Filtern
Erscheinungsjahr
- 2017 (1827) (entfernen)
Dokumenttyp
- Vortrag (711)
- Zeitschriftenartikel (474)
- Posterpräsentation (329)
- Beitrag zu einem Tagungsband (246)
- Sonstiges (24)
- Buchkapitel (18)
- Beitrag zu einem Sammelband (7)
- Forschungsbericht (7)
- Tagungsband (Herausgeberschaft für den kompletten Band) (5)
- Dissertation (2)
Sprache
- Englisch (1827) (entfernen)
Schlagworte
- Nanoparticles (48)
- Fluorescence (42)
- Concrete (39)
- Corrosion (37)
- Nanoparticle (37)
- LIBS (26)
- XPS (25)
- Additive manufacturing (22)
- NDT (22)
- Quantum yield (22)
Eingeladener Vortrag
- nein (711)
In this thesis a protocol based on a direct competitive and non-competitive immunoassay using the microarray format was developed to screen emulated hybridoma supernatants against the drug carbamazepine (CBZ). As support, epoxy slides were manufactured by coating microscope glass slides with epoxy silanes. The manufactured epoxy slides showed similar capacity for protein immobilization as commercially available NEXTERION slides, but showed a higher autofluorescence background. On the epoxy slides, protein A, Cys-A, G and Cys-G were immobilized as antibody capturing coating. It could be shown that the Cys-tag considerably increased the immobilization of all compared proteins, especially of protein G. Protein Cys-G immobilized at pH 8-9 was considered the most suitable protein for antibody immobilization due to good spot uniformity and a high binding capacity for IgG. Additionally, in immobilization experiments it could be shown, that 10-500 fold excess of bovine IgG, introduced by two different fetal bovine serum (FBS) products, showed no significant competition on the immobilization of mice or goat IgG on protein Cys-G. To examine the captured antibodies for affinity to CBZ, the CBZ-TOTA-DY654 tracer was custom synthesized. It could be demonstrated, that the tracer antibody interaction was competitive with the tracer precursor, CBZ-TOTA-NH2 and CBZ. Furthermore, the synthesized tracer was also successfully used by externals to evaluate CBZ affine hybriodoma cells in flow cytometry. In the simulated screening, five antibodies with known affinity to CBZ were diluted in a cell culture medium. The screening method allowed to differentiate between affine antibodies (IC50 < 20 µg/ml) and unaffine antibodies (IC50 > 20 µg/ml), when concentrations of 0.1 µg/ml IgG or greater have been used. Of five applied antibodies, all highly affine clones (CE2 and B3212M) were reported as positives while no false-positive samples were observed. The screening included competitive, with around 89500 fold excess of CBZ, and non-competitive tracer incubation on different segments of the same chip, which resulted in total signal suppression on the competitive segment. The screening was performed in 20 hours, only a few nanoliters, of each simulated supernatant, were consumed in the screening process, furthermore in the method standard 96 well MTPs were used and no cleanroom facilities were required.
The aim of this work was the preparation of a novel stationary monolithic phase for affinity chromatography and HPLC-applications. Therefore, we have chosen porous glass filters that are available with different pore sizes as raw materials to prepare monolithic columns. We purchased VitraPOR 4 (10-16 μm pore size) and VitraPOR 5 (1.0-1.6 μm pore size) monolithic glass filters. The physical properties of these glass filters were characterized. The surface area, pore size distribution and the porosity were determined using mercury intrusion porosimetry and BET. These glass filters only exhibit flow through pores and therefore show no bimodal pore size distribution in the mercury intrusion curves. Due to their low permeability, the applied filters that exhibit an inner diameter of 8.0 mm and a length of 15.0±0.1 mm could be operated at flow rates more than 10 ml/min. High flow rates are favorable for fast separation experiments.
The fine fraction of bottom ash from municipal solid waste incineration is characterized of both a high pollution and relevant resource potential. Methods for studying the environmental behaviour of solid residues are leaching tests. Various leaching test are adopted all over Europe with liquid to solid ratio of 2 or 10 l/kg. In Germany three different leaching Tests are valid with the commencement of the draft of the ordinance of reuse of mineral waste as alternative building ordinance. Comparing two batch tests, only the concentration for chloride is comparable. To evaluate the metal resource potential in the sand fraction wet chemical Methods have been applied. Methodical problems were caused mainly by the material heterogeneity and especially for precious metals due to their low concentration around 1 mg/kg. Other Methods have been available, but hardly applicable.
The presentation focuses on the current state of the optical spectroscopic studies on plasmon enhanced upconversion luminescent processes of silica-metal core-shell nanocomposites. A general introduction of the upconversion process, the theoretical basis of plasmonic enhancement, the theoretical requirements in regard to NP architecture for plasmon enhanced UC will be outlined. The first proof-of-concept measurements show the difficulty in realization the theoretical measurement parameters in laboratory conditions and underline the need for shifting the experiments to single particle level.“
The application of inorganic nanoparticles as reinforcement agent for polymer composites is constantly growing. Improving the performance of the material with desirable properties requires understanding of the interaction between polymer chains and nanoparticles and the properties of the interphase as well. Boehmite, a mineral of aluminum with basic unit of AlO(OH), is a novel and promising nanofiller which leads to enhanced performance of polymer composites. It has been recently reported that boehmite nanoparticles have reinforcing effect on epoxy matrix in carbon-fiber composites. It was primarily assumed that these improvements are due to very high Young’s modulus of boehmite particles. However, in our latest study we presented new values for the Young’s modulus of boehmite much lower than those reported earlier. This brings up the importance of interphase properties, e.g. the crosslink density, which can have the dominant role in the overall material property. Nevertheless, due to resolution limitations of conventional nanoprobing approaches, characterization of the interphase between individual particles and matrix is a challenge.
In this study, the main goal is to investigate the interphase of the epoxy/boehmite nanocomposites using AFM-based methods. We simplify the three-dimensional nanocomposite system to a two-dimensional horizontally layered sample with a large and easy to access interphase area. For this purpose, 1µm coatings of hydrothermally synthesized boehmite are prepared as the substrate on which the epoxy is later molded and cured. AFM surface potential and force maps were obtained on the cross-sectional cut of epoxy/ boehmite sample. The results show unexpectedly a large interphase area (approx. 1 µm) with different electrical and mechanical properties comparing to bulk epoxy. The average force-distance curves from this region showed more elastic behavior compared to bulk. The underlying mechanism of this influence is not fully understood yet. Thus, further investigation on the interphase region using the novel Nano-IR approach provides more information about the chemical characteristics. Numerical simulation will give complementary information to understand the effect of nanoparticles on the crosslinking density of the interphase. This can be different to bulk epoxy due to either different local temperature gradients or due to a surface selectivity of boehmite towards the monomer molecules.
Boehmite nanoparticles (AlOOH) were recently found to improve properties such as crack resistance, shrinkage and compressive strength in epoxy composites. Concentration and surface modification of boehmite nanoparticles are key factors for abovementioned enhancements. To understand the underlying mechanisms, more detailed research of micro- and nanoscopic mechanical properties is required. The presented study aims to investigate the influence of concentration and surface modification of boehmite on the stiffness of the bulk epoxy by means of AFM-based approaches: Force-Distance curves (FDC) on the sub- microscale and Intermodulation AFM and amplitude-dependent force spectroscopy (ADFS) on the nanoscale. For this purpose, stiffness-maps of epoxy filled with boehmite, with and without surface modification (HAc-boehmite) were obtained by FDC. These measurements showed a slight increase in overall stiffness of composite with increasing the nanoparticle content. The stiffening effect was observed to be intensified with HAc-boehmite. Since the lateral resolution of FDC is not high enough to distinguish nanoparticles, this effect was assumed to be due to the inevitable inclusion of nanoparticles in the measurement. By using Intermodulation-AFM, yielding ADFS stiffness maps with the resolution of <10 nm, we were able to calculate the average stiffness of bulk epoxy without the interference of nanoparticles. It was expected that the stiffness of regions faraway from particles would be equal to neat epoxy. In contrast, the results showed a drastic increase in stiffness of epoxy with increasing boehmite concentration (0, 1, 2.5, and 15%) especially in case of introducing 15wt% HAc-boehmite. Another important observation was formation of a spatial structure with non-homogenous stiffness distribution in bulk epoxy with HAc-boehmite. The underlying mechanisms of described observations are not fully understood yet. One hypothesis is the local increase in crosslinking density which we aim to investigate in our further studies by combining Dynamic Mechanical Thermal Analysis (DMTA) and Intermodulation-AFM.
Additive Manufacturing provides an important enabling technology for the digital transformation of the economy. As an emerging technology it has seen a remarkable development over the last three decades. Nevertheless, it is far from a broad adoption with several barriers to overcome yet. One of the major challenges is the lack of standards. The critical role of standardization for innovation is generally recognized, still the topic too often has been neglected in strategic roadmapping exercises for emerging technologies. Too little is known about the complex dynamics and interrelations of standardization and innovation. The anticipation of standardization needs and the timely and efficient implementation of standards is challenging. This paper aims at contributing to a better understanding of the role that standards play in the multi-dimensional system of innovation. It analyzes the trajectories of innovation in Additive Manufacturing in a systematic and holistic way, focusing on standardization activities with regard to coordination, stakeholders involved, the timing and types of standards developed. Putting standardization in context of the multi-dimensional innovation system of Additive Manufacturing the research shows where standards can support the diffusion of an emerging technology.
Leaking methane (CH4) from infrastructures, such as pipelines and landfills, is critical for the environment but can also pose a safety risk. To enable a fast detection and localization of these kind of leaks, we developed a novel robotic platform for aerial remote gas sensing. Spectroscopic measurement methods for remote sensing of selected gases lend themselves for use on mini-copters, which offer a number of advantages for inspection and surveillance over traditional methods. No direct contact with the target gas is needed and thus the influence of the aerial platform on the measured gas plume can be kept to a minimum. This allows to overcome one of the major issues with gas-sensitive mini-copters. On the other hand, remote gas sensors, most prominently Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensors have been too bulky given the payload and energy restrictions of mini-copters. Here, we present the Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS), which combines a novel lightweight TDLAS sensor with a 3-axis aerial stabilization gimbal for aiming on a versatile hexacopter. The proposed system can be deployed in scenarios that cannot be addressed by currently available robots and thus constitutes a significant step forward for the field of Mobile Robot Olfaction (MRO). It enables tomographic reconstruction of gas plumes and a localization of gas sources. We also present first results showing its performance under realistic conditions.
Isotope amount ratios (hereafter referred to as simply isotope ratios) are proving useful in an ever increasing array of applications that range from studies unravelling transport processes, to pinpointing the provenance of specific samples as well as trace element quantification by using isotope dilution mass spectrometry (IDMS). These expanding applications encompass fields as diverse as archaeology, food chemistry, forensic science, geochemistry, medicine and metrology. However, to be effective tools, the isotope ratio data must be reliable and traceable to enable the comparability of measurement.
The importance of traceability and comparability in isotope ratio analysis has already been recognized by the Inorganic Analysis Working Group (IAWG) within the CCQM. Three pilot studies have focused on the quality of isotope ratio determinations (P48 “U isotope ratios in urine”, P75 “stable isotopes in Methionine”, P105 “87Sr/86Sr in wine”). Moreover, isotope ratio measurements are fundamental to IDMS amount of substance determinations. For example, when Pb quantification using IDMS is undertaken, this requires the measurements of Pb isotope ratios. While the requirements for isotope ratio accuracy and precision in the case of of IDMS are generally quite modest, “absolute” Pb isotope ratio measurements for geochemical age dating and source rock characterization as well as forensic provenance and fingerprinting studies require Pb isotope ratio measurements of the highest quality. To support present and future CMCs on isotope ratio determinations, a Key Comparison was urgently needed. Therefore, it was decided at the IAWG meeting in Paris in April 2011 that a Key Comparison on the determination of Pb isotope ratios in a pure Pb solution and in a bronze sample should be organized and accompanied by a pilot study.
Measuring Pb isotope amount ratios in a pure Pb solution, while seemingly straight forward, rigorously tests the ability of analyst to correct for any instrumental effects (such as mass discrimination and blank correction) on the measured ratios. Pb, present in trace amounts in a metal matrix sample (e.g. Pb in bronze), provides a real world test of the whole chemical and instrumental procedure, from chemical separation and sample purification to analysis and subsequent correction of appropriate instrumental effects on the separated samples.
A suitable bronze material with a Pb mass fraction between 10 and 100 mg·kg-1 was available at BAM. A high purity solution of Pb with a mass fraction of approximately 100 mg·kg-1 was also available. By comparing the Pb isotope ratio results obtained for the bronze sample with the Pb isotope ratio results from the Pb solution, potential biases arising from the processing of the bronze sample could be effectively identified and separated from the instrumental effects arising from the measurement and data processing protocol.
The increased application of higher-strength steels and filler materials necessitates a more profound understanding of the interactions between the welding process, the heat input, the cooling conditions and the resulting metallurgical processes in the weid and its surroundings. Strategies, which help to improve the strength properties and life-time of welded stmctures to such an extent that the utilisation of higher-strength materials can be justified and their lightweight construction potential can thus be exploited to the füll, can only be derived from the interaction between all the influencing factors. Examples of a few investigations on welded joints between higher-strength fine-grained structural steels with regard to the interactions between the main variables influencing the cold cracking are presented in this article.
The efficiency of gas sensor application for facilitating the safe use of hydrogen depends considerably on the sensor response to a change in hydrogen concentration. Therefore, the response time has been measured for five different-type commercially available hydrogen sensors. Experiments showed that all these sensors surpass the ISO 26142 standard; for the response times t90 values of 2 s to 16 s were estimated. Results can be fitted with an exponential or sigmoidal function. It can be demonstrated that the results on transient behaviour depend on both the operating parameters of sensors and Investigation methods, as well as on the experimental conditions: gas change rate and concentration jump.
Various methods have been used for introducing fire retardant additives into polymers. Deposition of thick fire retardant coatings directly onto polymer substrates is an alternative technique. An important advantage of the coating technique is the preservation of the physical and chemical integrity of the polymer material. Moreover, the fire retardancy of the polymer materials can be achieved following their production. Suitable coating materials are inorganics, intumescent, char-forming, oxygendiluting, and cooling or radical quenching layers. The most important problem is to achieve sufficient coating thickness to withstand the direct attack of flame and to protect the polymer bulk from pyrolysis, otherwise blistering of coating, caused by emitted pyrolysis gases, is often observed. To avoid blistering of coating, the adhesion between polyolefin substrate and fire retardant coating has to be extraordinarily high.
In order to achieve such a high level of adhesion, the polymer surface has to be modified with adhesion-promoting functional groups. The deposition of thin plasma polymers as adhesion-promoting layers with NH2, OH or COOH groups has been the most suited method. These functional groups are able to form covalent bonds and other interactions between the fire-resistant coating and the plasma-modified polyolefin substrate. Additionally, the plasma polymer counteracts the strong mechanical stresses in the laminate on exposure to high temperatures by its flexibility.
Bacterial biofilms represent a ubiquitous form of microbial life on Earth. Due to an evolved armory of protean biological responses to external stimuli, bacteria are able to adhere to, colonize and thrive on virtually all surfaces, whether natural or synthetic, even in challenging environmental conditions. In addition to significant health risks, biofilms are among the salient contributors to the deterioration of metals and their alloys, thereby causing safety risks for technical equipment. Hence, understanding the interaction mechanisms of electroactive sessile bacteria with metal surfaces is vital for facilitating the development of efficient control strategies and novel anti-fouling surfaces in various industries and technologies.
The present study focusses on a combined spectroelectrochemical approach, melding methods of surface enhanced Raman spectroscopy (SERS) and electrochemical techniques, to investigate the chemical characteristics and redox activities of electroactive bacteria during the initial stages of biofilm formation. Gold has been selected as a model substrate due to its inert character, considerably high surface enhancement factor, as well as its capability to allow surface chemistry modifications and substrate polarization in order to precisely control the surface charge. Square wave voltammetry (SWV) and cyclic voltammetry (CV) studies have been performed for quantitative determination of flavin concentration and electrochemical impedance spectroscopy (EIS) has been utilized to study the changes in electrochemical processes within biofilms during different stages of growth. Shewanella sp. have been chosen as microorganisms within this work due to their versatile exoelectrogenic respiratory behavior and their distinct ability to reduce metals via extracellular electron transfer mechanisms involving self-secreted electron shuttle redox molecules such as flavins. To further explicate the process of diffusion of flavins within biofilms, a model system has been developed to simulate the structural features of the bacterial extracellular polymeric substances typically found in biofilms. This has been achieved by creating hydrogel films comprised of calcium-cross-linked alginate. The results demonstrate an interplay of factors contributing to the initial phases of bacterial settlement and biofilm formation as a function of environmental parameters. Furthermore, the results allow insight into the diffusion of flavins, much like they would in a natural biofilm, and how their redox behavior affects the biofilm development.
Capillary electrophoresis (CE) is an analytical technique that
separates analytes based on their electrophoretic mobility with
the use of an applied voltage.
Nanoparticles separation using CE exhibits good separation and
analysis efficiency, especially for nanoparticles smaller than 30
nm. The coupling of CE with inductively coupled plasma mass
spectrometry (ICP-MS) provides the possibility to detect
nanoparticles in the concentration range of nanograms per litre
and enables the simultaneous detection of nanoparticles and its
[1][2] ionic counter parts.
Our objective is to develop a fast and reliable separation method
for differently modified nanoparticles using capillary
electrophoresis.
The performance of a miniaturized channel for the separation of polymer and metal nanoparticles (NP) using Asymmetrical Flow Field-Flow Fractionation (AF4) was investigated and compared with a conventional AF4 system. To develop standard separation methods, experimental parameters like cross flow, gradient profile and injection time were varied and optimized.
Corresponding chromatographic parameters were calculated and compared. Our results indicate that the chromatographic resolution in the miniaturized channel is lower, whereas significantly shorter analyses time and less solvent consumption were obtained. Moreover, the limit of detection (LOD) and limit of quantification (LOQ) obtained from hyphenation with a UV-detector are obviously lower than in a conventional channel, which makes the miniaturized channel interesting for trace analysis.
A common method for nanoparticle separation, which was introduced in 1976 by Giddings, represents asymmetrical field-flow fractionation (AF4). It is a flow based separation method, which can be theoretically used to separate particles range from 1 nm to 50 µm. However, when the particles are smaller than 10 nm, separation with AF4 will become difficult to perform. Because in this case strong separation force, which induces aggregation of particles, should be applied. This will decrease recoveries of analytes and limit its application in accurate quantitative analysis. Capillary electrophoresis (CE) is another well-developed separation technique, in which samples will be separated in relation to their electrophoretic mobility. In recent years, CE has been used to separate different kinds of nanoparticles like, gold colloids or CdSe Quantum dots. However, till now only separation of particles smaller than 50 nm was reported. Because large size distribution of bigger particles will result in strong peak broadening and long separation time.
A two-dimensional coupling of AF4 and CE might provide us a new separation method, which can extend the separation ranges of both methods and be a way to characterise particles with large size distributions.
Inhibition of Herpes Virus by Specific and Non-specific Interactions With Graphene Conjugates
(2017)
Herpes viruses (HSV) are global, host-adapted pathogens that cause a widespread diversity of diseases. The frequency of HSV infections all over the world has amplified over the last years, making it a major concern in the area of public health. Therefore, synthesis of systems that can inhibit development of these viruses is required. Various compounds already have shown inhibition of HSV, but concentration of these inhibitors is relatively high and resistance against those drugs is challenging.
Combination of biological knowledge, about structure of the active site on the surface of HSV that is responsible for inhibition of the pathogen, with the chemistry of graphene results in 2D systems with the ability of specific and nonspecific interactions with HSV. In this work, 2D nanomaterials with picomolar IC50 against HSV are synthesized by conjugation of peptides to the surface of graphene.
2D nanomaterials are characterized by various methods, including XPS, AFM and IR. Biological evaluation showed high potency of synthesized nanomaterials to inhibit HSV and therefore underlined possibility to use such materials in future biomedical applications.
Graphene and its derivatives have recently attracted much attention for sensing and deactivating pathogens. However, mechanism of multivalent interactions at the graphene-pathogen interface are not fully understood. Since different physicochemical parameters of graphene play a role at this interface, control over graphene’s structure is necessary to study the mechanism of these interactions. In this work, zwitterionic graphene nanomaterials (ZGNMs) were synthesized with defined isoelectric points and exposure, in terms of polymer coverage and functionality. Then, the switchable interactions of ZGNMs with E. coli were investigated to study the validity of the generally proposed “trapping” mechanism for inactivating pathogens by functionalized graphene derivatives. The ZGNMs were able to controllably trap and release E. coli by crossing their isoelectric points.
Metal organic frameworks and coordination polymers play an important role in different fields of applications. Moreover, particularly fluorinated metal-organic frameworks (FMOFs) are in the focus of interest during the last years. In most cases, fluorine is implemented using perfluorinated organic linkers at the synthesis, usually performed by solvothermal synthesis. However, only few examples are known so far where fluorine is coordinated directly to the metal cation. Recently, we reported about mechanochemical syntheses and characterization of fluorine-containing coordination polymers of alkaline earth metals by milling M(OH) (M: Ca, Sr, Ba) with fluorinated benzene dicarboxylic acids 2 and we reported about mechanochemical syntheses of alkaline earth metal fluorides with ammonium fluoride. Now we are reporting about a combination of both synthesis routes. That is the first mechanochemical synthesis of coordination polymers where fluorine is coordinated directly to the metal cation.
The present paper provides a discussion on all these topics and it offers solutions for it. The authors present an analytical solution of a Delta J based crack driving force based on an R6 type approach but modified for cyclic loading. The gradual build-up of the crack closure effect is modelled by the so-called cyclic R curve which describes the crack size dependency of the fatigue crack propagation threshold in the short crack regime. It is explained how the cyclic R curve is experimentally determined and how it can be estimated by a modified Kitagawa-Takahashi approach.
Strategic aspects for the development of measurement uncertainty annexes for ISO testing standards
(2017)
The presentation shows an overview over the current situation of the development of measurement uncertainty annexes for ISO mechanical testing standards. The comparability of measurement uncertainty statements is not ensured. The utilization of ready calculated measurement uncertainty values remains unclear. Partly the measurement uncertainty values clash with existing product standards where minimum values e.g. for the materials strength are determined. A route forward is shown to solve the current problems.
The presentation describes why the issue of thermal drift of extensometers has become important. It shows the possible sources of thermal drift of extensometers. It shows with a simple theoretical example calculation that the permitted strain error in standards can be exceeded if the temperature fluctuation at the extensometer is too high, but this effect remains mostly unknown because of missing data of the extensometer temperature throughout the test. This will be discussed in fatigue standard committees with the aim to improve the quality of fatigue testing results.
The authors, Li et al., of the paper entitled “Analysis on the Issues in ISO 6892-1 and TENSTAND WP4 Report Based on Data to Confirm Tests by 21 Laboratories” (J. Test. Eval.
DOI: 10.1520/JTE20150479 (online only)) have expressed views that the authors of this rebuttal believe to be based on fundamental misunderstandings and misinterpretations of the tensile testing standard ISO 6892-1:2009, ISO 6892-1:2016, and its former versions, thus leading to erroneous conclusions. This refutation is intended to clarify the understanding of ISO 6892-1 and to address the misunderstandings and the misinterpretations of the authors of the paper. The present standard ISO 6892-1:2016 has a long history dating back to the 1970s. At that time, the tensile testing procedure was standardized on the National and International scale in parallel. To understand the present standard, the knowledge of the history helps to understand the background of details of the testing procedure implemented today. The history of the tensile testing standard has been discussed extensively during the annual international standardization meeting of ISO committee TC 164 SC1 for the last few years, at which some of the authors of the Li et al. paper attended. The authors continue to disagree with facts that were agreed by the consortium of the European research project TENSTAND and by the present international experts involved in ISO TC 164 SC1. It appears that the principal objective of the authors regarding their present publication was to increase the testing speed during tensile testing. However, the international standardization community has previously declined similar proposals by some of the authors. Many Arguments presented by Li et al. were thus refuted. The conclusions of their paper are misleading and the international standardization community for tensile testing refused to revise the present standard, ISO 6892-1 (2016), according the authors’ proposals.
The digitalization of industrial processes is the most discussed topic in society these days. New business models have been developed to benefit from the opportunities offered by a digitally connected world. However, the focus in on the smart factory consisting of autonomous acting cyber physical systems (CPS). The efficient implementation of such CPS within an industrial environment requires the digitalization of the corresponding production processes. The digital twin of the process under investigation enables to develop sophisticated monitoring and control strategies which are necessary to fulfil the requirements of individual product design.
The need for a digitalization of the welding process is a logical consequence especially with regards to its industrial importance. The theoretical investigations and derived mathematical models of the welding process are well known since many decades. Anyhow, there is still a lack of industrial applicability of such models for an efficient and safe design of welded components. With respect to structural welding simulation that targets the heat effects of welding in terms of global quantities like temperature, solid phase distribution and residual stresses as well as distortions, the limited predictability of these quantities for arbitrary process parameters hinders its usability.
This presentation aims to give an overview of the current state of the art in structural welding simulation to predict the evolution of welding induced temperatures, stresses and distortions. Emphasis is given to industrial applicability of such models by reduction of the calculation times for large real-world structures and improved prediction of optimal process parameters. Furthermore, the role of such models within a weld data management system is demonstrated. The accumulation and relational storage of simulation and measuring data improves the overall process knowledge. This enables virtual cause and effect analyses of new process parameters as basis for a control system design.
A plethora of innovative materials are produced by depositing thin and ultrathin coatings on different substrates. For instance, hard disks able to store terabytes of information are based on multiple magnetic and non-magnetic nano-layers. Moreover, protectives coatings might be used to enhance the mechanical properties of substrate materials; for instance Zn-based coatings are used in the Al industry.
In this context, solid analytical techniques are required to provide fast multi-elemental chemical analyses with high depth resolution (to monitor the different layers) and high sensitivity (to detect major, minor and trace elements). Direct solid analytical techniques, including Secondary Ion Mass Spectrometry, Secondary Neutral Mass Spectrometry, Auger Electron Spectroscopy or X-Ray Photoelectron Spectroscopy provide very valuable information about the atomic chemical composition of the surfaces/coatings; however, they also have some major drawbacks, such as high operating costs, complex sample pre-treatment and handling, low sample throughput and/or severe matrix effects that result in difficult quantification procedures. In order to overcome some of these drawbacks Glow Discharge Mass Spectroscopy (GD-MS) is proposed as a complementary methodology that provides an ideal solution for fast and accurate bulk and layer analyses. In this work, we evaluate the advantages and limitations of this technique and we discuss about recent progresses and new applications.
Innovative material with outstanding physical and chemical properties are produced upon the deposition of thin and ultrathin coatings on different substrates. For instance, hard disks able to store Tera-bytes of information are based on the deposition of multiple nano-layers, which include magnetic and non-magnetic layers. Many other analogous examples, including photovoltaic cells, coated Al substrates, oxidized thin film composite membranes, coated glasses, coated polymers, etc. could be cited. The physical performance of these emerging materials is directly related to their chemical properties, including the elemental distribution within the different layers and at the layer-interfaces, or the presence of critical non-desired trace elements. Therefore, quality control and R+D advances require the development of direct solid analytical techniques able to provide fast multi-elemental chemical analysis of these materials, with high depth resolution (to monitor the different layers) and high sensitivity (to detect major, minor and trace elements).
Atomic spectrometry techniques have long been used for direct elemental chemical characterization. Techniques, such as Secondary Ion Mass Spectrometry or Auger Electron Spectroscopy provide very valuable information about the chemical composition of the surfaces/coatings; however, they also have some major drawbacks, such as high operating costs, complex sample pre-treatment and handling, low sample throughput and/or severe matrix effects that result in difficult quantification procedures. To overcome some of these drawbacks Glow Discharge Mass Spectroscopy is proposed as a complementary methodology that provides an ideal solution for fast and accurate bulk and layer analyses. In this work, we evaluate the advantages and limitations of this technique and we discuss about recent progresses and new applications.
Analysis of writing materials in Genizah fragments written during the first half of the XIth century
(2017)
My doctoral dissertation in progress focuses on ink composition on some fragments found in the Cairo Genizah and written by the leaders of the Jewish communities in Fustat during the first half of the XIth century. This is a project at the intersection of historical (Hebrew paleography) and scientific (physics, chemistry and materials science) disciplines. Indeed, I’m analyzing the corpus I constituted (written by Ephraim ben Shemarya and Yephet ben David from the Palestinian congregation and Elhanan ben Shemarya, Abraham ben Sahlan and Sahlan ben Abraham from the Babylonian community). The interests of such a study are numerous: provide insights on trade, local technologies, and social structures. If sufficient data is collected, the tabulated results have the potential for use as an indirect geochronological marker, in particular in the case of iron-gall ink. The composition of the vitriol used for the iron-gall ink preparation depends on the place of extraction. While attributing the vitriol used to a specific source of extraction is seldom possible, a number of origins can be excluded thanks to such analysis. Though ink composition alone cannot be used as a direct geochronological marker, superposition of chemical, palaeographical, codicological, and textual data would help to date and localize and serve as an additional argument for a typology and dating of other Hebrew scripts.
The CRISPR-Cas9 system revolutionized genetic engineering approaches with its simple design and high accuracy. The system comprises only two components – a synthetic guide RNA and the Cas9 protein. Our aim is to use this system to study factors influencing ectoine production.
Here, we use the CRISPRinterference variant to downregulate the expression of the ectoine synthesis gene ectA.
The Cairo Geniza is an “archive” discovered in the 19th century in Ben Ezra Synagogue in Fustat, a district in Old Cairo (Egypt), located south of the center of modern Cairo. The giant collection of mostly Jewish documents that vary in genres, languages and writing supports contains a large number of early medieval Hebrew manuscripts, mostly in fragmentary form. The larger part of the Cairo Geniza is stored today in the Cambridge University Library.
The Geniza provides sources for the literary, linguistic, historical studies of the various aspects Jewish life. As the documents attest, at least two Jewish communities co-existed in Fustat up to 11th century: a so-called Babylonian and Palestinian. These communities had different leaders, different traditions and lived independently. The differences seem to manifest themselves also in the paleographical, codicological and some material properties of the manuscripts produced by each community.
My work addresses the ink composition in the documents attributed to the members of these communities. For the determination of the inks type and composition I employ reflectography and µ-XRF spectrometry, respectively. The preliminary typological studies indicate that iron-gall inks were found predominantly in the manuscripts attributed to the Palestinian community.
Additive Manufacturing provides an important enabling technology for the digital transformation of the economy. As an emerging technology it has seen a remarkable development over the last three decades. Nevertheless, it is far from a broad adoption with several barriers to overcome yet. One of the major challenges is the lack of standards. The critical role of standardization for innovation is generally recognized, still the topic too often has been neglected in strategic roadmapping exercises for emerging technologies. Too little is known about the complex dynamics and interrelations of standardization and innovation. The anticipation of standardization needs and the timely and efficient implementation of standards is challenging. This paper aims at contributing to a better understanding of the role that standards play in the multi-dimensional system of innovation. It analyzes the trajectories of innovation in Additive Manufacturing in a systematic and holistic way, focusing on standardization activities with regard to coordination, stakeholders involved, the timing and types of standards developed. Putting standardization in context of the multi-dimensional innovation system of Additive Manufacturing the research shows where standards can support the diffusion of an emerging technology.
Additive Manufacturing provides an important enabling technology for the digital transformation of the economy. As an emerging technology it has seen a remarkable development over the last three decades. Nevertheless, it is far from a broad adoption with several barriers to overcome yet. One of the major challenges is the lack of standards. The critical role of standardization for innovation is generally recognized, still the topic too often has been neglected in strategic roadmapping exercises for emerging technologies. Too little is known about the complex dynamics and interrelations of standardization and innovation. The anticipation of standardization needs and the timely and efficient implementation of standards is challenging. This paper aims at contributing to a better understanding of the role that standards play in the multi-dimensional system of innovation. It analyzes the trajectories of innovation in Additive Manufacturing in a systematic and holistic way, focusing on standardization activities with regard to coordination, stakeholders involved, the timing and types of standards developed. Putting standardization in context of the multi-dimensional innovation system of Additive Manufacturing the research shows where standards can support the diffusion of an emerging technology.
The Westend Bridge is located on the A100 Highway in Berlin. An integrated continuous dynamic monitoring system, composed of 20 velocity sensors, 5 temperature sensors, 3 strain gauges, 1 crack sensor and 2 inclination sensors, was implemented by the Federal Institute for Materials Research and Testing in 2000. The system runs continuously with occasional intermittence and led to a huge amount of data over a 14-year span. In this article, variations of the strain, crack and inclination measurements during the last 14 years are presented. It is noted that the observed crack and inclination of the bridge are strongly influenced by seasonal temperature variation. It further induces change in the relationship between the strains measured in both concrete and prestressed tendon. Application of k-means cluster Analysis technique in both the crack and strain measurements can partition them into different seasonal phases by identifying ‘turning points’ that indicate annual periodical bridge change. In the period of these two ‘turning points’, a strong linear relation of the strains in two materials is observed. In the rest of the year, a nonlinear relationship between the strains recorded in both the concrete and the prestressed tendon is noted. The possible reason is the additional thermal load due to the change in temperature difference between the bridge’s surface and soffit. Finally, a health index in a Framework of regression model and process control theory is proposed by investigating the linear relationship between the strains in concrete and prestressed tendon. The tendency of the health index in the 14 years may suggest the long-term bridge change during that time frame.
Originally introduced in the field of earthquake engineering hybrid testing, i.e. the simultaneous combined application of numerical simulation techniques and execution of experiments, is nowadays used in different areas of experimental analysis. The focus of this paper is on the presentation of the so-called substructuring method as a hybrid method in fire engineering. Motivation are EU standards for fire resistance tests of columns or beams. According to these codes building elements are considered as stand-alone elements whereas in real fires each building element interacts with its adjacent elements. Therefore, to conduct a fire test in a more realistic fashion, the concept of hybrid substructuring as a special experimental technique has been adopted to fire engineering. Due to this concept the entire building, which is exposed to a real fire, is decomposed into two parts. One part is represented by the building element under test in a special furnace, whereas the remaining building environment is simulated by a model, based on the equations of thermomechanics. The paper addresses the historical development of the substructuring method in fire engineering supplemented by presentation of the results of realized fire resistance tests in substructuring mode on different types of specimens.
High temperature oxidation of 9–12% Cr ferritic/martensitic steels under dual-environment conditions
(2017)
In normal operations, the opposite surfaces of the power plant components are exposed to two different environments, i.e. air/flue gas on the one side and steam on the other side. Exposure under such dual-environment can lead to accelerated corrosion of the components on the air side. The oxidation behaviour of ferritic/martensitic steel T92 was investigated under dual-environment in a specially designed test equipment. The samples were exposed to dry oxyfuel flue gas (CO2–27%N2–2%O2–1%SO2) on one side and to steam on the other side up to 1000 h at 650°C. The formation of oxide scales was characterised by optical microscopy and scanning electron microscopy with attached energy-dispersive spectroscopy. Oxidation rate of specimens under dual-Environment condition was almost three times higher than that in single-environment condition. This is explained based on hydrogen transport through the bulk alloy from the steam side to the flue gas side.
A two-dimensional numerical mesoscale model has been created representing a microstructure of a typical 2205/1.4462 duplex stainless steel to further elucidate the mechanisms of hydrogen-assisted crack initiation and propagation in multiphase non-hydride forming metallic microstructures. Hydrogen-assisted cracking (HAC) was simulated by considering different stress and strain behavior as well as different diffusion behavior in both phases. For simulation of crack initiation and propagation, the element elimination technique has been applied. The model allows the simulation of path-free crack propagation which contributes to a better understanding of the HAC process in two-phase microstructures. As a particular result, the analyses revealed that a global macroscopic elastic deformation might already cause plastic deformation in both phases entailing respective HAC.
The work presents the effects of the change of the laser cladding parameters on microstructure, chemical composition and mechanical properties of Inconel 686 overlays (coatings). To obtain the best quality of These coatings the various parameters of laser cladding such as the power density of the laser beam, the laser beam velocity and overlapping ratio of the weld tracks were applied. The substrates were boilers plate made of the 13CrMo4-5 steel. Ni - base alloys characterize by the excellent high-temperature corrosion resistance, good strength and good ability to work in aggressive environments. This could be achieved by the reduction of the substrate melting and its dissolution into the overlays. The microstructure, chemical composition of the obtained overlays were investigated by means of a light microscope, a scanning electron microscope (SEM) equipped with the EDS detector. The overlays had cellular-dendritic structure. The variations of the chemical composition (especially Mo, Ni and W ) in the interdendritic and dendritic regions were observed. The interdendritic regions were enriched during solidifications in Mo and W and had lower content of Ni.
Under the Comité Consultatif pour la Quantité de Matière (CCQM), a key comparison, CCQM-K104, was coordinated by the National Institute of Metrology (NIM). The comparison was designed to demonstrate a laboratory's performance in determining the mass fraction of the main component in a complex high purity organic material. Nine NMIs or DIs participated in the comparison. Eight participants reported their results. An additional impurity was resolved from the avermectin B1a peak and was tentatively identified as an unknown impurity by NMIA (National Measurement Institute (Australia)). It was subsequently identified by NIM as a diastereoisomer of avermectin B1a at the C-26 position. Final reference value (KCRV) = 924.63 mg/g, with uncertainty (k=1) = 3.89 mg/g, and expanded uncertainty = 8.97 mg/g. The degrees of equivalence with the avermectin B1a KCRV for each participant were reported. The measurement results and degrees of equivalence should be indicative of the performance of a laboratory's measurement capability for the purity assignment of organic compounds of high structural complexity (relative molecular mass range of 500 Da -1000 Da and low polarity (-log KOW ≤ -2).
P92 is one of the important steels for super heater tubes used in combustion plants. However, in fossil fuel fired environments the formation of oxides and sulfides are challenging the material. To understand early corrosion mechanisms, which are important for process prediction, high temperature in-situ ageing experiments of Fe-Cr-Mn alloys in SO2 and SO2+H2O atmosphere were performed, applying energy dispersive X-ray diffraction (EDXRD) analysis.
Transport packages for spent nuclear fuel have to be assessed with respect to specific transport conditions which are defined in the regulations of the International Atomic Energy Agency. The physical state of the spent fuel and the fuel rod cladding as well as the geometric configuration of the fuel assemblies are important inputs for the evaluation of the package capabilities under these conditions. Cracks or failures in the fuel rod cladding can cause the release of gas, volatiles or fuel particles into the cavity. The amount of substances in the cavity has to be considered in the assessment of the activity release and criticality safety.
The mechanical analysis of the compound system formed by the fuel rod cladding and the spent fuel pellets is very difficult due to the limited knowledge of the material properties and the insufficient understanding of the interaction between pellets and cladding and between adjacent pellets. The variation of fuel assembly properties regarding cladding material, burn-up and the history of usage makes reliable predictions of the fuel rod behavior even harder.
For a better understanding about the behavior of spent fuel rods, JRC and BAM have started a joint research project. In this context, JRC has developed a test device which allows quasi-static 3-point-bending test on fuel rod segments in the hot cell. The loads are applied with respect to the boundary conditions of the activity release assessment. This paper deals with the numerical calculation of a single fuel rod segment under bending load. The aim is to identify the governing mechanical parameters by the variation of constitutive assumptions, contact conditions, inner constraints, etc. This knowledge helps for the interpretation of the experimental results. Furthermore, the improved understanding about the behavior of the cladding-pellets system will be beneficial for the assessment of spent fuel transport conditions.
Transport packages for spent nuclear fuel have to be assessed with respect to specific transport conditions which are defined in the regulations of the International Atomic Energy Agency. The physical state of the spent fuel and the fuel rod cladding as well as the geometric configuration of the fuel assemblies are important Inputs for the evaluation of the package capabilities under These conditions. Cracks or failures in the fuel rod cladding can cause the release of gas, volatiles or fuel particles into the cavity. The amount of substances in the cavity has to be considered in the assessment of the activity release and criticality safety.
The mechanical analysis of the compound system formed by the fuel rod cladding and the spent fuel pellets is very difficult due to the limited knowledge of the material properties and the insufficient understanding of the interaction between pellets and cladding and between adjacent pellets. The variation of fuel assembly properties regarding cladding material, burn-up and the history of usage makes reliable predictions of the fuel rod behavior even harder.
For a better understanding about the behavior of spent fuel rods, JRC and BAM have started a joint research project. In this context, JRC has developed a test device which allows quasi-static 3-point-bending test on fuel rod segments in the hot cell. The loads are applied with respect to the boundary conditions of the activity release assessment. This paper deals with the numerical calculation of a single fuel rod segment under bending load. The aim is to identify the governing mechanical parameters by the variation of constitutive assumptions, contact conditions, inner constraints, etc. This knowledge helps for the interpretation of the experimental results. Furthermore, the improved understanding about the behavior of the cladding-pellets system will be beneficial for the assessment of spent fuel transport conditions.
This project aims to develop capacity to produce certified reference materials (CRMs) for environmental analysis by transferring know-how between the partners and combining their skills to focus on environmental CRM production. The production process includes good manufacturing practices for processing materials, method development, the validation and application of homogeneity, stability and characterisation tests, the calculation of individual uncertainties (between-unit inhomogeneity, long term stability, characterisation) and combination of uncertainties to determine overall uncertainty of the matrix reference materials. An inter laboratory comparison registered as a EURAMET project is set as the ultimate project outcome, confirming the partners’ capabilities in applying newly acquired skills.
The work focuses on the potential of structural and chemical examinations by scanning electron microscopy based methods for archaeometric studies on ceramics. Achieved by a single preparation technique (polished block sections), the feasibility and benefits of electron backscatter diffraction are demonstrated as case studies using polychrome examples of pre-Columbian pottery (Wari, Moche and Cajamarca). Elemental and phase maps allow for separate consideration of clay and temper. Identification of mineral phases and intergrowths of temper particles provide information for clarifying clay procurement and firing techniques with respect to local versus non-local pottery to enlighten trade relations, technological transfer and shared heritage of pre-Columbian cultures.
Ferritic alloys containing Cr form Cr5S6 precipitates along grain boundaries in hot SO2 environment. Grain boundary precipitates may influence the steel’s mechanical behavior. Cr5S6 precipitates were reconstructed three-dimensionally using FIB tomography analysis to determine the volume, number, and penetration depth. The volume growth of Cr5S6 precipitates increased only for the initial aging time of 3 h but became constant after 6 h. The number of precipitates increased linearly.
The shock absorbing material damping concrete is for the foundation in dry interim storage facilities for radioactive waste in Germany. In case of a potential cask drop damping concrete minimizes the mechanical loads to the cask. In course of safety analyzes this accident scenario is considered by numerical simulations using the finite element method. To get reliable results of numerical simulations a suitable material model is needed to take the characteristics of damping concrete into account. Due to the lack of sufficient material knowledge a research project was started to characterize the material’s behavior under different load conditions. This paper presents the test program to analyze the material behavior of damping concrete which is characterized by large volume change and
strain rate hardening dependence. The determined Parameters were used to adapt an existing material model of the FE-code ABAQUS®. This model has to handle the mechanical damage behavior of damping concrete which occurs under compression and shear loads during a potential cask drop. To verify the material model numerical simulations are compared with dynamic penetration tests, which were conducted with specimens assembled similar to the real application of the damping concrete footings. The transferability of the material
model to a real accident scenario was verified by a drop test with a full-scale cask on a damping concrete footing.
This study aimed to assess the measurement capabilities of participating National Metrology Institutes/ Designated Institutes (NMIs/DIs) and expert laboratories in determining of low-polarity organics in surface water. This comparison was organized by Government Laboratory, Hong Kong (GLHK).
At the CCQM Organic Analysis Working Group (OAWG) Meeting held in November 2012 in Hong Kong, GLHK initially proposed a CCQM key comparison and a parallel pilot study programme on pharmaceuticals in surface water. Further discussion at the CCQM Meeting held in April 2014 in Paris, the OAWG approved a CCQM Track C comparison (CCQM-K126) on low polarity pharmaceuticals in surface water. In the meeting, the programme was supported by more than six National Metrology Institutes/ Designated Institutes (NMIs/ DIs).
CCQM-K126 officially commenced in July 2014 and had registration from nine NMIs/DIs. Participants were provided two bottles (40 mL each) of surface water and were requested to determine the mass fraction of spiked carbamazepinein in surface water. The coordinator received nine sets of results from eight NMIs/DIs in February 2015. Apart from one using an immunoassay technique, all participants applied isotope dilution liquid chromatography-tandem mass spectrometry (ID-LCMS/MS) technique as their determination technique.
A 30GHz liquid-crystal-based amplitude tuner is proposed for the first time. The amplitude of a signal can be controlled by using the interference principle. An input signal is divided into a tunable liquid crystal phase shifter and a fixed transmission line. Later, the divided signals are combined together at the output port. The output amplitude depends on the phase difference between the tunable and the fixed line. The low temperature co-fired ceramic technology is utilized to fabricate the device. The measurement shows an attenuation range of 11 dB to 30 dB with a maximum biasing voltage of 100V.
30GHz liquid-crystal-based amplitude tuner is proposed for the first time. The amplitude of a signal can be controlled by using the interference principle. An input Signal is divided into a tunable liquid crystal phase shifter and a fixed transmission line. Later, the divided signals are combined together at the output port. The output amplitude depends on the phase difference between the tunable and the fixed line. The low temperature co-fired ceramic technology is utilized to fabricate the device. The measurement shows an attenuation range of 11 dB to 30 dB with a maximum biasing voltage of 100V.
The German nuclear waste management strategy consists of dry interim storage of spent fuel inside dual purpose casks and its subsequent direct final disposal in a deep geological repository. Interim storage is limited to 40 years so far, but will have to be extended until repository site selection and operation is concluded, potentially up to 100 years. In this context, research on the long term performance of safety relevant cask components and fuel rod integrity during such extended periods of time is of outmost importance. The barrier function of the fuel cladding depends on its integrity under operational and accidental conditions along with storage and subsequent transportation and is mainly affected over time by altering of the cladding microstructure and by thermo-mechanical conditions during reactor operation and subsequent wet and dry storage.
This paper focuses on failure mechanisms regarding cladding embrittlement caused by physical phenomena concerning hydrogen dissolution and precipitation of hydrides in the zirconium matrix. Within this context, potential cladding integrity issues under extended interim storage conditions followed by transportation are emphasized.
Delayed hydride cracking (DHC) is a well-known time-dependent temperature-activated phenomenon failure mechanism of the fuel cladding during reactor operation. The phenomenon consists of hydrogen diffusion and hydride precipitation at the tip of an initial crack and the propagation of the crack to an approximate distance equal to the length of the hydride. This failure mechanism is temperature-activated phenomenon and enhances along with thermal cycling of the fuel cladding, e. g. during reactor shutdowns. DHC shows limited relevance under quasi static storage conditions with continuously lowering temperatures. However, the literature points that DHC may occur when the temperature during storage decreases to a certain level after some decades and in combination with stress concentrations in the cladding material.
When spent fuel is transferred to dry storage by vacuum drying, the cladding temperature raises up to peak temperatures of ~370°C. Under these conditions, hydrides dissolute into the zirconium matrix up to the solubility limit defined by the peak temperature and this amount of hydrogen can precipitate in a radial re-oriented fashion due to the temperature decrease during storage. Cladding materials with radially precipitated hydrides show significant embrittlement. Radially oriented hydrides are perpendicularly oriented to hoop stresses representing the most critical configuration. Brittle failure of the cladding then occurs by crack propagation through radially oriented hydrides and finally through the zirconium matrix. The susceptibility to radial hydride precipitation depends on cladding material type and microstructure, hydrogen content, pre-drying hydride distribution, irradiation conditions, and temperature and stress histories during drying and storage operations.
This paper addresses major considerations concerning spent fuel cladding embrittlement due to hydride precipitation with regard to the boundary conditions of dry spent fuel storage in Germany. Analytical, numerical, and experimental approaches are to be discussed by BAM in order to identify the specific needs for future R&D work in that area with the purpose to provide the necessary data base for proper safety demonstration and evaluation along with future extended storage licensing procedures.
Ferritic-martensitic high temperature alloys are widely used as boiler tube and heat exchanger materials in combustion based power plants. All technologies have in common that the applied materials are exposed to different temperatures, process pressures and reactive atmospheres which lead to a change of the material properties and a further degradation of the material.
To date corrosion analytics mainly proceeds via the use of various microscopic techniques and the analysis of the corrosion products after the reaction is completed. Comprehensive efforts have been made to study high temperature corrosion by the use of environmental SEM’s or in-situ TEM technologies. The here presented work will show a different approach to study high temperature gas corrosion in a multiple gas atmosphere by energy dispersive X-ray diffraction (EDXRD). For this technique high energetic white X-ray radiation (10-100 keV) was used as radiation source instead of conventional monochromatic radiation. It enables us to study crystallization procedures on short and medium time scales (1 min < t < 24 h) and the collection of Bragg-Signals of the phases of interest as a function of process time. Their occurrence can directly be correlated with thermodynamic and kinetic parameters. A special designed corrosion reactor was used to combine high temperature gas corrosion experiments with the collection of diffraction patter. The crystallization and reaction paths for oxide and sulfide formation was followed in-situ on Fe-Cr and Fe-Cr-Mn model alloys in a hot SO2 containing (T=650 °C) atmosphere.
The ageing of Fe-Cr model alloys in 0.5 % SO2 and 99.5 % Ar atmosphere was investigated to aim in a fundamental and systematic analysis of the combined oxidation and sulfidation mechanism. The crystallization and reaction paths for oxide and sulfide formation were followed in-situ by energy dispersive X-ray diffraction (EDXRD) in an early stage of corrosion (30 s – 24 h). For this technique, high energetic white synchrotron X-ray radiation (10-100 keV) was used as radiation source. Diffraction pattern were collected continuously in an early stage of corrosion up to 24 h during the complete ageing experiment.
The crystalline phases, growing on top of the coupons, were identified directly via their specific dhkl values. The evolution of the extracted integral intensities of specific reflections of the corrosion products as a function of time access direct information about the kinetics of the nucleation and growth. The results presented here show for iron with 2 wt% Cr wuestite formation first. Wuestite vanishes after 10 min of reaction only and magnetite and hematite appear. Magnetite formation proceeds simultaneously with sulfide formation. Sulfides growth proceeds after an incubation time, which differs for low alloyed (2 wt% Cr) and high alloyed (9 wt% Cr) material.
The ageing of Fe-Cr model alloys in 0.5 % SO2 and 99.5 % Ar atmosphere was investigated to aim in a fundamental and systematic analysis of the combined oxidation and sulfidation mechanism. The crystallization and reaction paths for oxide and sulfide formation were followed in-situ by energy dispersive X-ray diffraction (EDXRD) in an early stage of corrosion (30 s – 24 h). For this technique, high energetic white synchrotron X-ray radiation (10-100 keV) was used as radiation source. Diffraction pattern were collected continuously in an early stage of corrosion up to 24 h during the complete ageing experiment.
The crystalline phases, growing on top of the coupons, were identified directly via their specific dhkl values. The evolution of the extracted integral intensities of specific reflections of the corrosion products as a function of time access direct information about the kinetics of the nucleation and growth. The results presented here show for iron with 2 wt% Cr wuestite formation first. Wuestite vanishes after 10 min of reaction only and magnetite and hematite appear. Magnetite formation proceeds simultaneously with sulfide formation. Sulfides growth proceeds after an incubation time, which differs for low alloyed (2 wt% Cr) and high alloyed (9 wt% Cr) material.
For the application of the time-temperature superposition principle a suitable relation is needed to describe the time-temperature shift factor α. Therefore, the Arrhenius equation is widely used due to its simple form and often leads to suitable results. Where, the Arrhenius equation presents a linear relation for the temperature-dependent shift factor in logarithmic scale ln(α) with the absolute inverse temperature (1/ϑ). However, in cases with a large temperature range which eventually include more complex reaction processes, the functional relation between ln(α) and (1/ϑ) is nonlinear in the ‘Arrhenius plot’. In those cases, the monotone change of the nonlinear range in the ‘Arrhenius plot’ can be interpreted as a transient range between two approximately linear or constant regions. An extended application of the modified Arrhenius equation from Nakamura (1989) is presented in this study for this transient range. The introduced method was applied to describe the time-temperature equivalence in the relaxation analysis of restoring seal force of metal seals, which are used in lid-systems of transport and interim storage casks for radioactive materials. But, the method is widely valid and can be used for different objectives which are characterized by thermorheologically simple behavior with nonlinear sensitivity to inverse temperature.
Accurate measurements of stable isotope abundance ratio variations are often reported using artifact based delta-scales, which rely on suitable isotopic reference materials (iRM) for their realization. For example, variations in the 26Mg/24Mg isotope abundance ratio in natural systems are typically reported as delta26Mg values that represents the relative difference between the 26Mg/24Mg ratio measured in a sample relative to its measurement preferably in an iRM. In the past, such delta26Mg measurements were referenced to NIST SRM 980, the initial zero of the delta26Mg scale. With the development of MC-ICPMS, the detection of small but measurable isotopic differences in different chips of SRM 980 became apparent. It was then replaced by a Mg solution (DSM3), the new zero of the delta26Mg scale. A potential replacement iRM for DSM3 has been developed, ERM-AE143. This iRM has also been measured for its absolute isotope amount ratios1,2 making it traceable to the SI.
The results of an delta26Mg intercomparison experiment include the Mg iRMs SRM 980, IRMM-009, ERM-AE143, AE144, AE145 standards DSM3 and Cambridge-1. The intercomparison involved 5 expert laboratories, consisting of 3 national metrological institutes (BAM, NIST, PTB) and 2 scientific research laboratories (GFZ Potsdam, UBremen).
The iRMs were measured relative to AE143 and cover a range of ≈5 ‰ in delta26Mg. IRMM-009 has the lowest delta26Mg value while DSM3 has the highest, spanning a range in values that covers natural Mg isotope variations. The 2SD reproducibilities of the individual values from the different laboratories range from 0.02 to 0.26 ‰. The mean delta26Mg values, calculated from the laboratory means however show 2SD reproducibilities varing between 0.025 and 0.093 ‰. Propagated measurement uncertainties suggest a standard uncertainty of about 0.1‰ for delta26Mg determinations.
Hepcidin-25 has attracted much attention ever since its discovery in 2001. It is widely recognized that this liver produced peptide hormone plays a major role in the regulation of iron levels in mammals and can reveal important clinical information about several pathological states in patients suffering from iron-related disorders.
With the aim to tackle the current difficulties in hepcidin quantification and improve the status of this promising biomarker in the clinical field, we developed a rapid and robust analytical strategy for the quantification of hepcidin-25 in human samples based on HPLC-MS/MS (QqQ) to be implemented in routine laboratories. The novelty of the method is the use of special HPLC vials to avoid adsorptive losses due to the basic character of the peptide that causes interaction with the silanol groups of the vial’s glass surface. Up to 90% decrease in the MS/MS signal was observed, when commercial HPLC vials were used, while vials treated with 3-(2-aminoethylamino)propylmethyl-dimethoxysilane or 1H,1H,2H,2H-perfluorooctyltriethoxysilane, leading to no significant losses in the dynamic range of physiological hepcidin-25 mean serum levels (10-20 µg/L).
Careful analytical validation was performed for determining the reproducibility, repeatability, limit of quantification (0.5 µg/L) and linearity (0.5-40 µg/L) of the method. Serum samples from 9 healthy volunteers were analyzed with a median hepcidin-25 level of 3.3 µg/L, comparable to results reported in the literature.
We developed a rapid and robust HPLC-MS/MS (QqQ) method for the quantification of hepcidin-25, a promising new biomarker in iron metabolism, in human samples. The novelty of the method is the use of special HPLC vials to avoid adsorptive losses due to the basic character of the peptide that causes interaction with the silanol groups of the vial’s glass surface. Up to 90% decrease in the MS/MS signal was observed, when commercial HPLC vials were used, while vials treated with 3-(2-aminoethylamino)propylmethyldimethoxysilane or 1H,1H,2H,2H-perfluorooctyltriethoxysilane, leading to no losses in the range of physiological hepcidin-25 mean serum levels (10-20 µg/L).
Artificial intelligence (AI), machine learning, and neural networks have revolutionized fields such as self-driving cars or machine translation. Indeed, AI has progressed so far that scientists such as Stephen Hawking now fear that it may destroy humankind altogether. So, let’s get started and use AI in surface science.
Here we train neural networks to use raw measurement data as input and immediately return the desired output parameters. We discuss the example of X-ray reflectivity measurements of ultrathin films, which contain reciprocal space information and must traditionally be fitted with dynamic scattering theory. Instead, we train the neural network with simulated X-ray data of multilayer structures and then apply it to measurement data. The neural network yields high accuracy results, is robust against noise, and performs significantly faster than fitting algorithms in real-time experiments. The presented neural network data analysis is becoming increasingly attractive, because free software has become very accessible and specialized computer chips (NPU) are currently being rolled out.
This paper addresses the quantification of the value of damage detection system and algorithm information on the basis of Value of Information (VoI) analysis to enhance the benefit of damage detection information by providing the basis for its optimization before it is performed and implemented. The approach of the quantification the value of damage detection information builds upon the Bayesian decision theory facilitating the utilization of damage detection performance models, which describe the Information and its precision on structural system level, facilitating actions to ensure the structural integrity and facilitating to describe the structural system performance and its functionality throughout the service life. The structural system performance is described with its functionality, its deterioration and its behavior under extreme loading. The structural system reliability given the damage detection information is determined utilizing Bayesian updating. The damage detection performance is described with the probability of indication for different component and system damage states taking into account type 1 and type 2 errors. The value of damage detection Information is then calculated as the difference between the expected benefits and risks utilizing the damage detection information or not. With an application example of the developed approach based on a deteriorating Pratt truss system, the value of damage detection information is determined, demonstrating the potential of risk reduction and expected cost reduction.
The presented development of a damping model is a research component of an experimental feasibility study about moisture in building materials measured with Bluetooth® Low Energy (BLE) signals. This study may be part of a structural health monitoring aiming on early damage detection in the built infrastructure and is increasingly focusing on wireless sensor Network technology. It is investigated, how the Received Signal Strength Indicator (RSSI) of a BLE signal, transmitted from the BLE-module embedded in building materials with changing moisture content is damped. The BLE-module communicates with a mobile Smart Device as tablet or mobile phone via 2.45 GHz-ISMfrequency band where water dipoles start to oscillate. If the BLE-signal transfers through a moist material, the moisture Content influences the RSS-Indicator. The damping model demonstrates this damping effect on RSSI by the abstraction of the reality observed in a real system.
Laser metal deposition is described with its applications for additive manufacturing. The necessary process chain is discussed, with regard to weld bead dimensions and 3D build-up strategy. Metallurgical cross sections, x-ray and tensile tests are conducted. As demonstrative components, a gas turbine burner and a turbine blade are shown
This key comparison aims to assess the core capabilities of the participants in gas analysis. Such competences include, among others, the capabilities to prepare Primary Standard gas Mixtures (PSMs), perform the necessary purity analysis on the materials used in the gas mixture preparation, the verification of the composition of newly prepared PSMs against existing ones, and the capability of calibrating the composition of a gas mixture. According to the Strategy for Key Comparisons of the Gas Analysis Working Group, this key comparison is classified as an RMO track A key comparison.
The artefacts were binary mixtures of propane in nitrogen at a nominal amount-of-substance fraction level of 1000 μmol/mol. The values and uncertainties from the gravimetric gas mixture preparation were used as key comparison reference values (KCRVs). Each transfer standard had its own KCRV. The results are generally good. All results are within ± 1 % of the KCRV.
Optimization of laser treatment parameters of Inconel 686 overlay weld on carbon steel 13Mo4-5
(2017)
The work presents the effects of the change of the laser cladding parameters on microstructure, chemical composition and mechanical properties of Inconel 686 overlays (coatings). To obtain the best quality of these coatings the various parameters of laser cladding such as the power density of the laser beam, the laser beam velocity and overlapping ratio of the weld tracks were applied. The substrates were boilers plate made of the 13Mo4-5 steel. Ni - base alloys characterize by the excellent high-temperature corrosion resistance, good strength and good ability to work in aggressive environments. Applied overlays had a proper combination of the metal substrate in particular small amount of Fe. This could be achieved by the reduction of the substrate melting and its dissolution into the overlays. The microstructure, chemical composition of the obtained overlays were investigated by means of a light microscope, a scanning electron microscope (SEM) equipped with the EDS detector. The overlays had cellular-dendritic structure. The variations of the chemical composition (especially Mo, Ni and W ) in the interdendritic and dendritic regions were observed. The interdendritic regions were enriched during solidifications in Mo and W and had lower content of Ni.
The 7th International Conference on Spectroscopic Ellipsometry (ICSE-7) was held in Berlin in June 2016, jointly organised by ICSE and BAM. The publication of the proceedings special issue in Applied Surface Science follows this event. In the special issue, about 100 articles on current topics of optics and surface science related to ellipsometry, polarimetry, and similar techniques are presented, underpinning the high significance of these techniques for many fields of materials science.
An understanding on crystallization behavior and kinetics in glasses is one of the important topics in the glass science and technology. Tsukada et al.1) found an extremely unique and curious phenomenon in the crystallization of multiferroic (ferroelectric and ferroelastic properties) ’-Gd2(MoO4)3 crystals in Gd2O3-MoO3-B2O3 glasses. That is, crystals formed in the crystallization break into small pieces with a triangle prism or pyramidal shape having a length of 50-150 um spontaneously during the crystallization in the inside of an electric furnace, not during the cooling in air after the crystallization. They proposed to call this phenomenon “self-powdering phenomenon”. To the best of our knowledge, such a self-powdering phenomenon has not been observed in the crystallization of any other glasses. To investigate this phenomenon is very important for the glass science and for the preparation of bulk crystallized glasses with ferroelastic crystals. In this work, the preparation of crystallized glasses keeping the original shape is challenged, and the mechanism of self-powdering phenomenon is proposed. Glasses with the compositions of 21Gd2O3-63MoO3-(16-x)B2O3-xTeO2 (mol%) (x=0, 2, 4, 8) such as 21Gd2O3-63MoO3-16B2O3 (GM16B) and 21Gd2O3-63MoO3-8B2O3-8TeO2 (GM8T8B) were prepared using a conventional melt quenching technique. The quenched glasses were heat-treated at some temperatures, and the crystalline phase present in the crystallized samples was identified by X-ray diffraction (XRD) analyses, and the morphology and birefringence of crystals formed were observed using a polarized optical microscope (POM). The densities of GM16B and GM8T8B glasses are 4.76 g/cm3 and 4.91 g/cam3, respectively, and these values are higher than the density of ’-Gd2(MoO4)3 crystal, 4.555 g/cm3. These differences in the density might induce the large stresses in the inside of crystals during the crystal growth. The crystallized glasses of GM16B with ’-Gd2(MoO4)3 crystals do not keep the original glass shape, showing self-powdering phenomenon (breaking into small pieces). However, the crystallized glasses of GM8T8B keep the original glass shape without indicating any self-powdering. It is proposed that the stress at the interface between the glassy phase and ’-Gd2(MoO4)3 crystalline phase might be reduced in GM8T8B glasses containing TeO2 with weak Te-O bonds.
Borosilicate glass has a wide range of technical applications due to its high chemical durability and thermal-shock resistivity. Here the effect of H2O on 16 Na2O, 10 B2O3,74 SiO2 glass is studied over a wide range of water contents from 0 to 8 wt.%. MIR spectra give evidence for the coexistence of strongly and weakly H-bonded hydrous species. Evaluation of NIR bands at 5200 cm-1 (molecular H2O), 4700 cm-1 (B-OH), and 4500 cm-1 (Si-OH) reveal that OH groups dominate up to ~6 wt.% H2O, with B-OH/Si-OH of ≈ 0.8. The incorporation of low amounts of H2O has strong impact on structure. NMR spectra of nominally dry glasses indicate a significant fraction (12 %) of 3-coordinated boron, but almost all boron is 4-coordinated after addition of 3 wt.% H2O. Raman spectra show that hydration results preferentially in transformation of Q4 to Q2 while Q3 remain unchanged, probably stabilized by bonding to BO4 tetrahedra. Viscosity measurements and differential thermal analysis give consistent results, confirming strong decrease of the glass transition temperature with addition of water from 849 K (dry) to 540 K (5 wt% H2O). An additional relaxation mechanism in hydrous glasses is inferred from dynamic mechanical analysis and is assigned to cooperative processes involving hydrous species. It is postulated that this relaxation mechanism plays an important role in crack growth kinetics.
Surface water-induced broadening of crack initiation probability of zinc aluminosilicate glasses
(2017)
The crack generation probability by Vickers indentation of glass surfaces is known to be influenced by the atmospheric conditions under which the Vickers experiment is performed [1]. However, the effect of surface water due to preparation and storage of the glass surfaces prior to the indentation is less understood. Therefore, zinc aluminosilicate glasses of perzinc, peraluminous as well as nominally NBO-free meta-aluminous composition were prepared by melt quenching. Surfaces of cut and polished specimens of these glasses were either stored for seven days under constant atmosphere (50 °C; 55% RH) or etched (HF: 20vol%; 20 min) shortly before indentation. The obtained results show a strong variation of crack initiation behavior depending on chemical composition of the glasses as well as sample preparation. All experiments were performed in dry nitrogen gas to minimize the influence of atmospheric humidity during indentation. While the regular glass surfaces exposed to humid air prior to Vickers indentation show a broad distribution of crack initiation probability, this distribution narrows down if etched glass surfaces are tested. SNMS depth profiling shows a water enriched layer at the surface (150 μm) for the non-etched and stored specimens leading to the conclusion that surface water causes broadening of the crack initiation probability of glass surfaces.
Borosilicate glass has a wide range of technical applications due to its high chemical durability and thermal-shock resistivity. Here the effect of H2O on 16 Na2O, 10 B2O3,74 SiO2 glass is studied over a wide range of water contents from 0 to 8 wt.%. MIR spectra give evidence for the coexistence of strongly and weakly H-bonded hydrous species. Evaluation of NIR bands at 5200 cm-1 (molecular H2O), 4700 cm-1 (B-OH), and 4500 cm-1 (Si-OH) reveal that OH groups dominate up to ~6 wt.% H2O, with B-OH/Si-OH of ≈ 0.8. The incorporation of low amounts of H2O has strong impact on structure. NMR spectra of nominally dry glasses indicate a significant fraction (12 %) of 3-coordinated boron, but almost all boron is 4-coordinated after addition of 3 wt.% H2O. Raman spectra show that hydration results preferentially in transformation of Q4 to Q2 while Q3 remain unchanged, probably stabilized by bonding to BO4 tetrahedra. Viscosity measurements and differential thermal analysis give consistent results, confirming strong decrease of the glass transition temperature with addition of water from 849 K (dry) to 540 K (5 wt% H2O). An additional relaxation mechanism in hydrous glasses is inferred from dynamic mechanical analysis and is assigned to cooperative processes involving hydrous species. It is postulated that this relaxation mechanism plays an important role in crack growth kinetics.
Due to the demand of monitoring the water quality regarding emerging pollutants, such as drug residues, selective, high-throughput and multi-target analytical methods must be established. On the one hand, the influence of sewage on natural surface waters must be routinely monitored. On the other hand, estimation of removal efficiencies of pollutants, such as drug residues, is in the focus of industrial and public wastewater treatment. Immunoassays, such as ELISA, offer the possibility to be highly sensitive and selective due to the high target affine and specific recognition of antibodies to target molecules. Batch-wise processing in microtiter plates allow the necessary high-throughput, but only a single analyte can be determined within one measurement.
To overcome these disadvantages, we developed a four-plex micro-bead based flow cytometric assay, which is adaptable for the microtiter plate format. The modular and self-prepared bead support consists of polystyrene-core-silica-shell particles. While the polystyrene core is used for encoding, by introducing different amounts of fluorescent dyes, the silica-shell creates a solid-support for the immunoassay: The target analytes, three drugs, carbamazepine, diclofenac and caffeine and the f ecal marker isolithocholic acid are covalently coupled to amino-groups on the surface via NHS-chemistry. A competitive immunoassay is subsequently conducted in a simple mix-and-read procedure. Finally, we could use SAFIA to assess the influent of treated and untreated waste water on the Douro river estuary in Portugal. The results of the analysis are comparable to ELISA. However, measurements could be carried out in 25% the time of analysis.
Hydrous silicate and borate glasses of up to 8 wt% water were prepared using wet condition of melting under external pressure. Rheological experiments were conducted to determine the effect of the total water content on viscous flow and kinetic fragility. The findings indicate that dissolved water acts as a strong fluxing agent in both glass types. Water decreases particularly viscosity at the glass transition range, makes the viscosity-temperature curve "longer" and thus decreases kinetic fragility. Recent IR and NMR data are presented to link the dynamics of hydrous silicate and borate glasses with their structure particularly with regard to changes in the water-, silicon- and boron-speciation.
An approach to develop an arc sensor for gap-width estimation during automated NG-GMAW with a weaving electrode motion is introduced by combining arc sensor readings with optical measurement of the groove shape to allow precise analyses of the process. The two test specimen welded for this study were designed to feature a variable groove geometry in order to maximize efficiency of the conducted experimental efforts, resulting in 1696 individual weaving cycle records with associated arc sensor measurements, process parameters and groove shape information. Gap width was varied from 18 to 25 mm and wire feed rates in the range of 9 to 13 m/min were used in the course of this study. Artificial neural networks were used as a modelling tool to derive an arc sensor for estimation of gap width suitable for online process control that can adapt to changes in process parameters as well as changes in the weaving motion of the electrode. Wire feed rate, weaving current, sidewall dwell currents and angles were used as inputs to calculate the gap width. Evaluation the proposed arc sensor model show very good estimation capabilities for parameters sufficiently covered during experiments.
Presentation of the work of division 9.4 with focus on the Key aspects of component welding applying higher-strength fine-grained structural steels. The increased application of higher-strength steels and filler materials necessitates a more profound understanding of the interactions between the welding process, the heat input, the cooling conditions and the resulting metallurgical processes in the weld and its surroundings. Strategies, which help to improve the strength properties and life-time of welded structures to such an extent that the utilisation of higher-strength materials can be justified and their lightweight construction potential can thus be exploited to the full, can only be derived from the interaction between all the influencing factors. Examples of a few investigations on welded joints between higher-strength fine-grained structural steels with regard to the interactions between the main variables influencing the cold cracking are presented.
185 cracks were initiated in a soda-lime-silica glass by Vickers indentation and grown under controlled dry nitrogen atmosphere. Direct observation of subcritical crack growth (SCCG) upon indentation was performed using a video camera with an image acquisition rate of 3 ms. The results show that the validity of K(c) relations used to determine the indentation fracture toughness from a single imprint is questionable. It seems that correlation of crack length to stress intensity necessitate the use of statistical significant data of multiple crack events.
The evolution and mechanistic underpinnings of termite immunity are not well understood. Given the intimate relationship between sociality and disease, this represents a major gap in understanding, particularly since termites represent the only animal group outside of Hymenoptera to have evolved such advanced forms of social living. We explore the evolution of termite immunity by conducting qualitative and quantitative transcriptomic analyses from twelve cockroach and termite species occurring along a gradient of sociality. We incorporate lineages spanning the origin of eusociality, and include species from a key transitional subsocial group: the wood roaches. Firstly, we analyze immune characteristics in the context of termite phylogeny. Here, we examine the evolution of immune traits during the transition to eusociality, and explore the extent to which immune adaptations are associated with evolutionary shifts in social complexity and ecology. Secondly, we conduct a quantitative analysis of responses to a common immune stimulus to examine the role of both sociality and caste in immunity. Here, we test the hypothesis that the evolution of division of labour – and associated increases in investment into costly altruistic (immune) traits – occurred at the expense of individual immunity in the sterile caste.
Differentiation of immune response with castes in termites by de novo transcriptome sequencing
(2017)
Eusociality is one major evolutionary transitions, during which the division of labor is considered as the hallmark feature. This character of evolution, also interpreted as task specialization, is associated with multiple morphological, physiological and behavioral adaptations required for brood care, foraging, and defense. With these adaptations which ultimately cause the formation of castes in insect sociality (mostly in termites, ants, some bees and wasps), while whether immune system is related to eusociality in termites is rare understood. We hypothesis that immune system in termite sociality had also differentiation along with the formation of castes. We address this issue by exploring the immune responses of different castes with de novo transcriptome sequencing. After injection with cocktail of heat-killed pathogens (Pseudomonas entomophila, Bacillus thuringiensis, Saccharomyces cerevisiae), the mRNAs from false workers, soldiers and reproductive of Neotermes canstaneus were sequenced. We found much more genes are regulated (1420 genes downregulated and 398 genes upregulated) in reproductives compared to soldiers (90 genes downregulated and 108 genes upregulated) and false workers (135 genes downregulated and 71 genes upregulated). In these upregulated genes, reproductives had 54 same genes as soldiers, while only 7 same genes as workers which almost is same number between soldiers and workers. In the downregulated genes, reproductives shared 50 and 41 same genes as soldiers
and workers, respectively. Besides, soldiers and workers had 29 same downregulated genes. From these findings, it is indicated that the immune system differentiates with division of labor during eusociality in termites.
Recent studies have shown that host-microbiota interactions can lead to dramatic changes in host phenotype. We investigate the causal drivers of microbe-associated shifts in host phenotype by examining how feeding behaviour is modulated by microbiota interactions in two omnivorous cockroaches: Blatta orientalis and Blatella germanica. We conducted food-choice experiments after challenging hosts with a common entomopathogenic soil bacterium to understand the impact of pathogens on host macronutrient preference. We find that immune challenge by a pathogenic microbe drives a sharp decline in carbohydrate intake and results in a relative increase in the ratio of protein to carbohydrate (P:C) consumed. Additionally, infected cockroaches reduce their Overall nutrient intake, which is consistent with an illness-induced anorexia-like response. We show for the first time that cockroach feeding behaviour is dynamically modulated by a pathogen, and examine the influence of modified feeding behaviour on host immunity. We also investigate whether in Addition to pathogens, gut commensals are causally responsible for shifts in host behavioural phenotype. Here, we conduct food-choice and immune-challenge experiments in germ-free cockroaches, which have been refaunated with gut microbiota that are experimentally adapted to variable macronutrient (P:C) diets.
The first sterile caste to evolve in termites was the soldier. While the importance of soldiers to termite society defense has long been recognized, the contribution of soldiers to other societal functions, such as colony immunity, is less well understood. We explore this issue by examining the role of soldiers in protecting nestmates against pathogen infection. Even though they are unable to engage in grooming behavior, we find that the presence of soldiers of the Darwin termite, Mastotermes darwiniensis, significantly improves the survival of nestmates following entomopathogenic infection. We also show that the copious exocrine oral secretions produced by Darwin termite soldiers contain a high concentration of proteins involved in digestion, chemical biosynthesis, and immunity. The oral secretions produced by soldiers are sufficient to protect nestmates against infection, and they have potent inhibitory activity against a broad spectrum of microbes. Our findings support the view that soldiers may play an important role in colony immunity, and broaden our understanding of the possible function of soldiers during the origin of soldier-first societies.
Effective immunity is essential for maintaining insect society integrity but the mechanisms that connect immunity at the level of the individual to the level of society are poorly understood. Here, we begin to resolve this issue by addressing the interaction between individual immunity and caste identity in the termite Neotermes castaneus. We characterize the transcriptomic responses of different castes to a general immune challenge by sequencing mRNAs from false workers, soldiers and reproductive following injection with a cocktail of heat-killed pathogens. We found many more genes to be differentially regulated in reproductives (1420 and 398 genes down- and upregulated respectively) than soldiers (90 and 108 genes) or false workers (135 and 71 genes). We go on to conduct a quantitative analysis of the specific changes to immune regulation across the castes following pathogen exposure, before discussing the implications of these findings for our understanding of the evolution of immunity in eusocial termites.
Recent studies have shown that host-microbiota interactions can lead to dramatic changes in host phenotype. We investigate the causal drivers of microbe-associated shifts in host phenotype by examining how feeding behaviour is modulated by microbiota interactions in two omnivorous cockroaches: Blatta orientalis and Blatella germanica. We conducted food-choice experiments after challenging hosts with a common entomopathogenic soil bacterium to understand the impact of pathogens on host macronutrient preference. We find that immune challenge by a pathogenic microbe drives a sharp decline in carbohydrate intake and results in a relative increase in the ratio of protein to carbohydrate (P:C) consumed. Additionally, infected cockroaches reduce their overall nutrient intake, which is consistent with an illness-induced anorexia-like response. We show for the first time that cockroach feeding behaviour is dynamically modulated by a pathogen, and examine the influence of modified feeding behaviour on host immunity. We also investigate whether in addition to pathogens, gut commensals are causally responsible for shifts in host behavioural phenotype. Here, we conduct food-choice and immune-challenge experiments in germ-free cockroaches, which have been refaunated with gut microbiota that are experimentally adapted to variable macronutrient (P:C) diets.
The first sterile caste to evolve in termites was the soldier. While the importance of soldiers to termite society defense has long been recognized, the contribution of soldiers to other societal functions, such as colony immunity, is less well understood. We explore this issue by examining the role of soldiers in protecting nestmates against pathogen infection. Even though they are unable to engage in grooming behavior, we find that the presence of soldiers of the Darwin termite, Mastotermes darwiniensis, significantly improves the survival of nestmates following entomopathogenic infection. We also show that the copious exocrine oral secretions produced by Darwin termite soldiers contain a high concentration of proteins involved in digestion, chemical biosynthesis, and immunity. The oral secretions produced by soldiers are sufficient to protect nestmates against infection, and they have potent inhibitory activity against a broad spectrum of microbes. Our findings support the view that soldiers may play an important role in colony immunity, and broaden our understanding of the possible function of soldiers during the origin of soldier-first societies.
Diverse animal species consume toxins, minerals or secondary compounds as an adaptive response to pathogen infection – a process termed self-medication. Recent studies have also shown that macronutrients can play an important role in an individual’s infection response. For instance African army worm caterpillars select a diet rich in protein and low in carbohydrate upon baculovirus infection. Here we investigate whether dietary choice of macronutrients also plays a role in immunity in the omnivorous cockroach: Blatta orientalis. After challenging individual cockroaches with a common entomopathogenic soil bacterium, Pseudomonas entomophila, we conducted food-choice experiments using two artificial diets differing in their relative protein to carbohydrate ratio. We show for the first time that cockroaches are able to self-select a protein-enriched diet as a response to bacterial infection. This is driven by a sharp decline in carbohydrate intake rather than an increase in protein intake. Additionally, infected cockroaches reduced their overall nutrient intake, which is consistent with an illness-induced anorexia-like response. The feeding pattern of bacteria-challenged individuals returned to normality approx 4 days after challenge. We also investigate whether cockroach survival and hemolymph immunity are enhanced in individuals when restricted to a protein-rich vs. carbohydrate-rich diet. Overall, our findings demonstrate that macronutrient preferences follow a general pattern independent of pathogen type. Furthermore, we show that interactions between nutrition and immunity are highly conserved in evolution, highlighted by the fact that caterpillars and cockroaches diverged some 386 million years ago.
A fundamental yet seemingly contradictory aspect of biological individuals is their capacity to remain the same while changing through time. This self-regulatory ability is facilitated by a number of factors that are shared by all complex multicellular life-forms. One such essential trait is an effective immune system. Here, I use concepts of individuality and immunity to explore the blurred line between society and individual in termite “superorganisms”. I discuss our current understanding of the breadth and mechanistic underpinnings of collective immunity in termites, before going on to explore the evolution of the immune system during the transition from a cockroach-like ancestor to a fully-fledged termite society. I end by discussing the possibly crucial role played by immunity during the emergence of eusociality, and in transitions in organismal complexity generally.
The evolution and mechanistic underpinnings of termite immunity are not well understood. Given the intimate relationship between sociality and disease, this represents a major gap in understanding, particularly since termites represent the only animal group outside of Hymenoptera to have evolved such advanced forms of social living. We explore the evolution of termite immunity by conducting qualitative and quantitative transcriptomic analyses from twelve cockroach and termite species occurring along a gradient of sociality. We incorporate lineages spanning the origin of eusociality, and include species from a key transitional subsocial group: the wood roaches. Firstly, we analyze immune characteristics in the context of termite phylogeny. Here, we examine the evolution of immune traits during the transition to eusociality, and explore the extent to which immune adaptations are associated with evolutionary shifts in social complexity and ecology. Secondly, we conduct a quantitative analysis of responses to a common immune stimulus to examine the role of both sociality and caste in immunity. Here, we test the hypothesis that the evolution of division of labour – and associated increases in investment into costly altruistic (immune) traits – occurred at the expense of individual immunity in the sterile caste.
The evolution and mechanistic underpinnings of termite immunity are not well understood. Given the intimate relationship between sociality and disease, this represents a major gap in understanding, particularly since termites represent the only animal group outside of Hymenoptera to have evolved such advanced forms of social living. We explore the evolution of termite immunity by conducting qualitative and quantitative transcriptomic analyses from twelve cockroach and termite species occurring along a gradient of sociality. We incorporate lineages spanning the origin of eusociality, and include species from a key transitional subsocial group: the wood roaches. Firstly, we analyze immune characteristics in the context of termite phylogeny. Here, we examine the evolution of immune traits during the transition to eusociality, and explore the extent to which immune adaptations are associated with evolutionary shifts in social complexity and ecology. Secondly, we conduct a quantitative analysis of responses to a common immune stimulus to examine the role of both sociality and caste in immunity. Here, we test the hypothesis that the evolution of division of labour – and associated increases in investment into costly altruistic (immune) traits – occurred at the expense of individual immunity in the sterile caste.
Electric contacts based on silver-glass dispersions are key components in optoelectronic microsystems and control modules for medical, information & communication and energy technology in our networked society. Driven by the complexity of modern production processes and ever shorter time-to-market requirements, the fast and specific development of tailored silver-glass dispersions has become a bottleneck of technology development. Nevertheless, the underlying mechanisms of silver dissolution, transport, and reprecipitation, and the resulting micro structure evolution during firing are poorly understood. The broad literature on the precipitation of colloidal silver particles and the related processes of silver dissolution and diffusion mostly refer to very small volume fractions of silver. Transferring these results to the sintering of glass-containing silver dispersions, is therefore highly questionable. In this case, silver dissolution, electrical contact between silver particles, transport and reprecipitation take place under special conditions. This includes short diffusion lengths (particle size < 10 μm), the presence of three-phase contacts silver - glass - sintering atmosphere, as well as silver reprecipitation at the sintering contacts as the driving force of silver transport. Here, a dynamic balance of the silver concentration can be expected to result from the ratio between silver dissolution and reprecipitation. The aim of the project is to gain basic insight into the mechanisms of dissolution, transport and reprecipitation of silver in sintering silver glass dispersions. In this context, the main focus is on gaining basic knowledge about the dissolution of metallic silver in low melting oxide glasses as the limiting factor of the sintering of silver-glass composites. In particular, we will strive to gain insight into the effect of the oxygen content of the sintering atmosphere, of the oxygen dissolved in the silver particles, of silver oxide on the surface of the silver powder, of the electric contact between the silver particles, as well as the basicity of the glass. Furthermore, we strive for insights into the silver mobility and the silver concentration that can be attained (silver solubility) in oxide glasses with a low melting point. Summing up all these aspects, a closed explanatory model for silver dissolution, transport and reprecipitation during the sintering of glass silver dispersions will be introduced.
Electric contacts based on silver-glass dispersions are key components in optoelectronic microsystems and control modules for medical, information & communication and energy technology in our networked society. Driven by the complexity of modern production processes and ever shorter time-to-market requirements, the fast and specific development of tailored silver-glass dispersions has become a bottleneck of technology development. Nevertheless, the underlying mechanisms of silver dissolution, transport, and reprecipitation, and the resulting micro structure evolution during firing are poorly understood. The broad literature on the precipitation of colloidal silver particles and the related processes of silver dissolution and diffusion mostly refer to very small volume fractions of silver. Transferring these results to the sintering of glass-containing silver dispersions, is therefore highly questionable. In this case, silver dissolution, electrical contact between silver particles, transport and reprecipitation take place under special conditions. This includes short diffusion lengths (particle size < 10 μm), the presence of three-phase contacts silver - glass - sintering atmosphere, as well as silver reprecipitation at the sintering contacts as the driving force of silver transport. Here, a dynamic balance of the silver concentration can be expected to result from the ratio between silver dissolution and reprecipitation. The aim of the project is to gain basic insight into the mechanisms of dissolution, transport and reprecipitation of silver in sintering silver glass dispersions. In this context, the main focus is on gaining basic knowledge about the dissolution of metallic silver in low melting oxide glasses as the limiting factor of the sintering of silver-glass composites. In particular, we will strive to gain insight into the effect of the oxygen content of the sintering atmosphere, of the oxygen dissolved in the silver particles, of silver oxide on the surface of the silver powder, of the electric contact between the silver particles, as well as the basicity of the glass. Furthermore, we strive for insights into the silver mobility and the silver concentration that can be attained (silver solubility) in oxide glasses with a low melting point. Summing up all these aspects, a closed explanatory model for silver dissolution, transport and reprecipitation during the sintering of glass silver dispersions will be introduced.
Damage development and damage tolerance of structures manufactured by selective laser melting
(2017)
The additive manufacturing technology of Selective Laser Melting (SLM) experiences a rapid development within an increasing marked of quite different application fields. The properties of SLM materials and structures are influenced by a number of tech-nological parameters such as the metal powder (particle size, homogeneity, cleanliness), the laser tool (power, beam diameter, pulse lengths), the scanning operation (speed, sequence and orientation of melting paths), parameters of the over-all equipment (design and preheating of the base plate, currents and turbulence in the protective gas atmosphere) and, last not least, the hatching strategy including the build-up direction of the structure with respect to the loading direction of the component.
For the perspective use of SLM structures as load carrying, safety-relevant components the knowledge of their mechanical properties is necessary. It is essential to understand these in the context of the manufacturing-related features and at the back-ground of the basic characteristics of metallic materials: crystal lattice, microstructure and material defects. The paper provides an overview on factors which affect the mechanical parameters stiffness, strength, ductility, toughness, fatigue crack propagation and fatigue strength in the context of selective laser melting.
Up to now, the mechanisms of surface nucleation and surface-induced texture formation are far from being understood. Corresponding phenomena are discussed hypothetically or even controversial, and related studies are restricted to very few glasses. As a main drawback, the vast majority of previous work on oriented growth of surface crystals do not consider the possible effects of glass surface treatments (like polishing defects, adhered particles and cracks, …) or ambient annealing conditions (vacuum or atmospheric pressure) which both can influence crystal nucleation and growth. Moreover, very few observations of crystal orientation related to surface crystallization were focused on separately growing crystals. In conclusion, up to now, no systematic studies on initially oriented crystal growth or nucleation from defined active nucleation sites have been pursued.
Therefore, the main objective of the proposed project is to gain a basic understanding of the mechanisms of surface-induced microstructure formation in glass ceramics. We shall answer the question whether preferred orientation of surface crystals is the result of oriented nucleation or caused by other orientation selection mechanisms acting during early crystal growth. In both cases, crystal orientation may be caused by the orientation of the glass surface itself or the anisotropy and orientation of active surface nucleation defects.
New techniques of experimental characterization of surface-crystallized glasses shall be applied to find answers to the questions posed above. Based on a controlled preparation and annealing of the glass sample surfaces, that includes the defined creation of active nucleation defects, and followed by the microstructural characterization especially during the very early growth stages of separated surface crystals, the orientation relations between defect and initiated surface crystal will be analyzed. In order to gain new insights, a couple of entirely new microstructure diagnostics techniques, including chemically contrasted XRM, laser-based sample preparation for XRM, and 3D electron backscatter diffraction shall be developed or applied.
This way, using X-ray microscopy as a pivotal technique for the non-destructive 3D characterization of relatively large samples at superior spatial resolution (but also complemented by other microstructure diagnostics techniques, e.g. TEM elemental mappings at cross-sectioned samples) unprecedented insights into the microstructure evolution upon surface crystallization of model glasses will be gained.
Up to now, the mechanisms of surface nucleation and surface-induced texture formation are far from being understood. Corresponding phenomena are discussed hypothetically or even controversial, and related studies are restricted to very few glasses. As a main drawback, the vast majority of previous work on oriented growth of surface crystals do not consider the possible effects of glass surface treatments (like polishing defects, adhered particles and cracks, …) or ambient annealing conditions (vacuum or atmospheric pressure) which both can influence crystal nucleation and growth. Moreover, very few observations of crystal orientation related to surface crystallization were focused on separately growing crystals. In conclusion, up to now, no systematic studies on initially oriented crystal growth or nucleation from defined active nucleation sites have been pursued.
Therefore, the main objective of the proposed project is to gain a basic understanding of the mechanisms of surface-induced microstructure formation in glass ceramics. We shall answer the question whether preferred orientation of surface crystals is the result of oriented nucleation or caused by other orientation selection mechanisms acting during early crystal growth. In both cases, crystal orientation may be caused by the orientation of the glass surface itself or the anisotropy and orientation of active surface nucleation defects.
New techniques of experimental characterization of surface-crystallized glasses shall be applied to find answers to the questions posed above. Based on a controlled preparation and annealing of the glass sample surfaces, that includes the defined creation of active nucleation defects, and followed by the microstructural characterization especially during the very early growth stages of separated surface crystals, the orientation relations between defect and initiated surface crystal will be analyzed. In order to gain new insights, a couple of entirely new microstructure diagnostics techniques, including chemically contrasted XRM, laser-based sample preparation for XRM, and 3D electron backscatter diffraction shall be developed or applied.
This way, using X-ray microscopy as a pivotal technique for the non-destructive 3D characterization of relatively large samples at superior spatial resolution (but also complemented by other microstructure diagnostics techniques, e.g. TEM elemental mappings at cross-sectioned samples) unprecedented insights into the microstructure evolution upon surface crystallization of model glasses will be gained.
In Germany, for the transport and storage of spent nuclear fuel, casks with double closure lid systems are used, which are equipped with Helicoflex® metal seals. The original interim storage period for these casks was planned to be 40 years. However, recent political developments indicate that a storage time of more than 80 years might be necessary. Therefore, the current storage licenses have to be renewed in due course, which requires extended knowledge of the long-term behaviour of all cask components.
At the Bundesanstalt für Materialforschung und -prüfung (BAM), metal seals have been investigated after ageing at temperatures between room temperature and 150 °C for up to 7 years. At regular intervals the seals have been tested for leakage rate as well as for their mechanical behaviour. From these tests pronounced influence of ageing could be shown which results in the decrease of the seal force and the useable resilience. The main reason attributed to these performance changes is the increasing permanent deformation of the outer layer of the seal due to creep. So far, an explicit analytical description of the long-term behaviour that could be used for predictions exceeding the tested ageing times and temperatures was not suitable.
In addition to the component tests that were already conducted, a comprehensive investigation programme has been started to describe the mechanical behaviour of the individual seal components.
The individual seal components are tested regarding different material characteristics including creep, deformation and microstructural properties. The comparability of the material characterization is ensured by comparing the basic raw material of the specimen with the actual component material.
Furthermore, detailed investigations of the time and temperature dependent deformation behaviour are realized by ageing seal segments at multiple temperatures for different periods of time and employing standardized tests.
By analysing the acquired data in combination with the ongoing long-term component tests a dataset for analytical prediction of the long-term behaviour of the seals is intended for an extended period of time under a certain temperature regime.
The work presents the microstructure, chemical composition and mechanical properties of Inconel 686 coatings after high - temperature corrosion in environment of aggressive gases. To produce the Ni - base weld overlays the QS Nd:YAG laser beam was used. The substrates were 13Mo4-5 boilers plate steel. Ni - base alloys characterize the excellent high temperature corrosion resistance, good strength and good ability to work in aggressive environments. Applied overlays had a proper combination of the metal substrate in particular small amount of Fe. This could be achieved by the reduction of the melting of the substrate and its dissolution into the overlays. The microstructure, chemical composition of the obtained overlays were investigated by means of a light microscope, a scanning electron microscope (SEM) equipped with the EDS detector. The overlays had cellular-dendritic structure. The variations of the chemical composition (especially Mo, Ni and W ) in the interdendritic and dendritic regions were observed. The interdendritic regions were enriched during solidifications in Mo and W and had lower content of Ni.
The microstructure of weld overlay Ni - base alloy deposited on carbon steel by laser QS-Nd:YAG
(2017)
Ni- base alloys are used as a one of the most important coating material and can be applied in a different environments and elements of devices having various applications. To protect the surface of the material from aggressive gases at high temperature, there are use different kinds of the Ni- base alloys. One of such alloy is Ni-Cr-Mo-W called commercial Inconel 686. This alloy based on NiCr22Mo9Nb (Inconel 625), in which content of molybdenum increased and niobium was replaced with the addition of tungsten, in order to counteract the strong segregation in the microstructure, which results in homogeneity of the chemical composition of the structure. Inconel 686 is also characterized by greater resistance to high temperature corrosion and heat resistance than Inconel 625. The Inconel 686 alloy was deposited on 13CrMo4-5 steel by laser QS - Nd:YAG. In the poster the microstructure (SEM) and chemical composition (EDS) of obtained weld overlays were investigated.
The layer-wise slurry deposition (LSD) is an innovative process for the deposition of powder layers with a high packing density for Additive Manufacturing (AM). A slurry with small organic content is repetitively spread as thin layers on top of each other by means of a doctor blade. During the deposition, the ceramic particles settle to form thin layers with a high packing density (55-60%). Each layer is then dried, resulting in the stacking of a dry powder bed with high powder packing. When coupled with a printing head or with a laser source, the LSD enables novel AM technologies inspired to the 3D printing or selective laser sintering, but taking advantage of having a highly dense powder bed.
The LSD -3D printing, in particular, offers the potential of producing large (> 100 mm) and high quality ceramic parts, with microstructure and properties similar to traditional processing.
This presentation will give an overview of the milestones in the development of this technology, with focus on the latest results applied both to silicate and to technical ceramics.
Several Additive Manufacturing (AM) processes are based on the deposition of a powder to form a powder bed layer-by-layer, which typically has a low packing density (35-50%) and consequently hinders the ability of sintering ceramic parts to full density.
The layerwise slurry deposition (LSD) is an innovative process for the deposition of layers in AM. In the LSD, a slurry with no or small organic content is repetitively spread as thin layers on each other by means of a doctor blade. During the deposition, the ceramic particles settle to form thin layers with a high packing density (55-60%). When coupled with a printing head or with a laser, the LSD enables novel AM technologies inspired to the 3D printing or selective laser sintering, but taking advantage of having a highly dense powder-bed.
The LSD combined with inkjet binder printing (LSD-print) was applied to a submicron Al2O3 powder to produce samples which had a comparable density to uniaxially pressed samples, both in the green and in the sintered state.
Mechanaochemistry is an effective method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions.
Mechanaochemistry is an effective method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of
mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions.
Mechanaochemistry is an effective method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions.