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Eingeladener Vortrag
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The mechanism of action of zirconium permanent modifiers on graphite surfaces was investigated in order to understand its influence on the analytical signal in atomic and molecular absorption spectrometry (AAS/MAS). For this, the molecule formation of CaF was studied, which is used for the indirect analytical determination of fluorine in high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). The kinetics of this reaction was established by monitoring its molecular spectrum at different atomisation temperatures. An Arrhenius plot showed a pseudo-first order reaction with respect to fluorine (n = 1). An intermediate state was isolated, and its structure was elucidated by spectroscopic methods: scanning electron microscopy with energy dispersive X-ray spectroscopy (SEMEDX), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XANES and EXAFS), and Raman microspectroscopy. We propose here a mechanism, where ZrO2 acts as a heterogeneous catalyst: after a pyrolytic step, an intermediate state of ZrO(OCaF) is activated, and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface. No evidence of the formation of zirconium carbide was found. Consequently, as the CaF formation is catalysed by a heterogeneous catalyst, surface modifications with ZrO2 nanoparticles and ZrO xerogels were investigated in order to increase the surface area. Their influence was evaluated in the molecule formation of CaF, CaCl, CaBr, and CaI. Graphite furnace modification with zirconium oxide nanoparticles proves to be the best choice for fluorine analysis with a signal enhancement of more than eleven times with respect a non-coated graphite furnace. However, the influence of zirconium modifications in the analytical signals of Cl, and I is lower than the F signals or even negative in case of the Br. Understanding zirconium modifiers as heterogeneous catalysts offers a new perspective to AAS and MAS, and reveals the potential of surface analytical methods for development of improved permanent modifiers and graphite furnace coatings.
Ni-base superalloy single crystals have been used in turbine blades for hot sections of gas turbines for over four decades. In order to increase the efficiency of the turbines, a continuous increase in the inlet temperature of combustion gases into the turbine has driven the design of turbine blades to complicated shapes and the presence of a complex pattern of cooling channels. These three-dimensional shapes, together with the inhomogeneous distribution of stresses along the blade, induce an also complicated triaxial stress state, which does not compare to uniaxial tests that are performed to characterize high temperature properties such as creep. A round notch on a test piece represents a simple configuration that generates a quasi-isostatic stress state across the notch. In the present contribution, the effect of a sharp round notch on the microstructural micromechanisms within the notched region cylindrical bars, loaded along [001] at 1020 °C and 160 MPa net stress, is studied. To this end, a series of interrupted creep tests is conducted on plain and notched bars and the microstructure is compared. Results are discussed in terms of degree microstructural coarsening, and dislocation activity. The effect of notch generation via grinding is also discussed in these terms. The presence of carbides evolving in from residual carbon is also shown and discussed. .Funding by the German Research Association (DFG) [grant number AG 191/1] is acknowledge
We analyzed the results of high-energy X-ray CT scans for three 20×16×16 in. block samples of Indiana limestone from our recent radial acidizing experiments with HCl. CT scans were done for complete samples, and 3D images of internal dissolution patterns were built. Each 3D image consists of submillimeter-size voxels to capture fine details of individual wormholes.
The obtained 3D images of acidized blocks allow us to observe from various angles the details of the wormholes obtained in the three experiments, which demonstrated wide pore-volume-to-breakthrough (PVBT) range with three different injection rates. Also, variation of the CT number reveals the presence of depositional layers in all block samples, and the obtained CT images were used to interpret the effect that rock layers might have on wormhole penetration at different injection rates.
Further, the built voxel models were used to calculate the radial distributions of dissolved rock volume, which otherwise are not obvious for such complex branched structures as wormholes. We observed how varied experimental conditions affected those distributions. The radial distributions were found very similar across the samples, which suggested the way to detect the effective wormhole penetration depth.
The exploration of metal phosphonates chemistry has gained great interest during the last decades, because of their structural diversity. Transition metal phosphonates are promising candidates for an application as electrocatalysts in oxygen evolution reactions (OER).
Here, we present the in situ investigation of mechanochemical syntheses of different manganese phosphonates by synchrotron X-ray diffraction. Nitrilotri(methylenephosphonic acid) and N,N-Bis(phosphonomethyl)glycine were chosen as ligands. The liquid-assisted milling process can be divided into three steps, including an amorphous stage. One of the products has not been obtained by classical solution chemistry before.
These metal phosphonates and/or their derivatives are considered to be active in electrochemical energy conversion. The verification of their applicability is one of the topics of our resent research.
Mechanochemistry is a versatile approach for green and fast synthesis of pure substances. By milling the reactants, various organic, inorganic, and metal-organic compounds can be obtained in high yields. Although mechanochemistry is widely used, the underlying mechanisms are not fully understood making mechanochemical reactions difficult to predict. Metal phosphonates are metal-organic compounds accessible by grinding. Because of their structural diversity, the exploration of the chemistry of metal phosphonates has gained considerable interest during the last decades. Transition metal phosphonates are promising candidates for an application as electrocatalysts in oxygen evolution reaction (OER). Here, we present the in situ investigation of the mechanochemical synthesis of a manganese(II)-phosphonate by synchrotron X-ray diffraction and thermography. The product has not been obtained by classical solution chemistry before and its crystal structure was determined from PXRD data. The milling process can be divided into different steps, with the product crystallization corresponding with the highest temperature rise. The activity of this metal phosphonate towards OER was measured and is presented here.
Mechanochemistry is a versatile approach for green and fast synthesis of pure substances. The exploration of the chemistry of metal phosphonates has gained considerable interest during the last decades due to their structural diversity. We synthesized manganese phosphonates in milling reactions. The mechanochemical reactions were investigated in situ to reveal the underlying mechanisms.
Two divalent manganese aminophosphonates, manganese mono (nitrilotrimethylphosphonate) (MnNP3) and manganese bis N-(carboxymethyl)iminodi(methylphosphonate)) (Mn(NP2AH)2), have been prepared by mechanochemical synthesis and characterized by powder X-ray diffraction (PXRD). The structure of the novel compound Mn(NP2AH)2 was determined from PXRD data. MnNP3 as well as Mn(NP2AH)2 exhibits a chain-like structure.
In both cases, the manganese atom is coordinated by six oxygen atoms in a distorted octahedron. The local coordination around Mn was further characterized by extended X-ray absorption fine structure. The synthesis process was followed in situ by synchrotron X-ray diffraction revealing a three-step reaction mechanism. The asprepared manganese(II) phosphonates were calcined on air.
All samples were successfully tested for their suitability as catalyst material in the oxygen evolution reaction.
A series of Ca-based coordination polymers were prepared mechanochemically by milling Ca(OH)2 with phthalic acid (H2oBDC), isophthalic acid (H2mBDC), and terephthalic acid (H2pBDC). The hydrated compounds [Ca(oBDC)(H2O)], [Ca(mBDC)(H2O)3.4], and [Ca(pBDC)(H2O)3] were prepared for the first time via mechanochemical routes. The refined structures were validated by extended X-ray absorption data. The new dehydrated compound [Ca(oBDC)] (1-H2O), obtained after the thermal post-treatment of 1 in a reversible phase transition process, was determined ab initio based on the powder X-ray diffraction (PXRD) data. The materials were thoroughly characterized using elemental analysis, thermal analysis, and spectroscopic methods: magic-angle spinning NMR and attenuated total reflection-infrared spectroscopy. The specific surface areas and sorption properties of the hydrated and dehydrated samples were determined using the isotherms of gas sorption and dynamic vapor sorption measurements.
Additive manufacturing (AM) offers a range of novel applications. However, the manufacturing process is complex and the production of defect-free parts with a high reliability is still a challenge. Thermography is a valuable tool for process surveillance, especially in metal AM processes. The high process temperatures allow one to use cameras usually operating in the visible spectral range. Here, we compare the results of first measurements during the manufacturing process of a commercial laser metal deposition (LMD) setup using a MWIR camera with those from a VIS high-speed camera with band pass filter in the NIR range.
Additive manufacturing (AM) opens the route to a range of novel applications.However, the complexity of the manufacturing process poses a challenge for the production of defect-free parts with a high reliability. Since process dynamics and resulting microstructures of AM parts are strongly influenced by the involved temperature fields, thermography is a valuable tool for process surveillance. The high process temperatures in metal AM processes allow one to use cameras usually operating in the visible spectral range to detect the thermally emitted radiation from the process. In our work, we compare the results of first measurements during the manufacturing processes of a commercial laser metal deposition (LMD) setup and a laser beam melting (LBM) setup using a MWIR camera with those from a VIS high-speed camera with band pass filter in the NIR range.
Aktuell werden Prozessmonitoringsysteme in der additiven Fertigung (AM) zur Überwachung der Energiequelle, des Bauraums, des Schmelzbades und der Bauteilgeometrie zumindest im metallbasierten AM schon kommerziell angeboten. Weitere Verfahren aus den Bereichen der Optik, Spektroskopie und zerstörungsfreien Prüfung werden in der Literatur als geeignet für die in-situ Anwendung bezeichnet, es finden sich aber nur wenige Berichte über konkrete Umsetzungen in die Praxis.
Die Bundesanstalt für Materialforschung und -prüfung hat ein neues Projekt gestartet, dessen Ziel die Entwicklung von Verfahren des Prozessmonitorings zur in-situ Bewertung der Qualität additiv gefertigter Bauteile in AM-Prozessen mit Laser- bzw. Lichtbogenquellen ist. Verschiedene Verfahren der zerstörungsfreien Prüfung, wie Thermografie, optische Tomografie, optische Emissionsspektroskopie, Wirbelstromprüfung und Laminografie werden in verschiedenen AM-Prozessen zum Einsatz gebracht und die Ergebnisse fusioniert. Die evaluierten Ergebnisse werden mit Referenzverfahren wie Computertomografie und Ultraschall-Tauchtechnik verglichen. Ziel ist eine deutliche Reduzierung aufwändiger und zeitintensiver, zerstörender oder zerstörungsfreier Prüfungen nach der Fertigung des Bauteiles und zugleich eine Verringerung von Ausschussproduktion.
Hier wird das Projekt als Ganzes vorgestellt und der Fokus auf verschiedene Methoden der Temperaturmessung mit Hilfe der Thermografie gelegt. Anforderungen an die Messtechnik für verschiedene AM-Systeme werden diskutiert und erste experimentelle Ergebnisse werden präsentiert.
Additive manufacturing (AM) offers a range of novel applications. However, the manufacturing process is complex and the production of defect-free parts with high reliability and durability is still a challenge. Thermography is a valuable tool for process surveillance, especially in metal AM processes. The high process temperatures allow one to use cameras usually operating in the visible spectral range. Here, we compare the results of measurements during the manufacturing process of a commercial laser metal deposition setup using a mid-wavelength-IR camera with those from a visual spectrum high-speed camera with band pass filter in the near-IR range.
Microbiologically influenced corrosion (MIC) is the deterioration of metals due to the metabolic activities of microorganisms. Microorganisms can take electrons directly from the metal surface (EMIC) thereby causing corrosion. Well known culprits of EMIC are: sulfate-reducing bacteria (SRB), acetogens and methanogens.
Our aims
- Develop a novel flow system to study MIC by methanogens to mimic industrial Environments
- Investigate the inhibitory concentrations of biocides targeting SRB on corrosive methanogenic strains
- Investigate the inhibitory effects of corrosion inhibitors on methanogens
- Compare the inhibitory concentrations to SRB
Microbiologically influenced corrosion (MIC) is an expensive but unpredictable problem for the industries. The most well-known culprit for MIC is the sulfate-reducing microorganisms (SRM), such as members from the genus Desulfovibrio. It has been widely accepted that SRM can contribute significantly to MIC through the production of hydrogen sulfide (HS-) or in some cases a direct electron uptake from the metal surface. However, in a real environmental system, SRM is not exclusive and often involved with other microorganisms that may also contribute to MIC, such as methanogens.
Methanogenic archaea can produce methane (CH4) using H2+CO2, formate, methylated amines or acetate. Methanogens are highly abundant in the environment and many are found in very extreme conditions, such as high temperature and high salinity. Previous researches have demonstrated that methanogens are capable of MIC, though the specific mechanisms are still under investigation. In the oil and gas industry, methanogens are not considered as the main contributor for MIC since the corrosion rates are often too low. However, the tests for methanogen-induced MIC are usually performed at static conditions, which cannot represent the system accurately. Here, we developed a novel anaerobic system to evaluate the corrosion potential of methanogens under flow conditions. We will use the Methanococcus maripaludis KA1 strain, which was isolated from a crude oil tank, as the organism of interest. A separate system for Desulfovibrio alaskensis will be established for corrosion rate comparisons. Furthermore, we will study the synergistic effects of M. maripaludis and D. alaskensis on MIC under flow.
Electrochemical study of polyaniline/silicon dioxide containing coatings in geothermal solution
(2018)
Polyaniline/Silicon Dioxide containing coatings were electrochemically investigated in a saline geothermal solution.
With the increase of exposure time, impedance values of coated specimens decreased at low frequency, which could be caused by the decrease of pore resistance due to electrolyte or water uptake.
Coating system needs further optimization work.
Geothermal brine is a complex system containing a wide variety of dissolved salts resulting from the condition s in a geothermal well. These fluids lead to corrosion in pipes and other parts of geothermal system construction and necessitate intense research efforts in finding new suitable materials. Carbon steel is susceptible to corrosion in geothermal brine especially when it is exposed to a high temperature and high-pressure medium, which is considered to be an aggressive environment. An artificial geothermal water, bas ed on a brine composition found in Indonesia, was used to investigate the performance of high alloyed materials. The electrolyte has pH 4 and contains 1,500 mg/l Cl-, 20 mg/l SO4 2-, 15 mg/l HCO3 -, 200 mg/l Ca 2+, 250 mg/l K+, and 600 mg/l Na+. In order to protect the bare material in geothermal application, it is necessary to either use high alloyed material s or coatings. In this research, a coating system consisting of polyaniline and silicon dioxide was investigated regarding its behavior to protect carbon steel. In detail, the effect of SiO2 and polyaniline (PANi) addition was evaluated by exposure and electrochemical tests for 7 days, i.e. electrochemical impedance spectroscopy (EIS) and open circuit potential (OCP) at room temperature and 150 °C with 1 MPa pressure.
Electrochemical deposition of polyaniline on carbon steel for corrosion study in geothermal solution
(2018)
Polyaniline has been widely developed for many applications, e.g., sensor, supercapacitor component, electrochromic devices, and anticorrosion pigments [1]. Although the addition of polyaniline pigment in organic coatings has been an alternative for corrosion protection in industrial application, the protection mechanism is still not fully understood [2]. Herein in this study, as a part of the development of polyaniline/silicon dioxide coating for geothermal application, polyaniline has been deposited electrochemically on carbon steel surface and tested in geothermal solution to study the contribution of polyaniline in the corrosion protection of a polyaniline-based composite in the geothermal system. The electrochemical deposition was carried out by immersing carbon steel in 0.1 M oxalic acid and 0.05 M aniline, with the polarization potential of -0.6 – 1.5 V vs. Ag/AgCl, and a scan rate of 10 mV/s. To observe the surface/interface reaction between the electrolyte and electrode surface during the electrochemical polymerization, electrochemical impedance spectroscopy (EIS) measurement was applied after each cycle. For corrosion study in the geothermal application, this experiment used an artificial geothermal solution with the composition of 1,500 mg/l Cl-, 20 mg/l SO42-, 15 mg/l HCO3-, 200 mg/l Ca2+, 250 mg/l K+, and 600 mg/l Na+, and pH 4 to simulate a geothermal brine found in Sibayak, Indonesia. Electrochemical measurements were performed by monitoring the open circuit potential over seven days, with the interruption of EIS every 22 hours. The experiments were performed at room temperature and 150 °C (1 MPa) in a free oxygen environment. Polyaniline coated carbon steel is more durable in a room temperature environment compared to 150 °C, which could be caused by the iron oxalate dissolution at elevated temperature. This degradation was further proven by the impedance spectra, which showed a reduction of approximately ten times for specimens measured at 150 °C as compared to the specimens measured at room temperature.
Geothermal brine is a complex system containing a wide variety of dissolved salts resulting from the condition s in a geothermal well. These fluids lead to corrosion in pipes and other parts of geothermal system construction and necessitate intense research efforts in finding new suitable materials. Carbon steel is susceptible to corrosion in geothermal brine especially when it is exposed to a high temperature and high-pressure medium, which is considered to be an aggressive environment. An artificial geothermal water, bas ed on a brine composition found in Indonesia, was used to investigate the performance of high alloyed materials. The electrolyte has pH 4 and contains 1,500 mg/l Cl-, 20 mg/l SO4 2-, 15 mg/l HCO3 -, 200 mg/l Ca 2+, 250 mg/l K+, and 600 mg/l Na+. In order to protect the bare material in geothermal application, it is necessary to either use high alloyed material s or coatings. In this research, a coating system consisting of polyaniline and silicon dioxide was investigated regarding its behavior to protect carbon steel. In detail, the effect of SiO2 and polyaniline (PANi) addition was evaluated by exposure and electrochemical tests for 7 days, i.e. electrochemical impedance spectroscopy (EIS) and open circuit potential (OCP ) at room temperature and 150 °C with 1 MPa pressure .
A transient simulation including the impact of the laser energy, the melting of the metal and the development of the weld pool was conducted to observe the evolution of the vapor capillary and the solidification of the melt in pulsed laser beam welding of AISI 304 steel. The phase field method was implemented to investigate the evolution and behavior of the liquid-gas interface during welding and to describe the condensed and vapor phases. The effects of phase transition, recoil pressure, thermo-capillary and natural convection, vaporization and temperature dependent material properties were taken into account. A Gaussian-like heat source under consideration of the Fresnel absorption model was used to model the energy input of the laser beam. The heat source model was extended by a newly developed empirical approach of describing multiple beam reflections in the keyhole. To validate this new model, the numerical results were compared to experimental data and good agreement regarding the size and shape of the weld pool was observed.
A simplified model for numerical simulation of laser metal deposition process with beam oscillation
(2018)
A simplified model for the numerical simulation of the laser metal deposition process with beam oscillation is proposed. The model studies circular and lateral oscillations in order to reduce the porosity of the deposited part, to increase the process efficiency and the gap bridging ability as well. The deposition rate is increased by modifying the shape and the width of the molten pool through an optimized laser beam power distribution and oscillation amplitude. The relationship between the process conditions and the shape of the fabricated part are determined. It is found that an increase of the amplitude by a lateral oscillation of the beam reduces the heat flux and hence the shape of the deposited wall. A good correlation between the numerically calculated results and the experimental measurements is obtained.
This work aims to find the thermal cycles during and after fusion welding through simulation by first calculating the resulting local temperature field in the quasi-stationary part of the process. Here complete-penetration keyhole laser beam welding with a laser power of 18 kW on a 15 mm thick slab of a low-alloyed steel at a welding speed of 2 m/min is considered. In order to physically depict the laser material interaction a multi-physics numerical model including the effects of phase transformation, thermo-capillary convection, natural convection and temperature-dependent material properties up to evaporation temperature is developed.
It uses a fixed keyhole geometry with a right truncated circular cone shape to introduce the laser beam energy to the workpiece. In a subsequent study, the resulting local temperature field is then used as an equivalent heat source in order to predict the unsteady thermal cycle during and after fusion welding. The translational movement of the laser beam through the workpiece is represented by a moving mesh approach. For the simulation, stationary heat transfer and fluid dynamics are described by a system of strongly coupled partial
differential equations. These are solved with the commercial finite element software COMSOL Multiphysics 5.0. The results of the numerical simulation are validated by experiments, where the weld bead shapes and the thermal cycles show good correlation.
The shape of the weld pool in laser beam welding plays a major role to understand the dynamics of the melt and its solidification behavior. The aim of the present work was its experimental and numerical investigation. To visualize the geometry of the melt pool in the longitudinal section a butt joint configuration of 15 mm thick structural steel and transparent quartz glass was used. The weld pool shape was recorded by means of a high-speed video camera and two thermal imaging MWIR and VIS cameras. The observations show that the dimensions of the weld pool vary depending on the depth. The regions close to the surface form a teardrop shaped weld pool. A bulge-region and its temporal evolution were observed approximately in the middle of the depth of the weld pool. Additionally, a transient numerical simulation was performed until reaching a steady state to obtain the weld pool shape and to understand the formation mechanism of the observed bulging phenomena. A fixed keyhole with an experimentally obtained shape was used to represent the full-penetration laser beam welding process. The model considers the local temperature field, the effects of phase transition, thermo-capillary convection, natural convection and temperature-dependent material properties up to evaporation temperature. It was found that the Marangoni convection and the movement of the laser heat source are the dominant factors for the formation of the bulging-region. Good correlation between the numerically calculated and the experimentally observed weld bead shapes and the time-temperature curves on the upper and bottom surface were found.
A three-dimensional multi-physics numerical model was developed for the calculation of an appropriate equivalent volumetric heat source and the prediction of the transient thermal cycle during and after fusion welding. Thus the modelling process was separated into two studies. First, the stationary process simulation of full-penetration keyhole laser beam welding of a 15 mm low-alloyed steel thick plate in flat position at a welding speed of 2 m/min and a laser power of 18 kW was performed. A fixed keyhole with a right circular cone shape was used to consider the energy absorbed by the workpiece and to calibrate the model. In the calculation of the weld pool geometry and the local temperature field, the effects of phase transition, thermo-capillary convection, natural convection and temperature-dependent material properties up to evaporation temperature were taken into account. The obtained local temperature field was then used in a subsequent study as an equivalent heat source for the computation of the transient thermal field during the laser welding process and the cooling stage of the part. The system of partial differential equations, describing the stationary heat transfer and the fluid dynamics, were strongly coupled and solved with the commercial finite element software COMSOL Multiphysics 5.0. The energy input in the transient heat transfer simulation was realised by prescription of the nodes temperature. The prescribed nodes reproduced the calculated local temperature field defining the equivalent volumetric heat source. Their translational motion through the part was modelled by a moving mesh approach. An additional remeshing condition and helper lines were used to avoid highly distorted elements. The positions of the elements of the polygonal mesh were calculated with the Laplace’s smoothing approach. Good correlation between the numerically calculated and the experimentally observed weld bead shapes and transient temperature distributions was found.
The geometry of the melt pool in laser beam welding plays a major role to understand the dynamics of the melt and its solidification behavior. In this study, a butt configuration of 15 mm thick structural steel and transparent quartz glass was used to observe the weld pool geometry by means of high-speed camera and an infrared camera recording. The observations show that the dimensions of the weld pool vary depending on the depth. The areas close to the weld pool surface take a teardrop-shape. A bulge-region and its temporal evolution were observed approximately in the middle of the depth of the weld pool. Additionally, a 3D transient thermal-fluid numerical simulation was performed to obtain the weld pool shape and to understand the formation mechanism of the observed bulging effect. The model takes into account the local temperature field, the effects of phase transition, thermo-capillary convection, natural convection and temperature-dependent material properties up to evaporation temperature. The numerical results showed good accordance and were furthermore used to improve the understanding of the experimentally observed bulging effect.
Combining experiments and all-atom molecular dynamics simulations, we study the conformational behavior of polyacrylamide (PAM) in aqueous alcohol mixtures over a wide range of temperatures. This study Shows that even when the microscopic interaction is dictated by hydrogen bonding, unlike its counterparts that present a lower critical solution temperature (LCST), PAM shows a counterintuitive tunable upper critical solution temperature (UCST)-type phase transition in water/alcohol mixtures that was not reported before. The Phase transition temperature was found to be tunable between 4 and 60 1C by the type and concentration of alcohol in the mixture as well as by the solution concentration and molecular weight of the polymer. In addition, molecular dynamics simulations confirmed a UCST-like behaviour of the PAM in aqueous alcoholic solutions.
Additionally, it was observed that the PAM is more swollen in pure alcohol solutions than in 80% alcoholic solutions due to y-like behaviour. Additionally, in the globular state, the size of the aggregates was found to increase with increasing solvent hydrophobicity and polymer concentration of the solutions. Above ist Phase transition temperature, PAM might be present as individual polymer chains in the coil state (r10 nm). As PAM is a widespread polymer in many biomedical applications (gel electrophoresis, etc.), this finding could be of high relevance for many more practical applications in high performance pharmaceuticals and/or sensors.
Die Ausführung von Abdichtungssystemen insbesondere an Ingenieurbauwerken der Verkehrsinfrastruktur greift in die unmittelbare Verfügbarkeit/Nutzbarkeit des Bauwerks ein und erfolgt deshalb i.a.R. unter höchstem Zeitdruck. Neuere materialtechnische Entwicklungen im Bereich der Flüssigkunststoff-Systeme erlauben kürzere Ausführungszeiten in einem erweiterten Einsatzspektrum. Zur Sicherstellung anforderungsgerechter Gebrauchseigenschaften des gesamten Brückenabdichtungssystems gibt die vorliegende Veröffentlichung Hinweise für die einzuhaltenden Baugrundsätze, bautechnologische Besonderheiten und Erfordernisse im Umgang mit Polymethylmethacrylat (PMMA) sowie qualitätssichernde Maßnahmen.
Der Vortrag stellt ein neuartiges Korrosionsprüfverfahren für Zinküberzüge auf Basis gelartiger Elektrolyte vor und führt die Vorteile gegenüber konventionellen Prüfverfahren auf. Basierend auf den Ergebnissen wird die Idee für einen IGF-Projektantrag in Kooperation mit dem Fraunhofer IKTS vorgestellt.
A new approach to the assessment of the corrosion behaviour of zinc coatings under atmospheric conditions can be achieved using gel-type electrolytes as an alternative to standard aqueous test electrolytes. Gel-type electrolytes allow minimally invasive corrosion investigations on zinc coatings. They also provide the possibility to carry out corrosion investigations onsite. By using gel-type electrolytes corrosion-relevant characteristic values such as corrosion currents and polarization resistanc-es can be determined. These allow to describe the formation and the stability of the formed corrosion product layers under various climatic conditions. With this knowledge, a prediction of the zinc coating life cycle is possible. In this contribution, the value of gel-type electrolytes for corrosion research on zinc coatings is presented.
A new approach to the assessment of the corrosion behaviour of zinc coatings under atmospheric conditions can be achieved using gel-type electrolytes as an alternative to standard aqueous test electrolytes. Gel-type electrolytes allow minimally invasive corrosion investigations on zinc coatings. They also provide the possibility to carry out corrosion investigations onsite. By using gel-type electrolytes corrosion-relevant characteristic values such as corrosion currents and polarization resistances can be determined. These allow to describe the formation and the stability of the formed corrosion product layers under various climatic conditions. With this knowledge, a prediction of the zinc coating life cycle is possible. In this contribution, the value of gel-type electrolytes for corrosion research on zinc coatings is presented.
Electrochemical tests, hardness measurements, and microstructure analysis are performed to study the influence of austenitizing, quenching, and tempering parameters on the corrosion resistance of the martensitic stainless steel grade X50CrMoV15 (1.4116). Different heat treatment states were studied using an adapted EPR-Test to evaluate the chromium distribution and depletion caused by the formation and dissolution of chromium rich carbides. The EPR results were correlated with pitting corrosion behavior, demonstrating the strong effect of heat treatment parameters on the susceptibility of martensitic stainless steels to corrosion phenomena.
Acoustic emission testing
(2018)
Acoustic Emission
(2018)
Das Phänomen Schallemission (eng. Acoustic Emission, AE) ist eine Begleiterscheinung bei aktiven Mechanismen und Prozessen wie sie in Werkstoffen auftreten, die einer Belastung durch Krafteinwirkung oder durch Änderung der Umgebungsbedingungen ausgesetzt sind. Plastische Verformung, Risswachstum, Korrosion oder der Übergang zu einer anderen Phase generieren u.a. transiente elastische Wellen, die sich im Werkstoff und an der Materialoberfläche ausbreiten. Auftretende Auslenkungen von wenigen hundert Pikometern sind mit piezo-elektrischen AE Sensoren detektierbar. Aufzeichnungsraten von bis zu 40 MHz ermöglichen dabei zeitliche Auflösungen von einigen Nano- bis Mikrosekunden. Die Dechiffrierung der detektierten Informationen ist für die Material- und Versagenscharakterisierung sowie für Anwendungen in der Struktur- oder Prozessüberwachung ein zentraler Forschungsschwerpunkt.
Nach einem kurzen Überblick zu den Grundlagen werden ausgewählte Ansätze der AE Methode vorgestellt und diskutiert:
1) AE Monitoring von Pipelines als Referenzmessung für die Entwicklung eines akustischen faseroptischen Monitorings (AGIFAMOR)
2) Schwellwertfreie AE Messung im 4-Punkt-Rohrbiegeprüfstand BAM_9.1 (AGIFAMOR)
3) Kombination von AE mit Röntgen-Mikrotomografie und die Anwendung der frequenzbasierten Mustererkennung ermöglichen eine Zuordnung von AE und Mechanismen (Ergebnisse aus dem SNSF Projekt Nr. 127'134, Baensch 2014, Diss. ETH No. 22372)
The geometry of the melt pool in laser beam welding plays a major role to understand the dynamics of the melt and its solidification behavior. In this study, a butt configuration of 15 mm thick structural steel and transparent quartz glass was used to observe the weld pool geometry by means of high-speed camera and an infrared camera recording. The observations show that the dimensions of the weld pool vary depending on the depth. The areas close to the weld pool surface take a teardrop-shape. A bulge-region and its temporal evolution were observed approximately in the middle of the depth of the weld pool. Additionally, a 3D transient thermal-fluid numerical simulation was performed to obtain the weld pool shape and to understand the formation mechanism of the observed bulging effect. The model takes into account the local temperature field, the effects of phase transition, thermo-capillary convection, natural convection and temperature-dependent material properties up to evaporation temperature. The numerical results showed good accordance and were furthermore used to improve the understanding of the experimentally observed bulging effect.
In this study, a three-dimensional CFD-simulation model was developed to simulate the fluid flow in the weld pool. The CFD-model showed a bulging region in the middle of the depth, which is separated from the top surface and bottom surface by two narrowing regions. It can be concluded that the interaction of the movement of the laser source with the Marangoni vortex leads to a teardrop shape at the upper and bottom surface of the workpiece. Additionally, it shows that the bulging in the weld is a result of the backflows on the upper and lower sides due to the thermo-capillary-driven flows. The weld pool shape was used as a heat source in a two-dimensional thermomechanical model, which allows a highly accurate transformation of the weld pool dimensions obtained from the CFD model. This developed technique allows the consideration of physical aspects, which cannot be considered when using traditional heat sources. The mechanical model has shown that the chronological order of the solidification of the weld has a significant influence on the nature and distribution of the stresses in the weld. High tensile stress has been observed in the bulging region, i.e. in the susceptible region for solidification cracking, when compared to the other narrowing regions, which show compressive stress.
In this study, a three-dimensional CFD-simulation model was developed to simulate the fluid flow in the weld pool. The CFD-model showed a bulging region in the middle of the depth, which is separated from the top surface and bottom surface by two narrowing regions. It can be concluded that the interaction of the movement of the laser source with the Marangoni vortex leads to a teardrop shape at the upper and bottom surface of the workpiece. Additionally, it shows that the bulging in the weld is a result of the backflows on the upper and lower sides due to the thermo-capillary-driven flows. The weld pool shape was used as a heat source in a two-dimensional thermomechanical model, which allows a highly accurate transformation of the weld pool dimensions obtained from the CFD model. This developed technique allows the consideration of physical aspects, which cannot be considered when using traditional heat sources. The mechanical model has shown that the chronological order of the solidification of the weld has a significant influence on the nature and distribution of the stresses in the weld. High tensile stress has been observed in the bulging region, i.e. in the susceptible region for solidification cracking, when compared to the other narrowing regions, which show compressive stress.
One of the main factors affecting the use of lasers in the industry for welding thick structures is the process accompanying solidification cracks. These cracks mostly occurring along the welding direction in the welding center, and strongly affect the safety of the welded components. In the present study, to obtain a better understanding of the relation between the weld pool geometry, the stress distribution and the solidification cracking, a three-dimensional computational fluid dynamic (CFD) model was combined with a thermo-mechanical model. The CFD model was employed to analyze the flow of the molten metal in the weld pool during the laser beam welding process. The weld pool geometry estimated from the CFD model was used as a heat source in the thermal model to calculate the temperature field and the stress development and distributions. The CFD results showed a bulging region in the middle depth of the weld and two narrowing areas separating the bulging region from the top and bottom surface. The thermo-mechanical simulations showed a concentration of tension stresses, transversally and vertically, directly after the solidification during cooling in the region of the solidification cracking.
In recent years, laser beam welding has found wide applications in many industrial fields. Solidification cracks are one of the most frequently encountered welding defects that hinder obtaining a safe weld joint. Decades of research have shown that one of the main causes of such cracks are the strain and the strain rate. Obtaining meaningful measurements of these strains has always been a major challenge for scientists, because of the specific environment of the measurement range and the many obstacles, as well as the high temperature and the plasma plume. In this study, a special experimental setup with a high-speed camera was employed to measure the strain during the welding process. The hot cracking susceptibility was investigated for 1.4301 stainless steel, and the critical strain required for solidification crack formation was locally and globally determined.
This paper represents the results for proposed optical flow method based on the Lucas-Kanade (LK) algorithm applied to two different problems. The following observations can be made:
- The estimated strain and displacement for conducted tensile test are generally very close to those measured with conventional DIC-technique.
- The LK technique allows measurement of strain or displacement without special selection of a region of interest.
Using a novel optical measurement technique together with the optical flow algorithm, a twodimensional deformation analysis during welding was conducted. This technique is the first to provide a measurement of the full strain field locally in the immediate vicinity of the solidification front. Additionally, the described procedure of the optical measurement allows the real material-dependent values of critical strain characterizing the transition to hot cracking during laser welding processes to be determined.
Hard and wear resistant coatings deposited by PVD techniques have been characterized for decades for their capabilities to protect steel substrates from corrosion. In the present work the effect of Mg incorporated into TiN coatings is described in terms of the corrosion behavior as well as the mechanical and structural properties.
TiN and TiMgN films with Mg contents between 10 and 35 at.% were deposited onto mirror polished 100Cr6 (1.3505) steel samples with 2.5 and 5 μm thickness by using DC magnetron sputtering. The corrosion protection capabilities of the coatings were characterized by neutral salt spray (NSS) test, considering the amounts and sizes of growth defects inherent in each coated sample as determined by a recently developed optical scan method (Large Area High Resolution mapping). The defect data were statistically analyzed for improved interpretation of NSS test results. Chosen growth defects were additionally analyzed by focused ion beam technique. Furthermore the coating composition and morphology, the hardness and the tribological behavior were characterized.
Polished steel samples coated with 2.5 μm TiMgN containing about 35 at.% Mg were in the plane free of corrosion after 24 h in a NSS test. TiMgN with 10 or 20 at.% Mg only provided a slightly improved corrosion protection in relation to pure TiN coatings, which was limited to certain types of growth defects. The highest Mg containing coatings exhibited a decreased hardness down to 1200 or 1800 HV depending on type of deposition (HV 1200: Ti- and Mg-target with rotating substrate holder, 1800: Mg-plugged Ti-target with static substrate holder), but also showed a strongly improved wear resistance against Al2O3 related to pure TiN. By analyzing the NSS test results it was found that the corrosion behavior of the coated samples did not only depend strongly on the Mg content, but also on the sample individual defect concentrations. Therefore this subject is extensively discussed.
One of the biggest problems in high-voltage silicone rubber insulation cable accessories is the damage on electrical treeing, initiated by partial discharges. The electrical treeing starts at unavoidable imperfections inside the material or at interfaces. The damage is usually irreversible and leads around the starting points to a partial destruction of the material. To prolong the lifetime and thereby to increase the assurance of the structural component commonly, for mechanical improvement constituted filler is modified to obtain a self-healing silicone rubber. Damage mechanism is analysed to address the filler to the damage mode.
Der Vortrag widmet sich der „ELLIPSOMETRISCHE KLASSIFIZIERUNG VON KOHLENSTOFFSCHICHTEN“ und beschreibt die Punkte: 1. Anwendungen Kohlenstoffschichten–Carbon–based films (DLC) aus dem Vortrag N. Ohtakeet. al. (ISO TC 107, Tokyo 2017),2. Präparation der Kohlenstoffschichten für ISO TC 107 Ringversuch aus Vortrag M. Hiratsuka et. al. (ISO TC 107, Tokyo 2017), 3. Ellipsometrische Charakterisierung von Kohlenstoffschichten, Ergebnisse des Ringversuchs (ISO TC 107, Tokyo 2017) Vortrag Beck et. al. und 4.Deutsche Normungsaktivitäten national/international zur Ellipsometrie DIN NA 062-01-061 (DIN 50989-1)/TC 107 (PWI DE)“ im Einzelnen.
The paper addresses “WHITE LIGHT INTERFERENCE MICROSCOPY, ELLIPSOMETRY, AND INSTRUMENTED INDENTATION TESTING AS REFERENCE PROCEDURES“ and is subdivided in the following sections: 1. Measurement vs. testing vs. reference procedures, 2. White light interference microscopy (WLIM) for determination of step height h, 3. Spectroscopic ellipsometry (SE) for determination of layer thickness d and 4. Instrumented indentation testing (IIT) for determination of indentation hardness HIT. The following points are discussed in more detail: methodology of measurement and testing, uncertainty budgets for direct (WLIM), model-based (SE) and formula-based (IIT) reference procedures by means of specific examples. It is shown that standardization efforts are connected to reference procedures.
Der Vortrag gibt den aktuellen Stand der Normung im Bereich der Oberflächen-technik insbesondere der Oberflächenanalytik und der Oberflächenmess- und -prüftechnik wider.
Vorgestellt wird der Status technischer Berichte, Normenentwürfe und Normen u.a. zur Charakterisierung von funktionellen Glasoberflächen für bioanalytische Anwendungen, zur Messung der Schichtdicke von Nanomaterialien mittels Ellipsometrie, zur Kalibrierung von Interferometern und Interferenzmikroskopen für die Formmessung, zur Rockwelleindringprüfung zur Bewertung der Schicht-haftung, zu den Grundlagen der Ellipsometrie, zur Messung der Schichtdicke mittels Wirbelstromverfahren, zur Schichtpotentialmessung von Mehrfach-Nickelschichten, zu Filtern und Augenschutzgeräten gegen Laserstrahlung sowie zur Bestimmung der Schichthaftung mittels Zugversuch.