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Eingeladener Vortrag
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Mechanical characterization of high-density polyethylene in contact with diesel and biodiesel fuels
(2016)
Renewable resources become more and more relevant to maintain energy demands for an increasing global population. Biosynthetic fuels like biodiesel might replace conventional petrochemical fuels, such as diesel. However, more research is needed to characterize the interaction between the different fuels and polymeric materials widely used in the fuel infrastructure as well as for automotive parts. Especially changes in the structural properties and mechanical behavior of the polyethylene (PE-HD) have to be addressed.
The presented work comprises the direct interaction of high density polyethylene (PE-HD) with diesel and biodiesel, resulting in swelling and plasticization. Also long-term degradation phenomena will be discussed.
The chosen PE-HD types are typical thermoplastic resins for container and storage tank applications. The impact of diesel and biodiesel in PE-HD is investigated by changes in the mechanical properties with emphasis on the Charpy impact strength. Furthermore, structural and dynamic influences on the polymeric material induced by diesel and biodiesel are proven in Dynamic Mechanical Analysis (DMA). Both methods, Charpy impact strength and DMA, reveal softening effects due to the migration of diesel and biodiesel into the amorphous regions of PE-HD.
Since biodiesel is more prone to oxidative degradation compared to diesel, the fuel/air/polymer-interaction is studied for partly immersed tensile test specimens. Main focus of the evaluation is the co-oxidation. Here, the accelerated deterioration of PE caused by the sorption of the facile oxidation of biodiesel into the solid polymer might be a major degradation mechanism in this context.
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.
Due to their chemical structure, a rigid disk-like aromatic core and flexible alkyl chains attached to the core, discotic liquid crystals (DLCs) can organize and stack themselves into columns in a hexagonal columnar mesophase, a mesophase in between the plastic crystalline and isotropicphase. The overlap of the π orbitals of the aromatic core in the hexagonal columnar mesophase leads to a high charge-carrier mobilitie along the column axis – these columns can be considered as “moleculer nanowires” making liquid crystals a promising class of materials for electronic applications. Previous studies on DLCs showed that the phase behavior of DLCs is susceptible to nano confinement. Here in this study, the thermotropic collective orientational order of 2,3,6,7,10,11 hexakis[hexyloxy] triphenylene (HAT6), a triphenylene based DLC, and the effects of nano confinment on of its phase behavior were investigated by broadband dielectric spectroscopy (BDS) and differential scanning calorimetry (DSC). HAT6 was embedded into nanoporous anodic aluminum oxide membranes by melt infiltration in the isotropic phase under argon atmosphere. The filled membranes have the thickness of 80 µm and the diameter of 15mm and parallel aligned tubular nanopores having the pore diameters of 25, 40, 80 and 180 nm. The filling degree for each sample was checked by thermogravimetric analysis (TGA) in order to ensure complete filling. The bulk HAT6 forms, a hexagonal columnar phase between the isotropic phase above 371 K, and the plastic crystalline phase below 340 K. Unlike the bulk, the confined HAT6 forms two peaks in the heat flow during the plastic crystalline-to-hexagonal columnar phase transition, which might be the evidence of two different phase structures close to the wall and in the pore center. Moreover, the isotropic-to-columnar transition of the confined HAT6 shifts with decreasing pore diameter to lower temperatures.
The Full-Notch Creep Test (FNCT) is widely used to characterize the slow crack growth (SCG) behavior of polyolefin materials in “inert” media as well as effects of environmental stress cracking (ESC) in which the medium has decisive influence on damage mechanism and time to failure tf*. Usually the FNCT is applied as a standardized testing method (ISO 16770) using a few universal liquid media, such as solutions of Arkopal N 100 (detergent).
Selected relevant PE-HD materials are investigated also in real media and influences of temperature and geometry of specimen and notch are explicitly addressed. The investigations comprise also the ESC behavior of PE-HD in media that are sorbed to a significant extent – such as Diesel and Biodiesel – based on comparison with samples previously saturated with those media.
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.
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.
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.
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.
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.
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.