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To better understand the mechanism of hydrogen assisted cracking (HAC), it is important to investigate the 3D structure of the cracks non-destructively. Since, cracks introduced by HAC are usually very small, conventional x-ray imaging methods often lack the required spatial resolution.
However, the detection of those cracks can be enhanced by taking advantage of refraction at interfaces within the sample.
To image this refractive deflection we employ analyser based imaging (ABI). In this work we aim at proving the enhanced crack detection of ABI by investigating an alluminum alloy weld.
Ferritic steels with Cr-contents up to 13 wt. % are used as heat exchanger or boiler tube materials in combustion based power plants. These materials are subject to aggressive corrosion caused by the reaction of the steel with highly corrosive gases under high temperatures up to 650°C. The early stages of corrosion and sulfidation especially and the influence of the Cr-content in the alloy are thereby not understood but of fundamental interest.
Our work shows corrosion mechanisms and presents corrosion models for Fe and different Fe-Cr-alloys under pure SO2 und SO2+O2 atmospheres for different time scales. Modell alloys of high purity are used to focus on the reaction of the intended elements: Fe, Cr, S, and O. Long-time experiments (≥12h) took place in tube furnaces and short-time experiments (≥5min) in a special designed light furnace. Heating and cooling took place under inert atmosphere. The reactive gases were added not until the experimental temperature was reached. Samples were analyzed using high resolution synchrotron X-ray diffraction using a micro focus setup and electron microscopy including FIB.
Many earlier studies on corrosion and sulfidation on iron based alloys show a higher corrosion rate and material loss when sulfur was present in the atmosphere. In contrast, later studies propose an inhibiting effect of sulfur containing atmospheres. On the one side, most likely due to the formation of a protective layer of Mx(SO4)y -phases at the scale-gas interface. On the other side, a very recent study proposes the theory that MxSy-phases limit the further diffusion of elements. Up to now, no Mx(SO4)y –phases were detected in our samples, but sulfide phases nucleated within the oxide phases. For pure Fe our samples show FeS at the scale-metal interface working as a diffusion barrier for Fe-Cations from the base material in to the oxide scale. The above lying spalled off oxide-sulfide scale shows a wide area of small voids and accumulations of FeS-Crystals at the bottom. Under the main oxide scale a second generation of oxide-sulfide scale starts to form. For the Fe-Cr-alloys the inner oxide scale only shows FeS- and CrS-phases surrounded by hollow space. The here presented study will explain and discuss a new growth model for the shown phenomenon.
Modulare Hüftprothesen können individuell der Anatomie des Patienten angepasst werden und haben dadurch eine positive Auswirkung auf dessen Lebensqualität. Unter Betriebsbelastung sind in der zusätzlichen Konusverbindung zwischen Schaft und Kopfteil Relativbewegungen möglich. Selbst an Titan-Bauteilen bewirken diese durch Verletzung der Passivschicht Reibkorrosion und infolgedessen Spaltkorrosion. Verunreinigungen wie z.B. Knochenrückstände in der Konusverbindung bewirken eine erhöhte Relativbewegung und führen zusätzlich zu einer örtlichen Spannungsüberhöhung durch lokale Pressung. Die an der Mantelfläche des Schafts entstehenden Korrosionsdefekte reduzieren die Schwingfestigkeit des Schafts erheblich, so dass dort Schwingrisse initiiert werden können, welche dann durch die üblichen zyklischen Schwell-Biegebelastungen bis zum Restgewaltbruch wachsen.
The role of metal reducing bacteria (MRB) in corrosion is being controversially discussed in the literature. They can utilize metals including iron, uranium and manganese as well as many organic compounds as electron acceptors. The reduction of Fe(III) compounds to soluble Fe(II) species leads to the destruction of passive films on steel, resulting in acceleration of general and local corrosion processes. Recent research shows that the secretion of electron shuttles like riboflavins also contribute to the extracellular electron transfer (EET).
The aim of this project is to understand the chemical and electrochemical interaction mechanisms of MRB with steel surfaces by means of combined in situ techniques. An electrochemical XANES (x-ray absorption near edge spectroscopy) cell has been designed to study the changes of passive film chemistry in the presence of biomolecules and MRB. Electrochemical quartz crystal microbalance (eQCM) is used for studying the kinetics of bacterial cell attachment and diffusion of biomolecules in model biofilms. In situ investigations are complemented by ex situ spectroscopic and microscopic analysis to investigate the biofilm structure, composition and cell viability.
Via the combination of electrochemical methods with spectroscopic techniques and QCM we are able to follow biological processes and resulting degradation of steel surfaces in a non-destructive manner. The selection of model systems and a defined biological medium allows the identification of the effects of individual surface and environmental parameters. The fundamental understanding of bacterial attachment mechanisms and initial steps of biofilm formation will contribute to the development of new antifouling strategies.
Oft sind von außen nicht sichtbare „Ungänzen“ im Innern die Ursache für das Versagen von Bauteilen. In manchen Fällen genügt eine herkömmliche metallographische Präparation, um der Schadensursache auf die Spur zu kommen. In anderen Fällen aber sind die Ungänzen zu klein oder ihre Lage zu ungewiss, um sie mit zufälligen Schnitten zu treffen. Zudem würde man durch Fehlversuche das Bauteil zu stark schädigen und so wertvolle Spuren verlieren sowie die weitere Untersuchbarkeit einschränken. In solchen Fällen ist es im wahrsten Sinn des Wortes zielführend, die Ungänzen mit Hilfe eines räumlich abbildenden ZfP-Verfahrens zu lokalisieren und dann mit den erhaltenen Koordinaten eine metallographische Zielpräparation präzise durchzuführen. Als Methoden kommen z.B. Mikro-Computer-Tomographie (µCT) und Tauch-Ultraschall in Frage. Bauteile können kleine elektronische Komponenten sein, aber auch große Bauteile wie Wellen aus Fahrzeugen oder Anlagen.
In the course of miniaturizing modern technology down to the molecular scale, much remain unknown about the materials behavior and the deviations from the bulk that might arises from confinement effects. Here, a combination of nano-sized relaxation spectroscopies (Broadband dielectric spectroscopy (BDS) and Specific heat spectroscopy (SHS); employing AC nanochip calorimetry) were utilized to investigate the glassy dynamics of ultra-thin films of Poly (vinyl methyl ether) (PVME) and of blends PVME / Polystyrene (PS) 50:50 wt-%,, which are miscible in bulk (thicknesses: ca. 8 nm – 160 nm, film thickness was controlled by ellipsometry, film topography by AFM). Both methods are sensitive to different probes; where SHS senses entropy fluctuations while BDS measures dipole fluctuations. For BDS measurements, a recently developed nano-structured electrode sample arrangement is employed, where ultra-thin films are spin-coated on an ultra-flat highly conductive silicon wafer, sandwiched between a wafer with nanostructured SiO2 nano-spacers with heights between 35 nm and 70 nm. For PVME films, two thickness independent processes were observed and interpreted to be the α-processes of a bulk-like layer and a process due to an absorbed layer to the substrate. This adsorbed layer further undergoes a confinement effect that results in the localization of the segmental dynamics, which results in an Arrhenius-like temperature dependence. A detailed analysis of the dielectric strengths of both processes reveals that the thickness of the adsorbed layer decreases with increasing temperature, while that of the bulk-like layer increases. For the blend system, by measuring the dynamic Tg in dependence of the film thickness, SHS showed that the Tg of the whole film was strongly influenced by a nanometer-thick surface layer at the polymer/air interface due to a self-assembling process. The dynamic Tg obtained from the SHS measurements decreased with decreasing film thickness. On the other hand, BDS measurements showed a completely different behavior. At high temperatures, the temperature dependence of the relaxation times of the films follows that of bulk-like PS/PVME; obeying the VFT-law. With decreasing temperature, the temperature dependence deviates from the VFT to an Arrhenius law; where the apparent activation energy decreases with decreasing film thickness. This is the first example where confinement induced changes were observed by BDS for ultra-thin films. All results were analyzed in detail in a comprehensive discussion.
The optical properties of semiconductor nanocrystals (SCNCs) depend on constituent material, particle size, and surface chemistry, with the size of the photoluminescence (PL) quantum yield (QY) and the PL decay kinetics being largely controlled by the number of dangling bonds, which have to be properly passivated for high quality materials. Hence, PL measurements can provide insight not only in SCNC photophysics, yet can be also used for quality control of SCNC synthesis and surface modification. In this respect, steady state and time-resolved fluorometry and confocal microscopy with time correlated single photon counting were used to study the PL properties of core-shell CdSe SCNCs with different shells and surface chemistries on ensemble and single particle level, thereby focusing on a correlation of ensemble PL QY and PL decay kinetics with particle brightness, PL time traces, and the On-time fraction of single SCNCs. Additionally, confocal PL images were correlated with AFM measurements in order to derive the amount of absorbing, yet non-emissive ”dark” SCNCs, the presence of which resulting in an underestimation of ensemble PL quantum yields. The results of this study can help to identify synthetic routes and surface modifications, which minimize the fraction of dark SCNCs.
The optical properties of semiconductor nanocrystals (SCNC) are controlled by constituent material, particle size, and surface chemistry, specifically the number of dangling bonds favoring nonradiative deactivation, and hence also by particle synthesis. In this respect, the fluorescence properties of coreshell CdSe SCNCs with different shells and surface chemistries were studied on ensemble and single particle level, using steady state and timeresolved fluorometry and confocal microscopy with time correlated single photon counting detection. Special emphasis was dedicated to correlate ensemble photoluminescence (PL) quantum yields and decay kinetics with particle brightness, PL time traces, and the Ontime fraction of the single SCNCs. Additionally, the confocal PL images were correlated with AFM measurements in order to derive the amount of absorbing, yet nonemisssive ”dark” SCNCs, the presence of which leading to an underestimation of ensemble PL quantum yields. The results of this study can help to identify synthetic routes and surface modifications minimizing the fraction of dark SCNC, thereby closing the gap to the ultimate goal of colloidally and photochemically stable SCNCs with a PL quantum yield of close to unity.
Maintaining a consistent product quality is critical for the thin film industry. Therefore, the development of highly accurate protocols able to detect variations and nonidealities in manufactured thin film devices is essential and helps improve production quality and decrease manufacturing costs. The present work will discuss the accuracy and reproducibility in the determination of the thickness of thin films relevant for optoelectronic industry using spectroscopic ellipsometry, starting with the importance of set-up calibration, the need for very well defined calibration standards suitable for real devices and not least, the importance of accurate data analysis. As ellipsometry is an indirect method and theoretical modelling is needed to obtain the desired information regarding the investigated samples (e.g. thickness, roughness, optical constants), the model uncertainty has to be discussed and taken into account. If for ideal samples consisting of single layers with well-known optical constants the determination of thickness and roughness is straight forward and pretty accurate, for real samples, more complex theoretical models are needed and extracting accurate information regarding the samples can be very challenging. With careful calibration and a multidisciplinary approach, a combined measurement methodology can be developed enabling reliability, comparability, and accuracy. For production-relevant operation, maintaining the ease of use and scalability of ellipsometry as a technique can also be retained.
In the present study, internal damage to an AlSi12CuMgNi alloy reinforced with planar random Al2O3 short fibres was investigated after compression testing. Due to the alloy composition, this composite contains a second reinforcement phase in the form of eutectic Si, which builds interpenetrated networks in the volume and increases the creep resistance and load-bearing capacity of the material. Materials with their fibre plane parallel and transversal to the load direction were characterized in order to investigate the dependence of load partition and damage on fibre plane orientation. In-situ compression testing during neutron diffraction measurements showed that internal damage is strongly influenced by the load partition between matrix and reinforcement. Moreover, micro-computed tomography was performed in the same material after ex-situ compression for damage analysis. In the case of a fibre plane perpendicular to the applied load, breakage and interconnected cracks appeared in a significantly higher volume fraction than with a fibre plane parallel to load.
Two polyethylene types with ultra high (UHMWPE) and high molecular weight (HMWPE), which are used as neutron radiation shielding materials in storage casks for radioactive waste, were subjected to gamma irradiation doses up to 600 kGy and subsequent thermal ageing at 125 °C for up to one year. One material was a medical grade UHMWPE and the other a HMWPE containing an antioxidant. Degradation effects in the materials were characterized using colorimetry, UV-Vis spectroscopy, MIR and FTIR measurements, DSC and, in the case of HMWPE, insoluble content determination. Both materials exhibited a yellowing upon irradiation. The discoloration of UHMWPE disappeared again after thermal ageing, which is why it was attributed to annealable color centers in the form of free radicals entrapped in the crystalline regions of the polymer that recombine during thermal ageing. Furthermore, oxidation species were observed with MIR and FTIR spectroscopy. For HMWPE, the yellowing occurred during both irradiation and thermal ageing and was correlated to antioxidant decomposition. Additionally, black spots were observed after thermal ageing of HMWPE that were attributed to reaction products of antioxidant derivatives and catalyst residues. While only little evidence of oxidation species was found in the light material parts, oxidation is expected to concentrate in the black spots as the catalyst residue promotes hydroperoxide decomposition and thus radical formation that initiate polymer oxidation
A test campaign was launched to determine the mechanical properties of the HL-LHC 11 T Nb₃Sn magnet components in order to accurately model the mechanical properties in Finite Element simulations that predict the stress and strain distribution in these magnets. Static and dynamic test methods have been applied for determining elastic materials behavior, and highly accurate Young’s moduli are obtained with the dynamic methods resonance and impulse excitation. These non-destructive methods also enable temperature dependent modulus measurements during in situ heat cycles.
Polymers are favorable materials for gas separation membranes. In general, gas transport experiments are performed with films in the range of 100 µm thickness. However, in large-scale processes very thin selective polymer layers in the range of 100 nm to 1 µm are used. Moreover, it was shown that thin films behave different compared to thick films with respect to gas transport properties and physical aging as well. Thus, for fundamental research it is important to realize gas transport experiments with thin films. The Quartz Crystal Microbalance (QCM) is a very sensitive method to detect mass changes in the range of nanograms. Therefore, this method enables sorption experiments with thin films or layers attached to the QCM crystal (100 nm up to 1 µm). Here, we present the experimental set-up for using the QCM technique for characterizing the gas sorption behavior of thin polymer films in a temperature controlled pressurized environment (up to 50 bar) - also quartz crystals and crystal holders were optimized. The study aims for the characterization of long-term behavior and physical aging of high-performance polymers for gas separation membranes - such as polyimides and polymers of intrinsic microporosity (PIMs) and respective nanocomposites. Especially the differences of the behavior of thin films compared to films with thicknesses up to 100 µm as well as nanofiller induced-effects are adressed.
Low-alloyed CrMoV steels, such as T24, are widely used for welded components in fossil power stations due to their excellent creep-strength. Spectacular failure cases in the recent years exhibited severe cracking in T24 welds. The results showed that hydrogen-assisted cracking (HAC) occurring up to 200 degree Celsius cannot be excluded. Hence, a basic understanding is necessary on how hydrogen affects the material properties of welded microstructures. In this regard, each weld microstructure (HAZ and weld metal) has influence on the HAC susceptibility and respective hydrogen diffusion. Thus, the present contribution summarizes different results obtained from experiments with grades T24 (CrMoV alloy) and T22 (CrMo) and thermally simulated HAZ. Tensile tests were conducted with hydrogen charged specimens and compared to hydrogen-assisted stress corrosion cracking results obtained from slow strain rate tests (SSRT) up to 200 degree Celsius. Electrochemical permeation and degassing experiments were performed to identify a particular weld microstructure influence on hydrogen diffusion and trapping (especially in the HAZ). The results showed that T24 base material has improved resistance to hydrogen-assisted degradation/cracking. In contrast, the as-welded HAZ had remarkably increased susceptibility (tesnile tests at hydrogen concentration of 1 to 2 ppm). SSRT experiments confirmed this at elevated temperatures for both the T24 and the T22. Hence, the evaluation of a particular degradation of the mechanical properties should be performed independently for each weld microstructure. In addition, the HAZ showed decreased diffusion coefficients (at room temperature) of approximately one magnitude compared to the base materials. Trapped hydrogen was determined in the T24 at temperatures up to 120 degree Celsius compared to 75 degree Celsius in the T22. This has to be considered in case of changing operational temperatures, e.g. in the case of start-up and shutdown processes of boiler components.
Derzeit wird der Einsatz metallener Werkstoffe in CCU-/CCS-Anlagen hinsichtlich deren Korrosionsbeständigkeit und eine eventuell daraus resultierende Herausforderung diskutiert. Während des CO₂-Transportes vom Abscheide- zum Injektionsort kann es aufgrund der den CO₂-Strom begleitenden Beimengungen, wie Wasser, O₂, SOₓ , NOₓ , Temperaturschwankungen durchaus zu Kondensationseffekten und daraus resultierenden Schäden kommen.
Es konnte gezeigt werden, dass die sich möglicherweise innerhalb einer CO₂-Rohrleitung bildenden Kondensate infolge von Begleitstoffen wie SO2 und NO2 eine viel korrosivere Wirkung auf Rohrleitungswerkstoffe entfalten, als in reinem CO₂.
In letzter Zeit kommen immer mehr alternative Energiequellen als Ersatz fossiler Brennstoffe zum Einsatz, so auch die Solarthermie. Jedoch sind die Betriebsbedingungen aufgrund der chemischen Zusammensetzung der Wärmeträgermedien und herrschenden Temperaturen extrem hinsichtlich Korrosion. Da die Kraftwerke bei maximaler Lebensdauer ökonomisch vertretbar sein müssen, ist eine Werkstoffauswahl basierend auf Voruntersuchungen notwendig, um einen sicheren und verlässlichen Betrieb dieser Anlagen zu gewährleisten.
Die Werkstoffauswahl hängt von der Betriebstemperatur eines Kraftwerks bzw. der chemischen Zusammensetzung des Wärmeträgermediums ab. In hochkorrosiven Umgebungen werden aufgrund ihrer sehr guten Korrosionsbeständigkeit Nickelbasislegierungen nicht nur für stark korrosiv beanspruchte Bauteile als die Lösung angesehen. Jedoch kann es durchaus beständigkeitsbedingte Einschränkungen für den Einsatz geben, wofür die hier vorgestellten Ergebnisse dienen sollen.
In diesem Beitrag wird die Beständigkeit ausgewählter hochlegierter Werkstoffe (inklusive einer neuentwickelten Legierung in einer Nitrat-Salzschmelze (60 % NaNO3/40 % KNO3) vorgestellt, die mittels elektrochemischer Messungen und Auslagerungsversuchen ermittelt wurde.
Since geothermal wells are a feasible energy source to replace fossil fuel supply, many technologies have been developed to take advantage of geothermal energy. Nevertheless, service conditions in geothermal facilities are due to the chemical composition of hydrothermal fluids and temperatures, in many cases, extreme in terms of corrosion.
Therefore, materials selection based on preliminary material qualification is essential to guarantee a secure and reliable operation of the facilities. The corrosion behavior of different high-alloyed metals including Duplex and austenitic stainless steels as well as a nickel alloy have been evaluated in artificial geothermal fluids simulating the conditions in some locations with geothermal potential in Germany as well as two sites in Indonesia. The suitability of carbon steel 25CrMo4, stainless steels X2CrNiMo17-12-2, X2CrNiMo-22-5, X2CrNiMoCuWN25-7-4 and super austenitic steel X1CrNiMoCu32-28-7 in these geothermal fluids obtained by electrochemical measurements and exposure tests is limited. The nickel alloy NiCr23Mo16Al shows an excellent corrosion resistance against pitting corrosion. Excluding its high cost, it is a very good alternative to be used in the construction of geothermal facilities having highly saline brines. Stainless and Duplex steels exhibit a limited corrosion resistance concerning pitting and crevice corrosion. Beside of the higher alloyed materials, also the lowalloyed steel 25CrMo4 could be employed as a constructional material for the geothermal power plant in stagnant highly acidic non Saline environments, as long as the wall thickness of the material vs. corrosion rate is taken into account.
The formation of biofilms on different materials provokes high costs in industrial processes, as well as in medical applications. Therefore, the interest in development of new materials with improved surfaces to reduce bacterial colonization rises. In order to evaluate the quality and safety of these new materials, it is highly important to ensure world-wide comparable tests that are relying on statistical evidence. The only way to reach this statistical safety is through a high-throughput Screening under standardized test conditions.
We developed a flow through system for cultivation of biofilm-forming bacteria under controlled conditions with a total capacity for testing up to 32 samples in parallel. Quantification of the surface colonization was done by staining the bacterial cells with a fluorescence marker, followed by epifluorescence microscopy. More than 100 images of each sample were automatically taken and the surface coverage was estimated with the free open source software gmic (http://gmic.eu), followed by a precise statistical evaluation. Overview images of all gathered pictures of the whole material coupon were generated to illuminate the colonization characteristics of the selected bacteria on certain materials.
With this method, differences in bacterial colonization on different materials can be quantified in a statistically validated manner. The innovative and solid test procedure will support the design of improved materials for medical and industrial applications such as implants, ship hulls, pipelines, heat exchangers, aquaculture equipments, photovoltaic-panels and fundaments of wind power plants.