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Eingeladener Vortrag
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In coal-fired power plants using oxyfuel combustion process with carbon capture and sequestration, instead of air, a mixture of oxygen and recirculated flue gas is injected in the boiler. A series of steels were exposed to CO2-SO2-Ar-H2O gas mixtures at 600 °C for 1000 h to compare their high temperature corrosion behavior. During the corrosion process, carburization, decarburization and recrystallization were observed underneath the oxide scale depending on the gas mixture and alloy composition. The conditions that lead to carburization are not yet completely understood, but decarburization can be simulated using thermodynamic and kinetic models. In this work, the results of these simulations are compared with measured values for one of the alloys that displayed a decarburized region. Since the mobility of carbon in the scale is not known, two strategies were adopted: simulation of alloy-atmosphere contact; and estimation of the carbon flux to produce the observed decarburization. The second approach might give an insight on how permeable to carbon the scale is.
In the beginning of the 1980s earth building has undergone a renaissance, which nowadays leads to an increasing use of load-bearing earth constructions and in particular, earth block masonry. At present, there are no common structural standards according to the semi-probabilistic design concept, which is the state-of-the-art in European standards.
A solid database is needed for the determination of the partial safety factor on the resistance side. Therefore, compressive strength tests were carried out with two types of earth blocks and two types of prefabricated earth mortar. The evaluation showed that the variation of the compressive strength was remarkably less than expected, which seems to indicate high quality standards of the components earth block and mortar with regard to industrial production.
On the basis of these results and together with the reliability method, a partial safety factor for earth block masonry subjected to compression was determined. The main aim of the research was the development of a first valid database for material parameters of earth block masonry with particular regard to statistical characteristics. The results showed that a common calculation method for earth block masonry based on partial safety factors following the valid masonry construction standard is feasible.
Multi residential buildings, developed as highly energy-efficient and airtight are nowadays often fitted with mechanical Ventilation Systems as a way to overcome shortcomings and even defects tinked to indoor climate. The presented study investigates the potential of low-emitting. natural building materials with hygroscopic properties to contribute to a healthy and comfortable indoor environment, while reducing the need for mechanical Ventilation.
A selection of natural building materials suitable for application as internal partition walls has been investigated with regards to their water vapour adsorption capacity.
Special emphasis was placed on the investigation of modified earth plasters as well as wood-based materials, used as wall lining to provide increased adsorption capacities.
In addition, tests on materials emissions (formaldehyde, VOCs, SVOCs and radon) as well as adsorption tests of airborne pollutants have been conducted in specially-designed fest chambers. All tests were performed at either the material or the component tevel.
Overall results to date suggest that natural materials contribute to an improved indoor environment quality through an increased moisture-buffering capacity, low emissions and the potential to adsorb airborne pollutants, therefore reducing the need for mechanical Ventilation.
Aluminium is still one of the most important contact metallisations for power electronic chips like MOSFETs or IGBTs. With a large difference in thermal expansion coefficients (CTEs) between aluminium and silicon and the temperatures generated in hot-spots during high power transients, these layers are prone to failure due to thermo-mechanical fatigue. Usually lifetime assessment is done by subjecting dedicated test specimens to standardised stress tests as e.g. active or passive thermal cycling. This paper proposes a novel method for accelerated stress testing and lifetime modelling of thin aluminium films in the high-cycle fatigue regime by isothermal mechanical loading. The proposed novel test method is suggested to complement or replace resource-demanding thermal cycling tests and allow simple in-situ monitoring of failure.
Evaluation of nano-sized internal oxidation in a Fe-13Cr alloy exposed to water vapor atmosphere
(2016)
The topotactic formation of nano-sized precipitates immediately under the internal oxide layer in a Fe-13Cr alloy exposed to oxidizing water vapor atmosphere was recently reported. The precipitates were identified as lath-shaped Fe-Cr spinel exhibiting a crystallographic orientation relationship with the ferritic matrix. The authors proposed that these precipitates could act as a precursor to the formation of the spinel layer observed in the adjacent part of the oxide scale.The occurrence of internal oxidation in Fe–Cr alloys subjected to similar conditions had been previously identified and directly correlated to the presence of water vapor. In the present work, we attempt to rationalize the processes occurring during the oxidation of this alloy through thermodynamic and kinetic analyses based on the CALPHAD approach, using the geometrical representation of phase equilibria and concepts developed to describe internal oxidation. The influence of water vapor on the mechanism and kinetics of formation of the nano-sized precipitates and its role in the overall oxidation process is also considered.
Visualization of surface modifications may be very challenging for coating/substrate systems of either almost identical optical constants, e.g. transparent films on substrates of the same material, or minor film thickness, substance quantity and affected area, e.g. ultra-thin or island films. Methods for visualization are optical microscopy (OM), imaging ellipsometry (IE), and referenced spectroscopic ellipsometry (RSE). Imaging ellipsometry operates at oblique incidence near Brewster angle of the bare, clean or unmodified substrate. In this configuration, reflected intensities are rather weak. However, the contrast to add-on and sub-off features may be superior. Referenced spectroscopic ellipsometry operates in a two-sample configuration but with much higher intensities. In many cases, both ellipsometric techniques reveal and visualize thin films, printed-pattern, laser-induced changes, and impurities better than optical microscopy. In particular for stratified homogeneous modifications, ellipsometric techniques give access to modelling and hence thickness determination. Modifications under investigation are polymer foil residue on silicon, laser-induced changes of ta-C:H coatings on 100Cr6 steel, imperfections of ta-C:H on thermal silicon oxide, degradation of glass, thin film tin oxide pattern on silicon, printed and dried pattern of liquids such as deionized water, cleaning agents, and dissolved silicone. © 2016 Elsevier B.V. All rights reserved.
The LEK94 is a Ni-base superalloy single crystal (SX) of the second generation, a materials class which is important for its high temperature creep resistance (>1000°C) in first stage blades of low-to-medium pressure gas turbines. Monocrystalline Ni-base superalloy SXs have a two-phase microstructure consisting of small cubes (' phase with the ordered L12 crystal structure, cube edge length: 500 nm), separated by thin channels (γ phase with fcc solid solution structure, channel width: 20 nm). The microstructural evolution during high temperature and low stress tensile creep has been thoroughly investigated previously, mainly for [001] loading, both in terms of dislocation activity (filling of γ channels, formation of dislocation networks, cutting of the γ’ phase) as well as phase coarsening (rafting, topological inversion). Other loading geometries have received less attention.
The present work studies high temperature and low stress creep deformation of the superalloy LEK 94 at temperatures around 1000°C, where rafting occurs. Differences between loading under different uniaxial, biaxial and triaxial stress states are discussed. Stereo-microscopy and g∙b analysis in the scanning transmission electron microscopy mode (STEM) are combined for microstructural analysis. The focus is set on the role of dislocation interactions with the aging microstructure. Both development in STEM characterization methods, as well as the roles of phase coarsening, γ channel filling, microstructural heterogeneity and γ’ phase cutting are discussed.
ISO 10156:2010 contains a test method and a calculation method for flammability of gases and gas mixtures for the selection of cylinder valve outlets. The calculation method is used also to classify gas mixtures according to the national and international dangerous goods and dangerous substances regulations, e.g. according to the UN Recommendations on the Transport of Dangerous Goods (UN TDG) and the Globally Harmonized System of Classification and Labelling of Chemicals (UN GHS). The calculation method for gas mixtures requires substance parameters of the single components. These are the coefficients for the fire potential (Tci) and for inerting ability, the so-called nitrogen equivalence (Kk), which have been estimated conservatively by means of flammability data.
BAM checked Tci and Kk values of ISO 10156:1996 using three-component diagrams (Flammable gas-Inert-Air) of the CHEMSAFE® database. The experimental fundamentals and the principles of the calculation method are summarized in this paper. The revised data for Tci and Kk values were adopted in the tables of ISO 10156:2010.
Furthermore, subcategorization of flammable gases has been proposed by a UN working group and shall be implemented in the GHS in the meantime. The subcategorization requires the lower flammability limit (LFL) as an additional indicator. Therefore, a test method and a calculation method for LFL were proposed by BAM and have been implemented in the new draft of ISO/CD 10156:2016.
The calculation method for gas mixtures is based on Le Chatelier’s rule and was extended by using the Kk values for inert components in the mixture. The calculated LFLs of methane-inert gas mixtures were compared with experimental values for different types of inert gases. It could be shown that calculated LFLs are in good agreement with experimental values if the Kk values derived from three-component flammability diagrams are used. Although using the Kk values of ISO 10156:2010 leads to higher deviations, the results are still on the safe side.
Complex materials (e.g., porous ceramics) need high resolution techniques at multi-scale levels. Microstructure is intimately linked to properties and performance. One technique (or even a few techniques) is not enough. X-ray refraction and CT are very powerful tools. Non-destructive characterisation and quantitative image analysis techniques (2D and 3D) are necessary to understand the anisotropy.
Several restoration projects of stained-glass windows have been performed in Lower Silesia (Poland) since 2010. The aim of the projects was to protect stained-glass windows against environmental impact of industial pollutants and acid rain by installing a protective glazing. The usefulness of protective glazing has been proved by climate measurements and determination of environmental impact before and after installation.
The presentation shows how the three-dimensional quantification of dislocations and their characteristic features, e.g. Burgers vector, line direction, dislocation density, is carried out at the transmission electron microscope in scanning mode (STEM) at Division 5.1 at BAM. Exemplarily, the methods are shown for Ni-base superalloy single crystals, for which a short introduction is given using further TEM techniques. Additional examples on low angle grain boundaries, nucleation of oxides at dislocations and interaction of dislocations and carbides are shown.
The content of the presentation was addapted, aiming at scientists who work within the DFG Priority Programme 1713 "Strong coupling of thermo-chemical and thermo-mechanical states in applied materials".
In Germany the damages on concrete motorways have increased during the past 15 years. This led often to a reduction of service life from 30 to 10 years. In spite of comprehensive research the reasons for these damages have not been clarified yet. But it is known that in this context the ASR plays a decisive role. Against this background ASR performance tests have been developed. However, these tests do not take into account the effects of mechanical loading due to cyclic traffic and climatic impact. Therefore in Germany the ASR research group 1498 was founded. The research group consists of three experimentally- and two multi-scale modelling oriented subprojects, which are working closely together. Selected findings of BAM’s experimental subproject SP4 are content of this contribution. The aim was to investigate the impact of a cyclic mechanical pre-damage on moisture transport. The pre-damaging was carried out on large-format beams using a cyclic four point bending test with a total number of 5 million load cycles. Thereby the damage process was monitored by using different NDT-techniques. After the mechanical pre-damaging, smallsized specimens were taken from loaded as well as unloaded areas of the large format beams. Absorption tests were carried out on these specimens using water and NaCl solution. Thereby moisture distribution was measured with Nuclear Magnetic Resonance (NMR) and Time Domain Reflectometry (TDR). Additionally, moisture suction was quantified integrally by means of gravimetric measurements. The analysis of the first test data shows that the mechanical loading influences the moisture transport.
The concrete prism test at 60°C facilitates accelerated testing of alkali-silica reactivity of aggregates within five months. Manual measurement is usually conducted to determine expansion of test specimen every 28 days. This conventional procedure gives only limited insight to expansion behaviour of ASR-affected prisms. Due to the large time intervals, expansion exceeding the critical value of 0.3 mm/m is likely to be noticed late. Continuous recording applied in this work resolves this problem and delivers beneficial information on the shape of the expansion curve.
Different types of aggregate have been tested applying continuous and manual measurement to the concrete specimens.
Models of ASR-induced expansion, available in the open literature, so far are validated with discontinuous data hardly tracing the modelled curve. Continuous measurement improves validation and further model development.
The martensitic steels X30CrMoN15-1 and 100Cr6 did not show any hydrogen enhanced wear in sliding friction tests against alumina balls in hydrogen gas environment. However, depending on the purity of the environment, unexpected high wear occurred at the alumina ball. The results of a tests series with a broad variation of test parameters are presented.
Sliding wear of martensitic steels in hydrogen – X30CrMoN15-1 and 100Cr6 – the role of water traces
(2016)
Initially the primary objective of the project has been the investigation of the influence of gaseous hydrogen on the wear of martensitic steels under heavy tribological stress. As a counter body an Al2O3 ball has been used because the material is inert and hard so that a low amount of wear was expected. If only the gas pressure is responsible for the absorption of hydrogen from the gas to pure α-iron it would require 15·105 MPa (~15 Mbar) to press 1 ppm into the material.
In the test series the Al2O3 balls showed in N2 and H2 atmosphere a higher wear compared to aerial experiments which showed a smaller wear track and a severer wear for the disc. Because of scattering and thereof following investigations it was shown that hydrogen has no noticeable influence but water traces in the gas are manipulating the outcome of the tests distinctly.
In coal-fired power plants using oxyfuel combustion process with carbon capture and sequestration, instead of air, a mixture of oxygen and recirculated flue gas is injected in the boiler. A series of steels were exposed to CO2-SO2-Ar-H2O gas mixtures at 600 °C for 1000 h to compare their high temperature corrosion behavior. During the corrosion process, carburization, decarburization and recrystallization were observed underneath the oxide scale depending on the gas mixture and alloy composition. The conditions that lead to carburization are not yet completely understood, but decarburization can be simulated using thermodynamic and kinetic models. In this work, the results of these simulations are compared with measured values for one of the alloys that displayed a decarburized region. Since the mobility of carbon in the scale is not known, two strategies were adopted: simulation of alloy-atmosphere contact; and estimation of the carbon flux to produce the observed decarburization. The second approach might give an insight on how permeable to carbon the scale is.
Hydroxyapatite (HA) is a bioceramic material with excellent biological properties. However, these properties are strongly dependent of ist crystallinity degree, with high values of crystallinity associated to poor resorption rates and bioactivity. This work evaluates the properties of HA samples produced by two different free-forming conformation methods, CNC machining and 3D printing. In both cases, porous gypsum samples were produced and subsequently converted into HA in a reaction with di-ammonium hydrogen phosphate at 100°C and pH 8. A total conversion of the samples was achieved after 36 h independently of the conformation method used. The microstructure, however, before and after the conversion is showed to be dependent on the method used. After conversion the machined samples achieved a Maximum compressive strength of 3.5 MPaforporosities of circa 80%, while 3D printed samples achieved a tensile strength of 2.0 MPa by porosities of 61%.
By means of an effective medium (EMA) based approach, it is possible to use spectroscopic ellipsometry to determine the mixing ratios between air and material in porous dielectrics and calculate a quantitative value of the porosity for these materials. As this method is model-based, it is very difficult to provide a quantitative measure for the accuracy of porosity values determined by this method. Valuable additional information can often be obtained by combining ellipsometry with other complementary methods. In the present study, the ellipsometry results were validated by Electron Probe Microanalysis (EPMA) with the option of layer analysis (by the socalled “STRATAGem” approach), gravimetry, and electron microscopy. We analysed porous TiO2 thin layers synthesised by means of a template synthesis Approach (evaporation induced self assembly).
Ellipsometry measurements on porous samples are difficult to analyse due to the complexity of the models necessary. Often it is difficult to decide if the measured data contains enough information to successfully determine the target quantities (mixing ratio, dielectric function of the matrix material). One method to decrease the complexity of the fit and therefore use the measurement data most efficiently is a multi-sample analysis. In the present case, multi-sample analysis was used for determining the porosity factors of the individual layers while using one common set of dielectric function values for the matrix in all cases.
While the results of the fit analysis in this case can be used to show the feasibility and also the limitations of the multi-method approach, the porosity values themselves show a promising agreement between the Independent methods. It can therefore be concluded that determining porosity values with ellipsometry is in accordance to other methods to the level of accuracy provided by the complementary methodologies.
It has been shown that selected types of substituents are able to vary the oxidative behavior of multi-walled carbon nanotubes. Such substituents investigated were sterically hindered secondary amino groups bonded in grafted piperidine units and covalently bonded bromine groups. Their interference and activity was preliminary determined in the model cumene and then in oil diesel fraction and low density polyethylene oxidation reactions. Results obtained indicate that chemical linking of amine moieties containing –NH groups directly to the carbon nanotubes core significantly increases their intrinsic anti-oxidative capacity while the grafting of Br-groups provokes the opposite functioning of the pristine samples. This inference was proved by thermogravimetric and differential thermal analysis of the polyethylene composites and experiments on profound aerobic oxidation of petroleum naphthenic fraction derived from the commercial Baku oils blend diesel cut.
Quality control requirements imposed on assays used in clinical diagnostics and point-of-care-diagnostic testing (POCT), utilizing amplification reactions performed at elevated temperatures of 35 to 95 °C are very stringent. As the temperature of a reaction vessel has a large impact on the specificity and sensitivity of the amplification reaction, simple tools for local in situ temperature sensing and monitoring are required for reaction and assay control. We describe here a platform of stem-and-loop structured DNA hairpins (molecular beacons, MBs), absorbing and emitting in the visible and red spectral region, rationally designed for precise temperature measurements in microfluidic assays for POCT, and their ap-plication for temperature measurements in a common DNA-based molecular biological assay utilizing thermophilic helicase-dependent amplification (tHDA). Spectroscopic studies of these MBs, rationally designed from DNA se-quences of different thermal stabilities, chosen not to interact with the DNA probes applied in the nucleic acid amplification assay, and temperature-dependent fluorescence measurements of MB-assay mixtures revealed the suitability of these MBs for temperature measurements directly in such an assay with a temperature resolution of about 0.5 °C without interferences from assay components. Combining two spectrally distinguishable MBs provides a broader response range and an increase in temperature sensitivity up to 0.1 °C. This approach will find future application for temperature monitoring and quality control in commercialized diagnostics assays using dried reagents and microfluidic chips as well as assays read out with tube and microplate readers and PCR detection systems for temperature measurements in the range of 35 to 95 °C.
The novel heat treatment concept, “quenching and partitioning” (Q&P) has been developed for high strength steels with enhanced formability. This heat treatment involves quenching of austenite to a temperature between martensite start and finish, to receive a several amount of retained austenite. During the subsequent annealing treatment, the so called partitioning, the retained austenite is stabilized due to carbon diffusion, which results in enhanced formability and strength regarding strain induced austenite to martensite transformation. In this study a Q&P heat treatment was applied to a Fe-0.45C-0.65Mn-0.34Si-13.95Cr stainless martensite. Thereby the initial quench end temperature and the partitioning time were varied to characterize their influence on microstructural evolution. The microstructural changes were analysed by dilatometer measurements, X-ray diffraction and scanning electron microscopy, including electron back-scatter diffraction. Compression testing was made to examine the mechanical behaviour. It was found that an increasing partitioning time up to 30 min leads to an enhanced formability without loss in strength due to a higher amount of stabilized retained and reversed austenite as well as precipitation hardening.
The book „Electropolishing“ by M. Buhlert is dealing with the electrolytic brightening, smoothing and deburring of technical materials like steel, copper, brass, aluminum, titanium and magnesium. The book content covers the basics and the main influencing parameters of the electropolishing process and provides detailed and application orientated procedure information for technical relevant materials.
After a brief introduction into the topic of electrolytic polishing in the first chapter, the author gives a detailed description of the basic electrochemical reaction mechanisms in the second chapter. The reader will also be informed about the physical and chemical parameters, which control the electrochemical removal process. Additionally, the author reports about the advantages and disadvantages of electropolishing.
The third chapter provides a detailed insight into the influencing manufacturing parameters affecting the results of the electropolishing process. Distinct aspects of the manufacturing e.g. workpiece preparation, electrolyte composition, polishing time, electrolyte temperature and alloy compositions will be discussed in detail by the author.
In the fourth and fifth chapter, the author gives useful hints and information about the parameter variation and the suitable handling of hull cells for the optimization of the removal process, followed by a particular overview about material specific electrolyte mixtures for common-used technical metals and alloys, like steel, aluminum, brass, magnesium, copper and titanium.
The sixth chapter of the book provides many selected manufacturing results and investigations on electropolishing of different metals and alloys, which allows the reader the opportunity to develop a systematic understanding of the topic and to adopt the knowledge on the optimization of his own electropolishing process.
Finally, the book concludes with a brief chapter about some remarks with respect to the work safety and environmental efforts.
In summary, this book contains a very detailed and clear arranged overview about the electropolishing method for the surface optimization process. For this reason, it is a suitable and useful lecture for people, which want to take an in depth look into the topic in order to start using this method or are interested in optimize their existing electropolishing processes.
The corrosion resistance of martensitic stainless steels (MSS) depends strongly on the chemical composition and the applied heat treatment. Both determine the distribution of the alloying elements in the microstructure and the resulting material properties. The addition of nitrogen is known to be beneficial for the pitting corrosion resistance of stainless steels. In case of MSS this effect is not only connected to nitro-gen itself because nitrogen can be used to substitute carbon which also influences the result of the heat treatment process. This paper shows the effect of nitrogen on the corrosion resistance in relation to the hardening process of MSS. Therefore the effects of austenitization temperature and cooling rate on microstructure, hardness and corrosion resistance were studied on the MSS X30CrMoN15 1 and X50CrMoV15. The effect of different cooling rates was studied using the jominy end quench test. The changes in corrosion resistance were detected with electrochemical potentiodynamic reactivation (EPR) and by the determination of critical pitting potentials. Besides this experimental approach thermodynamic calculations with the software thermocalc will be presented and used for the interpretation of the effect of nitrogen on the corrosion resistance of MSS.
Hydrogen can have an extreme degradation effects in steels, particularly concerning the mechanical properties. These effects can lead to hydrogen assisted cracking in micro-alloyed high strength steels during fabrication and/or operation in industrial applications. The Carrier Gas Hot Extraction method, which functionally combines a mass spectrometer with a Thermal Desorption Analysis process, was used for the detection of ultra-low diffusible hydrogen concentrations in the material specimens. The work shows the interaction between hydrogen and lattice defects in different micro-alloyed materials and HAZ. These steels were prepared in a quenched and tempered condition and in a thermo-mechanically rolled condition. The trapping characteristics of two steel grades, S690QL and S700MC, were studied with respect to the activation energy dependent on carbon content and micro-alloying elements such as Ti, Nb, Mo, Cr and V. The two steel grades exhibited several types of traps: carbide formations, dislocations and/or grain boundaries were common, which can influence activation energy and hydrogen solubility. The type and dimension of inclusions or particles also affected the hydrogen trapping behavior. A decrease of carbon and specific alloying elements in MC steels led to a change in the activation energy binding the trapped hydrogen. This thermo-mechanically hot
rolled steel revealed an increased interaction between hydrogen
and precipitations. The higher carbon content in the
quenched and tempered steel led to a higher interaction
between hydrogen and iron carbide, specifically in the
martensitic phase. Furthermore,the trapping behavior in HAZ showed a significant increase in activation energy, especially in the coarse grained microstructure.
Three high strength Nb-, Ti- and Ti+V- bearing S690QL steels were welded to investigate and compare the effects of microalloy addition on HAZ toughness. Charpy V notch impact tests from three microalloyed welds under different cooling rates have been performed. Fractographic examination shows that several factors including large-sized grain, upper bainite or hard second phase, interact to determine the brittle fracture mode and impaired toughness of Nb bearing weld at high heat input. In contrast to this reduced toughness, Ti bearing welds exhibits satisfied toughness regardless of at a fast or slow cooling rate as a result of limited austenite grain and refined favourable intragranular acicular ferrite structure. Moreover, in the case of such refined structure as matrix, TiN particles are found to be irrelevant to the fracture process and crystallographic misorientation results also confirms that high angle boundaries between fine ferrites plates provide much effective barrier for crack propagation and contribute to improved toughness.
We report on the in situ investigation of the Al13 sulfate synthesis by WAXS. Al13 sulfates were crystallized by precipitating hydrolyzed aluminum solutions by the addition of sodium sulfate. The measurements were performed using an acoustic levitator. The study provides information about the intermediates during the crystallization process.
Microstructure-property connections for porous ceramics: The possibilities offered by micromechanics
(2016)
Microstructure of porous ceramics is highly “irregular”: it comprises pores and microcracks of diverse shapes and orientations.
This makes their quantitative modeling challenging, and one
often resorts to empirical relations containing Fitting Parameters and having somewhat uncertain range of applicability. We review the substantial progress made in modeling of “irregular” microstructures that does not seem to have been sufficiently utilized in the context of ceramics. We discuss the possibilities offered by micromechanics in developing microstructure–property relations for porous microcracked ceramics. After an overview of relevant micromechanics topics, we focus on several issues of specific interest for ceramics: nonlinear stress–strain behavior, effective elastic properties, and thermally induced microcracking. We discuss extraction of microscale Parameters (such as strength of the intergranular cohesion, density of cracks and pores, etc.) from macroscopic data and identify the extent of uncertainty in this process. We also argue that there is no quantitative correlation between fracturing process and the loss of elastic stiffness.
Texture formation in amorphous Al86Ni6Y4.5La1.5Co2 splats by thermal and mechanical treatment
(2016)
The crystallization behavior of amorphous Al86Ni6Y4.5La1.5Co2 splats was analyzed by differential scanning calorimetry (DSC) and X-ray diffraction (XRD). Rietveld refinement was used to analyze the preferred orientation of fcc aluminum nanocrystals in the residual amorphous matrix after annealing. Fiber textures in [200] and [220] directions were found after heating to 360 C. The influence of cold rolling on the preferred crystal orientation was studied as a function of the thickness reduction of the specimen. It was found that cold rolling significantly increases the (220) texture, while the (200) texture remains unchanged. Based on the experimental results the formation of (220) and (200) texture during the crystallization of the amorphous splats was ascribed to two different processes, internal stresses induced during splat formation or cold-rolling.
Glass is an amorphous material. When compared to steel, both its density and weight is three times lower. Its high theoretical strength makes it stand out as a premier material for a variety of applications. One such application is acting as a pressure resistant vessel for gas storage. Because glass has a high theoretical strength this makes it potentially suitable to withstand much higher pressures than steel or composite vessels. As a result of its brittle character, glass breaks when reaching a critical stress level. Therefore, the stress distribution during pressure load needs to be homogeneous without local stress peaks. At those peaks an initial crack will occur and the material will break. This PhD thesis is primarily concerned with the determination of the strength of several structures made of single hollow glass fibers during inner pressure treatment. Therefore, different kinds of hollow glass structures with varying parameters of shape and dimension were examined concerning their strength by determining the burst pressure. The burst pressure method was compared to the tensile test method, which poses the common test method for examining the strength of a material. The conclusion reached was that both test methods lead to comparable results and therefore, the burst pressure method poses an adequate tool for examining the strength of a hollow material against inner pressure. Another tool used in this thesis is the Finite Elements Method (FEM) simulation of internal stress and expansion of glass structures during pressure treatment. FEM was used to validate the burst pressure test results. A few selected material parameters needed to be incorporated, most notably the Young’s Modulus. Therefore, the expansion of single glass fibers was measured with light microscope during pressure load. Within the parameters of expansion, wall thickness and applied pressure, the Young’s Modulus was calculated with the Barlow’s Formula. According to the results, different two-dimensional models from single fibers to complex structures with up to 1000 single fibers were constructed and simulated with the CFD software Comsol Multiphysics. The expansion as well as the principal stress during pressure load was calculated. Different dimensions as well as different geometries of the glasses were considered to find a structure with the highest possible free volume and at the same time as less stress peaks as possible. This calculation was made in order to determine the best structure for gas storage. For this purpose the calculations were done with different dimensions of round single fibers right up to hexagonal structures consisting of more than one thousand round single fibers, which resulted in constant expansion of the structure. Furthermore, the problem of occurring interspaces between round single fibers, regarding their burst pressure-decreasing influence, was approached. Closing these interspaces with glass or other materials to avoid unsolicited pressure load led to increased strength of the structure and low storage capacities due to the increased weight and less free inner volume. The behavior of hexagonal fibers was determined as single fiber as well as in bundled condition. The walls between two hexagonal single fibers with applied inner pressure showed homogeneously distributed stress. Merely the outer walls without counter pressure showed high deformation and high structural stress. Based on that knowledge, several structures were modeled varying in different aspects. The fibers with hexagonal shape showed optimal stress distribution and high storage capacities because of high free inner volume, provided that these fibers are surrounded by additional fibers with identical inner pressure. Reducing the wall thickness for even higher free inner volume led to similar distribution but higher stress and expansion. To overcome the problem with the high stress at the outer fibers, the influence of outer fibers with different shape and dimension was simulated as well as the influence of solid glass fibers at the outer layer of the structure. The results showed that a structure with hexagonal thin-walled fibers should be surrounded by round fibers with higher wall thickness. This way the high stress peaks at the outer fibers are lowered. The examined practical strength of glass is about 100 to 1000 times lower than the theoretical strength. This is caused by defects, which may occur at the glass surface by handling or inside the material by defective production. Since the modeled results are based on the theoretical strength, the optimal wall thickness with a good compromise of strength and free inner volume needs to be found in practical tests. If further handling of the structures is necessary, an outer layer of solid fibers works as a protection layer against damages at the outer hollow glass fibers and increases the strength. Additionally, the influence of collapsing fibers inside a structure on the remaining system has been modeled as well as the influence of defects like holes or cracks at the surface or manufacturing induced defects inside the material. Any kind of defect leads to areas of high stress, whereby failure occurrence will be encouraged. In order to approve the theoretical results, the simulated structures were compared to the previously manufactured and tested ones. Due to the burst pressure test results, the tested structures showed low strength compared to the theoretical strength. This was primarily caused by the existence of defects in the material and on the surface of the glass structures. Therefore, the production process needs to be optimized in order to prevent such defects. Furthermore, an additional protection against outer influence like air humidity or the physical contact to other materials is required.
Pharmacologically active compounds are omnipresent in contemporary daily life, in our food and in our environment. The fast and easy quantification of those substances is becoming a subject of global importance. The fluorescence polarization immunoassay (FPIA) is a homogeneous mix-and-read format and a suitable tool for this purpose that offers a high sample throughput. Yet, the applicability to complex matrices can be limited by possible interaction of matrix compounds with antibodies or tracer.
Caffeine is one of the most frequently consumed pharmacologically active compounds and is present in a large variety of consumer products, including beverages and cosmetics. Adverse health effects of high caffeine concentrations especially for pregnant women are under discussion. Therefore, and due to legal regulations, caffeine should be monitored. Automated FPIA measurements enabled the precise and accurate quantification of caffeine in beverages and cosmetics within 2 min. Samples could be highly diluted before analysis due to high assay sensitivity in the low μg/L range. Therefore, no matrix effects were observed.
The antiepileptic drug carbamazepine (CBZ) is discussed as a marker for the elimination efficiency of wastewater treatment plants and the dispersion of their respective effluents in surface water. The development of a FPIA for CBZ included the synthesis and evaluation of different tracers. Using the optimum tracer CBZ-triglycine-5-(aminoacetamido) fluorescein, CBZ concentrations in surface waters could be measured on different platforms: one sample within 4 min in tubes or 24 samples within 20 min on microtiter plates (MTPs). For this study, a commercially available antibody was used, which led to overestimations with recovery rates up to 140% due to high cross-reactivities towards CBZ metabolites and other pharmaceuticals.
For more accurate CBZ determination, a new monoclonal antibody was produced. In this attempt, methods for improving the monitoring during the production process were successfully applied, including feces screening and cell culture supernatant screening with FPIA. The new monoclonal antibody is highly specific for CBZ and showed mostly negligible cross-reactivities towards environmentally relevant compounds. Measurements at non-equilibrium state improved the sensitivity and selectivity of the developed FPIA due to slow binding kinetics of the new antibody. Additionally, this measure enables for CBZ determination over a measurement range of almost three orders of magnitude. The comprehensively characterized antibody was successfully applied for the development of sensitive homogeneous and heterogeneous immunoassays.
The new antibody made the development of an on-site measurement system for the determination of CBZ in wastewater possible. After comprehensive optimization, this automated FPIA platform allows the precise quantification of CBZ in wastewater samples only pre-treated by filtration within 16 min. Recovery rates of 61 to 104% were observed. Measurements in the low μg/L range are possible without the application of tedious sample preparation techniques.
Different FPIA platforms including MTPs, cuvettes and tubes were successfully applied. For the choice of the right format, the application field should be considered, e.g. desired sample throughput, usage for optimization or characterization of antibodies or if a set-up for routine measurements is sought for. For high sample throughput and optimization, FPIA performance on MTPs is advantageous. The best results for the application to real samples were obtained using kinetic FP measurements in cuvettes.
This chapter discusses different approaches for the densification of rock salt powders via compaction and sintering, focusing on the use of powder qualities obtained by crunching and milling of the natural rock salt. The chapter also examines the effect of compaction pressure, time and temperature on sintering of rock salt. Natural rock salt samples were crushed and milled in a disc mill to obtain fine powders in an experiment. The hot stage microscope allowed observing the in-situ volumetric shrinkage to be determined during the sintering process by measuring the area of the sample's projection in an optical setup by a CCD camera. Images were collected at a rate of 40 frames per minute. After the application of high pressures, the obtained samples are translucent and show the formation of macroscopic crack. Powder compacts prepared by uniaxial pressing, at different maximum pressures, were annealed at a constant heating rate (10 K min-1) to different maximum temperatures. These experiments were performed in a conventional sintering furnace under ambient atmosphere.
3-Aminovinylquinoxalines are readily accessible from (hetero)aryl glyoxylic acids or heterocyclic π-nucleophiles by consecutive four- and fivecomponent syntheses in the sense of an activation-alkynylation-cyclocondensation-addition sequence or glyoxylation-alkynylation-cyclocondensation-addition sequence in good yields. The title compounds are highly fluorescent with pronounced emission solvatochromicity and protochromic fluorescence quenching. Time-resolved fluorescence spectroscopy furnishes radiative and nonradiative fluorescence decay rates in various solvent polarities. The electronic structure is corroborated by DFT and TD-DFT calculations rationalizing the observed spectroscopic effects.
Selective Electron Beam Melting (SEBM) is a promising powder bed Additive Manufacturing (AM) technique for near net-shape manufacturing of high-value titanium components. However, as with every emerging technique, the manufacturing processes can still be greatly improved and optimised. In particular, the links between AM settings and the resulting sample porosity is of great interest, as the fatigue life of SEBM parts is currently dominated by the presence of porosity. In this study, the size, volume fraction, and spatial distribution of the pores in model samples have been characterised in 3D, using X-ray Computed Tomography (CT), and correlated to the SEBM process variables. A strong relationship was found with the different beam strategies used to contour, and infill by hatching, a part section. The majority of pores were found to be small spherical gas pores, concentrated in the infill hatched region. Rarer irregular shaped pores were mostly located in the contour region and have been attributed to a lack of fusion between powder particles.
Wood borers in structural timber - European regulations for their control and can TTIP comply?
(2016)
The control of wood boring beetles in structural timber is uniformly regulated in the European Union. Registration and authorization of wood preservatives for the European market has to follow a regulated procedure as described under the Biocidal Product Directive “EU 528/2012”. Non-biocidal measures of control such as by physical means are regulated individually by each member state on the national level. The Biocidal Product Directive demands voluminous data sets for product identity, environmental and health risk assessments, proof of efficacy, and management strategies to avoid the development of resistance, just to name the most important.
With TTIP (Transatlantic Trade and Investment Partnership) on the horizon, it must be expected that wood preservatives coming from the North American Market to Europe and vice versa will mutually be recognized in the future, despite existing differences in registration requirements. The presentation will focus on major differences in standard efficacy tests for wood preservatives with claims for beetle control, which, next to others, have to be passed before product placement on the respective market. Desirable needs for future harmonizing will be identified in order to overcome consumers distrust on each side of the partners.
Similar to the success story of digital photography a major upheaval has been observed in digital industrial radiology. This paper is split into 3 parts:
Part 1: Film Replacement and Backscatter Imaging: Computed radiography with phosphor imaging plates substitutes film applications. Digital Detector Arrays enable an extraordinary increase of contrast sensitivity in comparison to film radiography. The increased sensitivity of digital detectors enables the efficient usage for dimensional measurements and functionality tests substituting manual maintenance. The digital measurement of wall thickness and corrosion status is state of the art in petrochemical industry. Photon counting and energy discriminating detectors are applied up to 300 Kv provide increased thickness dynamic and material discrimination by synchronously acquisition of images of the high and low energy part of the spectrum. X-ray back scatter techniques have been applied in safety and security relevant applications with single sided access of source and detector. First inspections of CFRP in aerospace industry were successfully conducted with newly designed back scatter cameras. Numeric modeling is used to design X-Ray optics and inspection scenarios as well as conducting RT training.
Part 2: Computed tomography (CT)
Part 3: Micro Radiography and Micro CT.
Designing artificial macromolecules with absolute sequence order represents a considerable challenge. Here we report an advanced light-induced avenue to monodisperse sequencedefined functional linear macromolecules up to decamers via a unique photochemical approach. The versatility of the synthetic strategy—combining sequential and modular concepts—enables the synthesis of perfect macromolecules varying in chemical constitution and topology. Specific functions are placed at arbitrary positions along the chain via the successive addition of monomer units and blocks, leading to a library of functional homopolymers, alternating copolymers and block copolymers. The in-depth characterization of each sequence-defined chain confirms the precision nature of the macromolecules. Decoding of the functional information contained in the molecular structure is achieved via tandem mass spectrometry without recourse to their synthetic history, showing that the sequence information can be read.We submit that the presented photochemical strategy is a viable and advanced concept for coding individual monomer units along a macromolecular chain.
In this study a metal-matrix-composite with aluminum matrix and Al2O3 particles was investigated with x-ray refraction topography and in-situ tensile loading. It could be observed that after reaching a certain load the specific surface increased steadily. However, the classical radiographs taken for comparison show no damage in the sample.
In-line laser thermography for crack detection at elevated temperature: A Numerical modeling study
(2016)
The detection and characterization of cracks prior to damage is a technologically and economically highly significant task and is of very importance when it comes to safety-relevant structures. The evaluation of a components life is closely related to the presence of cracks in it. Laser thermography has already high capability for the detection of surface cracks and for the characterization of the geometry of artificial surface flaws in metallic samples. Crack detection in metallic samples at high temperature is highly significant in present manufacturing scenario. During the casting process of billets, surface cracks form, due to the suboptimal cooling rates. These cracks reduce value of the billet and must be removed using machining process after cooling. This secondary process increases cost of manufacturing. In this work we developed a heat transfer model for laser thermography to study the thermal contrast variation with increase in surface temperature using finite element method (FEM). Here we are mainly concentrating the capability of the scanning laser thermography in crack detection which are in elevated temperature and numerical modeling study of thermal contrast variation of crack with respect increase in metal surface temperature. This study is important to prove the capability of laser thermography for crack detection in elevated temperature. Since we are using High power CW Laser to local heating of the metal surface which can give relatively high thermal contrast even at elevated temperature compare to other heating source. Here we are modeled and simulated 2D laser scanning across a surface breaking crack and developed an algorithm to produce the vicinity of crack. The algorithm we developed applied for various surface temperature data. And validated the credibility of the algorithm with experimental data.
A significant number of German concrete motorway pavements have shown damage only a few years after construction. The alkali-silica-reaction (ASR) is often one of the reasons for this damage. German guidelines and regulations focus on the optimisation of the concrete composition to avoid damage due to ASR. Moreover, diverse research projects have dealt with the development and optimisation of ASR performance test methods with and without external alkali supply. However, the influence of other parameters on the occurrence and intensity of a damaging ASR had not yet been taken into account. Such parameters include, e.g., insufficient curing and the modifications of concrete’s porosity due to the use of slip form pavers. Likewise, the increased traffic loading had not yet been considered. The Federal Institute for Materials Research and Testing (BAM) assesses these parameters and processes in a number of projects. These projects aim primarily to increase the durability of the concrete pavements, in particular by improving preventive measures that may be taken before or after the construction of concrete pavements. This paper gives a short overview of BAM’s projects concerning ASR in concrete pavements. Furthermore, results regarding the influence of the cyclic traffic loading on ASR are presented.
A significant number of German concrete motorway pavements have shown damage only a few years after construction. The alkali-silica-reaction (ASR) is often one of the reasons for this damage. German guidelines and regulations focus on the optimisation of the concrete composition to avoid damage due to ASR. Moreover, diverse research projects have dealt with the development and optimisation of ASR performance test methods with and without external alkali supply.
However, the influence of other parameters on the occurrence and intensity of a damaging ASR had not yet been taken into account. Such parameters include, e.g., insufficient curing and the modifications of concrete’s porosity due to the use of slip form pavers. Likewise, the increased traffic loading had not yet been considered. The Federal Institute for Materials Research and Testing (BAM) assesses these parameters and processes in a number of projects. These projects aim primarily to increase the durability of the concrete pavements, in particular by improving preventive measures that may be taken before or after the construction of concrete pavements. This paper gives a short overview of BAM’s projects concerning ASR in concrete pavements. Furthermore, results regarding the influence of the cyclic traffic loading on ASR are presented.
We investigated the efficiency of phase gratings, i.e., the visibility upon variation of different parameters. Rotating around an axis parallel to the grid lines of the phase grating changes the grating’s shape and thereby the initial distribution of phase shifts. This yields high visibilities for shorter propagation distances than derived from box shapes. Tilting the grating in the scattering plane allows continuous tuning of the grating’s height that corresponds to an ideal phase shift for a particular photon energy. This opens the way for tuning the design energy suitable for the material under investigation. Our study included simulations for monochromatic sources with the sampling procedure for rectangular and triangular phase gratings.
Joining of dissimilar material has become highly popular research subject in the automobile industry due to the reduced weight and thereby increasing the fuel efficiency. Infrared thermography can be used as a natural tool to measure the temperature near the welding region and correlate the distribution of temperature to the weld quality. In the present work the quality of the dissimilar welded sample is identified using the temperature distribution in the vicinity of the weld pool region. A numerical model for CMT continues welding process has been modeled and simulated for the first time and compared with the experimental measurement.
Electron Beam Melting (EBM) as a means of Additive Manufacturing (AM), is of interest for the fabrication of intricate geometries for cellular materials in areas where complex architectures are needed, e.g. biomedical implants. Most studies have focused on specific geometries and so the effect of the structure on mechanical performance is not well understood. Many kinds of micro- and macro-scale defects can arise in additively manufactured components, so assessment of their influence on properties is needed. In this work, lattices of Ti-6Al-4V having a cubic structure have been manufactured by EBM, and the effect of heat treatments above and below the β-transus temperature on microstructure and compression response have been investigated. The former modifies only slightly the α + β structure and mechanical performance whereas the latter leads to coarse alternating α and β lamellae packets and α at the prior grain boundaries with a 10% loss in yield strength. The variation in the compressive yield stress with strut diameter is in good accord with simple models based on compressive deformation rather than shearing or buckling. Internal pores for struts aligned with the build direction are found around the edges of the solid form, in regions which seem to be associated with the EB scan pattern. Struts normal to the build direction show more significant defects but their redundancy means that they do not compromise the compressive performance in the build direction. Using a particle size in the range 45–100 μm minimum weld-track sizes were experimentally and numerically identified to be 176 and 148 μm in depth respectively with a depth-to-width ratio of 0.55. This produced a beam pass of the order of 300 μm oversizing small features (struts of 0.4 and 0.6 mm nominal diameter) when a contour around the strut periphery was applied.