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Dieses Dokument fasst den Projekfortschritt des BAM-Projektes "Ermittlung geeigneter Wärmeführungen zur Wasserstoffreduktion
beim Schweißen höherfester Feinkornbaustähle mit modifiziertem
Sprühlichtbogen" im Rahmen des Fachausschusses 1 "Schweißmetallurgie & Werkstoffverhalten" des DVS e. V. zusammen.
Dieses Dokument fasst den Projekfortschritt des BAM-Projektes "Ermittlung geeigneter Wärmeführungen zur Wasserstoffreduktion beim Schweißen höherfester Feinkornbaustähle mit modifiziertem Sprühlichtbogen" im Rahmen des Fachausschusses 1 "Schweißmetallurgie & Werkstoffverhalten" des DVS e. V. zusammen.
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.
The objective of the present work was the investigation and demonstration of the potential of sol-gel alumina layers as corrosion protection of commercial power plant steels under oxyfuel conditions. The starting points of this work were modified Yoldas-sols which were developed in the BAM-department 5.6. These sols were suitable for the spin-coating method only. The application of coatings on tubes by spin-coating is impossible. Therefore, the chemical composition of the modified Yoldas-sol had to be adapted to the dip- and spray-coating techniques.
Exclusively the sol with the composition s-0.52-6-1.5 with a nitrate/aluminium ratio of 0.52; a solid content of 6 wt.% and a PVP (binder) content of 1.5 wt.% could fulfill the necessary criteria: long-term stability; formation of a dense, crack-free and well adhered layer on polished metal surfaces; as well as high protective abilities against corrosion in H2O-CO2-O2-SO2.
The commercial power plant steel X20CrMoV12-1 (X20) and the steel X12Cr13 were successfully coated with the sol s-0.52-6-1.5 by means of the dip-coating method. An at least 400 nm thick alumina layer (δ-Al2O3) is necessary to ensure the corrosion protection of these steels. The corrosion of the coated samples compared to that of the uncoated ones was significantly reduced, even after 1000 h of exposure in a H2O-CO2-O2-SO2 atmosphere at 600°C. Sulfur and carbon were not detected at the substrate surface or beneath the coating. Hence the transport of the flue gas components SO2 and CO2 into as well as through the alumina layer could be hindered. The diffusion of the alloying elements (Cr, Mn, Si) into the alumina layer resulted in the formation of mixed oxides like δ-(Al,Cr)2O3. Formation of such phases considerably contributed to the corrosion protection.
The long-term stability of the sol s-0.52-6-1.5 and the high protective abilities of the alumina layer on commercial power plant steels provide a good basis for an industrial application.
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.
Dark-field Transmission electron microscopy (DFTEM) results were obtained and presented. The results are discussed with regard to additional microstructural characterisation of the primyra Phase and creep experiments of alloy 2618A. Different methods to determine the volume fractions of precipitate phases are presented.
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.
Entwicklung eines Verfahrens zur Untersuchung der Heißrissresistenz lasergeschweißter Verbindungen
(2016)
In den letzten Jahrzehnten hat sich die Strahlschweißtechnik signifikant weiterentwickelt und als effizientes und wirtschaftliches Werkzeug in der Industrie etabliert. Für die Untersuchung der Heißrissresistenz verschiedener Werkstoffe existieren zahlreiche eigen- und fremdbeanspruchende Tests. Diese wurden aber speziell für andere Schweißverfahren, insbesondere das Lichtbogenschweißen, konzipiert.
Daher besteht die Notwendigkeit eines geeigneten Heißrisstests, bei dem Werkstoffe realen Strahlschweißbedingungen ausgesetzt werden können. Die Entwicklung sowie die Standardisierung einer aussagekräftigen experimentellen Methode stellen einen wichtigen Schritt auf dem Weg zur Vermeidung von Heißrissen und damit für die Gewährleistung der Sicherheit von gefügten Bauteilen dar. Ziel der Forschungsarbeiten ist es, einen geeigneten Test zur effektiven Untersuchung der Heißrissanfälligkeit von lasergeschweißten Verbindungen zu konzipieren und zu entwickeln.
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.
Der Vortrag gibt einen Überblick die deutsche Ressortforschung. Neben einer Einordnung in das deutsche Wissenschaftssystem werden in einem historischen Überblick die Besonderheiten der Ressortforschung diskutiert. Besonderes Augenmerk wird der Frage gewidmet „Was ist gute Ressortforschung“. Kritisch erscheint besonders die Vereinbarkeit von exzellenter Wissenschaft und seriöser und unabhängiger Politikberatung.
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.
Zur Vermeidung der schädigenden Alkali-Kieselsäure-Reaktion in Betonbauwerken wird die Alkalireaktivität von Gesteinskörnungen im Vorhinein getestet. Der 60°C-Betonversuch ermöglicht eine vergleichsweise schnelle Einschätzung nach fünf-monatiger Testzeit. Dazu wird die Dehnung von Betonprüfkörpern, die mit der zu testenden Gesteinskörnung hergestellt wurden, manuell alle 28 Tage gemessen. Ein alternatives, an der BAM in den vergangen Jahren entwickeltes Verfahren setzt Dehnungssensoren ein, um kontinuierlich und online zu messen. Die Dehnungskurven sind eine gute Grundlage sowohl für die Prognose vom Expansionsverhalten während des Tests als auch für die Validierung von Expansionsmodellen.
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.
Einfluss des Schwefelgehalts auf die Korrosionsbeständigkeit des nichtrostenden Stahls 1.4404
(2016)
Die Korrosionsbeständigkeit nichtrostender Stähle wird maßgeblich von ihrer chemischen Zusammensetzung bestimmt. Der tendenzielle Einfluss ist für die Hauptlegierungselemente in der wissenschaftlichen Fachliteratur beschrieben. Bei Begleitelement Schwefel gibt es dagegen keine konkreten Untersuchungen die belegen, ab welchem Gehalt mit einer Verringerung der Korrosionsbeständigkeit zu rechnen ist. Im Lichtbogenschmelzofen wurden verschiedene Legierungen mit abgestuftem Schwefelgehalten hergestellt, um den Einfluss dieses Begleitelementes auf die Korrosionsbeständigkeit systematisch zu untersuchen. Die KorroPad-Prüfung und die Bestimmung kritischer Lochkorrosionspotentiale wurden zur Charakterisierung der Legierungen genutzt. Beide Methoden belegen eine zunehmende Verringerung der Lochkorrosionsbeständigkeit mit dem Schwefelgehalt.
Die Korrosionsbeständigkeit geschweißter Konstruktionen aus nichtrostenden Duplexstählen wird von den Schweißparametern und der Nachbehandlung der Oberflächen bestimmt. Eine etablierte Methode der Schweißnahtnachbehandlung ist das Strahlen der Oberfläche mit Glasperlen. Diese Methode soll aus wirtschaftlichen Gründen durch das Strahlen mit Korund ersetzt werden, welches deutliche Zeit- und Kostenvorteile bietet. Besonders bei der Lochkorrosionsbeständigkeit hat sich das Schleifen mit Korund bereits als nachteilig erwiesen, weshalb diese Umstellung auch beim Stahlen kritisch hinterfragt wird. Daher wurden Probeschweißungen bei der Firma Modersohn hergestellt und mit verschiedenen Oberflächenbearbeitungsmethoden (Glasperlenstrahlen, Korundstrahlen, Beizen, Elektropolieren, Schleifen) nachbehandelt. Diese verschiedenen Oberflächenzustände wurden analytisch (REM, Rauheit) charakterisiert und hinsichtlich ihrer Lochkorrosionsbeständigkeit vergleichend untersucht werden, um die Eignung des Strahlens mit Korund zu beurteilen.
Martensitische nichtrostende Stähle werden in verschiedenen technischen Bereichen eingesetzt, bei denen eine optimale Kombination aus hoher mechanischer Festigkeit und guter korrosiver Beständigkeit gefordert wird. Beide Eigenschaften werden in der Industrie primär durch die Wärmebehandlung gesteuert. Die Korrosionseigenschaften sind dabei stark von der diffusionsbedingten Bildung und Auflösung von Chromkarbiden abhängig. In vergangenen wissenschaftlichen Arbeiten konnte nachgewiesen werden, dass die Abkühlgeschwindigkeit nach dem Austenitisieren einen großen Einfluss auf die Bildung solcher Karbide hat. Der Einfluss der Abkühlgeschwindigkeit auf die Lochkorrosionsbeständigkeit wurde an den Stählen 1.4108 und 1.4116 systematisch untersucht. Mit Hilfe des Stirnabschreckversuches wurde dabei die Abkühlgeschwindigkeiten variiert und anschließend die Veränderung von Gefüge, Lochkorrosionsbeständigkeit und Härte untersucht. Als Ergebnis konnten kritische Abkühlgeschwindigkeiten ermittelt werden, bei denen eine kritische Verringerung der Korrosionsbeständigkeit einsetzt.
Härte, Schneidleistung und Korrosionsbeständigkeit sind die wichtigsten Qualitätsmerkmale von Schneidwaren, die nur durch eine optimal durchgeführte Wärmebehandlung des martensitischen nichtrostenden Stahls 1.4116 (X50CrMoV15) erreicht werden können. In der industriellen Fertigung wird die Korrosionsbeständigkeit von Schneidwaren durch Wechseltauchversuche überprüft, die herstellerübergreifend eine große Schwankung der Korrosionsbeständigkeit zeigen. In den letzten Jahren wurden neue elektrochemische Untersuchungsmethoden für die Werkstoffgruppe der martensitischen nichtrostenden Stähle entwickelt, welche die geringe Lochkorrosionsbeständigkeit von Schneidwaren auf das Phänomen der Chromverarmung zurückführen. Derzeit wird in der wissenschaftlichen und in der industriellen Gemeinschaft der Schritt des Anlassens als Ursache der Chromverarmung angesehen. Bei Schneidwaren sind die Anlasstemperaturen allerdings zu gering, um die auftretende Chromverarmung zu erklären. Aus diesem Grund wurde eine systematische Untersuchung der wichtigsten Wärmebehandlungsparameter: Härtetemperatur, Haltedauer, Abkühlrate und Anlasstemperatur durchgeführt, um den Einfluss aller Wärmebehandlungsparameter auf das Auftreten von Chromverarmung aufzuklären. Durch die elektrochemisch potentiodynamische Reaktivierung (EPR) erfolgte der Nachweis von Chromverarmung. Außerdem wurde die Lochkorrosionsanfälligkeit durch die anwendernahe KorroPad-Prüfung und die Bestimmung kritischen Lochkorrosionspotentiale ermittelt. Beides zeigt den Einfluss der durch die Wärmebehandlung erzeugten Chromverarmung auf die Lochkorrosionsbeständigkeit, die beim Einsatz und bei der Reinigung von Schneidwaren notwendig sind.
Die Korrosionsbeständigkeit martensitischer nichtrostender Stähle (MNS) wird wesentlich von der chemischen Zusammensetzung und dem Wärmebehandlungszustand beeinflusst. Beides bestimmt die Verteilung der Legierungselemente im Gefüge und die daraus resultierenden Werkstoffeigenschaften. Das Legieren mit Stickstoff bewirkt im Allgemeinen eine Verbesserung der Lochkorrosionsbeständigkeit von nichtrostenden Stählen. Bei martensitischen nichtrostenden Stählen ist dieser Effekt nicht nur auf den Stickstoffgehalt selbst zurückzuführen, sondern auch auf den gleichzeitig verringerten Kohlenstoffgehalt, der ebenfalls das Ergebnis der Wärmebehandlung beeinflusst. In dieser Arbeit wird der Einfluss von Stickstoff auf die Korrosionsbeständigkeit in Bezug zum Härtungsprozess von MNS dargestellt. Dazu wird vergleichend der Effekt von Austenitisierungsdauer, -temperatur und Abkühlgeschwindigkeit auf Gefüge, Härte und Korrosionsbeständigkeit der MNS X50CrMoV15 und X30CrMoN15 1 untersucht. Die Abkühlgeschwindigkeit wurde mit dem Stirnabschreckversuch gezielt variiert, um den Einfluss von Abkühlgeschwindigkeiten von > 100 K/s bis 1 K/s zu charakterisieren. Die Veränderungen der Korrosionsbeständigkeit werden durch die elektrochemisch potentiodynamische Reaktivierung (EPR) und durch die Bestimmung kritischer Lochkorrosionspotentiale dokumentiert. Neben diesem experimentellen Ansatz werden auch die Ergebnisse von thermodynamischen Berechnungen mit der Software Thermocalc vorgestellt und abschließend auch zur Interpretation des Einflusses von Stickstoff auf die Korrosionsbeständigkeit martensitischer nichtrostender Stähle genutzt.
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.
Wasserstoff kann in Überlagerung mit Beanspruchungen zu einem unerwarteten Werkstoffversagen in höherfesten Stählen führen (wasserstoffunterstützte Schädigung von Metallen, starke Abnahme des Verformungsvermögens). Hierbei besteht in der Schweißtechnik die Gefahr einer wasserstoffunterstützten Kaltrissbildung. Der Fokus des Vortrags liegt auf das Wasserstoffbindungsverhalten (Trapping) im Grundwerkstoff und im schweißsimulierten Gefüge. Die Ergebnisse zeigen Unterschiede hinsichtlich der Bindungsenergie und des Fallencharakters. Anhand dieser lassen sich Rückschlüsse ziehen über eine effektive Wärmebehandlung zur Wasserstoffreduktion im Gefüge. Das Ziel ist eine Reduzierung des Risikos einer wasserstoffunterstützten Rissbildung.
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.
Im Frühjahr 1969 wurde bei Ausgrabungen der Universität Bonn unter Leitung von Elmar Edel auf der Qubbet el-Hawa ein außergewöhnliches Depot mit Materialien einer antiken Gusswerkstatt gefunden. Im Zuge der Fundteilung gelangten die meisten Stücke des Konvolutes in das Ägyptische Museum der Universität Bonn und werden dort aufbewahrt.
Die Deponierung des für die Forschung zur antiken Metallurgie bisher einzigartigen Konvoluts geschah im Zuge der Nachnutzung von Grabanlagen aus dem Alten Reich (um 2100 v. u. Z.) in der ägyptischen Spätzeit (um 550 – 400 v. u. Z.). Das Depot enthält Objekte, die alle Fertigungsstufen von Metallgegenständen im Wachsausschmelzverfahren dokumentieren. Es wurden Stücke von Rohwachs sowie Wachsmodelle und die zu deren Herstellung genutzten Negativformen gefunden. Weiterhin enthielt es vollständige Gussformen, die in einem aufwendigen Mehrschalenverfahren hergestellt wurden und teilweise bereits für den Guss ausgebrannt worden sind. Schließlich zählen einige Metallfiguren sowie weitere figürliche Objekte zum Konvolut, die alle in den Bereich einer kunsthandwerklichen Werkstatt deuten. Eine Besonderheit stellen zudem Gussformen dar, in denen Fragmente von Metallfiguren zur Reparatur im Überfangguss vorbereitet waren.
Das Depot wurde in der Gesamtpublikation der Bonner Grabungen bisher nur summarisch vorgestellt. 2014/15 initiierten die Abteilung Ägyptologie der Universität Bonn und das LVR-LandesMuseum Bonn unter Ludwig D. Morenz und Michael Schmauder ein gemeinsames und von der Fritz-Thyssen-Stiftung gefördertes Forschungsprojekt, das von Martin Fitzenreiter, Johannes Auenmüller und Frank Willer geleitet wurde. In Kooperation mit Dietmar Meinel (Bundesanstalt für Materialforschung und -prüfung Berlin / BAM, Fachbereich 8.5 Mikro-ZfP), Roland Schwab (Curt-Engelhorn-Zentrum Archäometrie gGmbH, Mannheim), Gerwulf Schneider (FU Berlin, Exzellenzcluster TOPOI), Ursula Baumer und Patrick Dietemann (beide Doerner-Institut / München), Thorsten Geisler-Wierwille (Steinmann Institut für Geologie, Mineralogie und Paläontologie der Universität Bonn) sowie Ursula Tegtmeier (Labor für Archäobotanik der Universität Köln) wurden die Objekte des Konvolutes eingehend und mit zeitgemäßen Verfahren untersucht. Die Ergebnisse dieses Forschungsprojekts werden in dieser Publikation vorgelegt.
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.