuPhP2mH (4) were solved from powder X-ray diffraction data. The structure of β-CuPhPmH (2) was solved by single crystal X-ray analysis. The structures were validated by extended X-ray absorption fine structure (EXAFS) and DTA analyses. Disorder of the crystal structure was elucidated by electron diffraction. The relationship between the compounds and their reaction pathways were investigated by in situ synchrotron measurements.
Process monitoring of an intensified continuous production unit with compact NMR spectroscopy
(2016)
Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and relatively inexpensive analyzers, which feature advantages like low cost, low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, sufficient robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are cur-rently not available off the rack. Recently, promising benchtop NMR instruments with acceptable performance came to market and process integrated sensors developed on basis of such laboratory instruments are on their way.
Grating interferometric set-ups have been established in the last decade. They are promising candidates to obtain enhanced image contrast from weakly absorbing micro and nano structures. They are based on X-ray refraction and near-field diffraction using the Talbot effect.
At the expense of taking multiple images, Talbot-Lau grating interferometry allows separating the absorption, refraction, and scattering contributions by analysing the disturbances of a phase grating interference pattern. Contrary to other refraction enhanced methods, this technique can be applied using conventional X-ray tubes (divergent, polychromatic source). This makes it attractive to solve typical non-destructive testing problems.
We investigated the efficiency of phase gratings, i.e. the visibility (the amplitude of oscillations) upon variation of propagation distance and phase grating rotation around an axis parallel to the grid lines. This grating rotation changes the grating shape (i.e. the distributions of phase shifts). This can yield higher visibilities than derived from rectangular shapes.
Our study includes experimental results obtained from synchrotron radiation, as well as simulations for monochromatic radiation. The advantages of Talbot-Lau interferometry are demonstrated at the example of glass capillaries.
With increased usage of highly demanded, modern materials on safety
relevant parts (e.g. railway wheel sets, generator shafts, turbine disks, medical
implants, etc.) comprehensive analyses regarding the quality of the material are
requested. This gives a focus to non-destructive methods using ultrasound immersion
tank testing for classifying the degree of purity. Two autonomous standards,
ASTM E588 and SEP 1927, have been established for the definition, execution and
evaluation for this high resolution ultrasonic measurements on steel products.
The propagation of ultrasonic waves and the resulting sound field are strongly
dependent on the acoustical properties of the inspected material and the geometry
of probes and specimen. The definition of the measurement setup and the evaluation
methods appear to differ significantly in the given standards. ASTM E588 and
SEP 1927 prescribe the requirement for surface roughness and probe selection, are
using threshold based methods for cleanliness detection, but differ in computation
for the degree of purity. This has been the motivation for a comparison between
both standards with the main focus on amplitude depth dependency and overall spatial
resolution taking the influence of different material characteristics, geometry of
the specimen and sound fields into account.
A performance comparison between the use of non-focusing and focusing probes
respective to the threshold based detection will be presented in this contribution. In
addition, the usage of complex reconstruction algorithms (e.g. SAFT, echo tomography)
is compared with the traditional approaches of inclusion detection and
estimation of the degree of purity
Molybdenum disulfide (MoS₂) is a well-known solid lubricant for tribosystems running in vacuum or dry gases. Problems arise due to its sensitivity to humidity, which is a drawback for its application under ambient conditions. However, by using a physical vapor deposition (PVD) process, deposition parameters can be optimized not only to gain a coatings structure with favorable frictional properties but also to minimize the sensitivity to attack by water molecules. Therefore, an improved tribological behavior even under moist conditions can be achieved. MoS₂coatings are also candidates for being applied at cryogenic temperatures. They already have proven their suitability, e.g., for sliding support elements between superconducting magnets of the nuclear fusion-experiment Wendelstein 7-X. However, these coatings were exclusively produced for this particular application and the utilization for more common tribosystems may be precluded due to cost considerations. In view of a wider range of applications, pure and Cr containing PVD-MoS₂ coatings with an optimized structure were tested under varying environments including hydrogen gas and cryogenic temperatures. Results of the most promising variant are presented in this paper.