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Eingeladener Vortrag
- nein (1)
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