Universität Stuttgart
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Item Open Access Wetting, de-icing and anti-icing behavior of microstructured and plasma-coated polyurethane films(2019) Grimmer, Philipp E. S.; Hirth, Thomas (Prof. Dr. rer. nat.)Ice build-up on surfaces, for example on wings of airplanes or on rotor blades of wind turbines, impairs the functionality of transportation vehicles or technical systems and reduces their safety. Therefore, functional anti-ice surfaces are being researched and developed, which shall enable an easy removal or reduce the amount of ice on the surfaces at risk. The starting hypothesis for this work is that superhydrophobic polyurethane (PU) films with microstructure base diameters of 35 µm or more reduce the wetting by water, show a low ice adhesion for easy removal of ice and reduce or delay icing. Superhydrophobic PU films for passive anti- and de-icing were created by hot embossing and plasma enhanced chemical vapor deposition (PECVD). The hot embossing process as well as the plasma coating and etching processes were analyzed for the dependence of the surface characteristics on different process parameters. The functionalized PU films were characterized for their surface topography, surface chemistry, stability against erosion, wettability, ice adhesion and icing behavior. For comparison, the ice adhesion and icing behavior were examined on relevant technical materials (aluminum, titanium, copper, glass, epoxy resin of carbon fiber reinforced polymer and other fluoropolymers) and on some commercial anti-ice coatings. The PU films were chemically analyzed by IR spectroscopy. As the first process step for functionalization, microstructures of cylindrical, elliptical or linear shape were imprinted in PU films by a hot embossing technique with different ns-pulsed laser-drilled stamps and characterized by several microscopy methods. The microstructures had heights of 15 µm to 140 µm, diameters or widths of 35 µm to 300 µm and distances (pitch values) of 50 µm to 500 µm. The embossing process was analyzed and optimized in terms of the process parameters temperature, pressure, time, PU film release temperature and reproducibility of the microstructures. In a second functionalization step (PECVD) the microstructured surfaces were coated with thin, hydrophobic plasma polymers using different fluorocarbon precursors (CHF3, C3F6 and C4F8) or hexamethyldisiloxane (HMDSO). Different process parameters for plasma coating and etching (Ar or O2 plasmas) were used in order to create various nanoscale roughness values. Electron spectroscopy for chemical analysis (ESCA), spectroscopic ellipsometry and atomic force microscopy (AFM) were used for analysis of the chemical composition, the thickness and the nanoroughness of the plasma polymers. The functionalizations, especially the plasma coatings, were completely worn off by a UV/water weathering test (1000 h, X1a CAM 180 Test, SAE J-2527), but showed sufficient stability against sand erosion (DIN 52348), in a long-term outdoor test for 13.5 months and against fivefold repeated pull-off of ice. The silicone-like plasma coatings were more stable than the fluorocarbon plasma coatings. The wetting behavior of water was determined by static, advancing and receding contact angle measurements. Static contact angle measurements with diiodomethane (DIM) were made for determination of the surface free energies of the relevant surfaces. Advancing contact angles of over 150° and very low contact angle hysteresis values below 10° were reached on some of the cylindrically and elliptically structured PU samples with microstructure base diameters in the range of 35 µm to 50 µm. The measured water advancing contact angles did not reach the theoretical values of the Cassie-Baxter state. Starting from a mixed wetting state near Cassie-Baxter in case of the superhydrophobic PU surfaces, they approached the Wenzel state with an increasing pitch/diameter (P/d) factor. Fluorescence laser scanning microscopy images were taken of some microstructured, uncoated or plasma coated samples during the wetting by a water drop containing a fluorescent dye. These images show the Wenzel state or a mixed wetting state by visualization of the interface between the water droplet and the surface. A new icing test chamber and a test setup were developed for characterization of the ice adhesion and the icing behavior. The tensile ice adhesion was measured at -20 °C by pull-off of ice cylinders (highly purified water, (<0.056 µS/cm, diameter of 4 mm, similar to the diameter of large raindrops) and compared to the theoretical values and the wetting behavior. The technical material surfaces measured for comparison showed a high ice adhesion, which led to cohesive fractures especially on the metal surfaces, whereas some of the commercial anti-ice coatings showed lower ice adhesion values. The flat, plasma coated PU surfaces showed adhesive fractures with a reduced ice adhesion compared to the technical material surfaces and uncoated PU and revealed a good correlation of the ice adhesion with the wetting behavior of water (work of adhesion). On the other hand, the microstructured PU surfaces showed a greatly increased ice adhesion in comparison to the flat PU and technical material surfaces which was enhanced even further by the plasma coatings and did not correlate with the wetting behavior. The reason for this is the wetting transition from the Cassie-Baxter to the Wenzel state during the cooling or freezing process, leading to an increased ice-surface contact area and mechanical interlocking of the ice with the micro- and nanostructures. The freezing of water drops was examined in thermodynamic equilibrium (static experiment) and under quasi-steady conditions (dynamic experiment). In the static experiment, 15 µl water drops (corresponding to medium to large raindrops) at room temperature were dispensed onto a cold surface at a constant temperature of -20 °C. The freezing delay times, the crystallization times and the total freezing times were measured and compared to calculated expected values. On the flat samples, the freezing delay times could be extended by the plasma treatments. On the microstructured samples, the freezing (nucleation) could sometimes be delayed even further, but not always reproducible because of an unstable Cassie-Baxter state. In the dynamic experiment, 25 µl water drops (corresponding to large raindrops) were cooled down in quasi-steady conditions with the surface and the surrounding atmosphere by a constant, low cooling rate of 1 K/min while the water drop temperature was measured by an IR camera for determination of the surface-specific nucleation temperature and crystallization time. A lower nucleation temperature could be measured on the flat, plasma coated PU surfaces compared to uncoated PU and the hydrophilic glass and metal surfaces. The superhydrophobic PU surfaces did not show a further reduction of the nucleation temperature because of an unstable Cassie-Baxter state. The resulting measured nucleation temperatures were compared to the expected values calculated with an enhanced nucleation theory including a quasi-liquid interfacial layer of the ice nucleus and a Poisson process. Overall, it is shown that hot embossing and PECVD are useful processes for creating superhydrophobic PU surfaces with regard to a roll-to-roll process. The flat, plasma coated PU films show a reduced ice adhesion and lowered nucleation temperature compared to the relevant technical material surfaces. The microstructured, plasma coated PU films are far more water repellent than the flat, plasma coated PU surfaces or the other technical materials. However, the microstructures with base diameters of 35 µm or more and the nanoroughness of the plasma coatings cannot stabilize the Cassie-Baxter state of a freezing water drop enough for a low ice adhesion or a significant decrease of the nucleation temperature. These superhydrophobic PU films are therefore not more icephobic than the flat, plasma coated PU films. In the outlook, the reduction of the geometrical parameters of the microstructures (diameter D, distance P) and nanostructures (curvature radius R) of the surface functionalizations for lower ice adhesion values and nucleation temperatures is proposed.Item Open Access Diagnostik und Modellierung eines Mikrowellen-Plasmabrenners bei Atmosphärendruck(2017) Gaiser, Sandra; Hirth, Thomas (Prof. Dr.)Mikrowellen-Plasmaprozesse bei Atmosphärendruck bieten eine Vielzahl von Anwendungsmöglichkeiten. Dazu gehören das Plasmaspritzen zur Beschichtung, die Behandlung von Oberflächen für die Reinigung oder Aktivierung sowie der Abbau schädlicher Abgase. Für die Entwicklung und Optimierung dieser Verfahren sind sowohl experimentelle Untersuchungen als auch eine theoretische Betrachtung von Bedeutung. Diese Arbeit beschäftigt sich deshalb neben der Diagnostik vor allem mit der Modellierung und numerischen Simulation eines bei Atmosphärendruck betriebenen Mikrowellen-Plasmabrenners. Dazu wird die Simulationssoftware Comsol Multiphysics verwendet. Das Ziel ist es, mittels einzelner Modelle die unterschiedlichen physikalischen Vorgänge zu beschreiben und das Brennersystem zu optimieren. Die Simulationen werden schließlich schrittweise miteinander verknüpft, um so ein möglichst selbstkonsistentes Modell der Plasmaquelle zu erhalten. Die Simulationsergebnisse werden zudem mit experimentellen Daten verglichen. Zunächst werden die Verteilung des Mikrowellenfeldes im Plasmabrenner sowie die Resonanzfrequenzen der Resonatoranordnung berechnet, was die Grundlage für eine zuverlässige Zündung und den Betrieb des Plasmas bildet. Anschließend wird ein Modell der kalten Gasströmung erstellt. In dieses wird schließlich eine Wärmequelle implementiert, um den Einfluss des heißen Plasmas auf die Strömung zu untersuchen. Die Gasströmung soll dahingehend optimiert werden, dass sie das Plasma einschließt, um so eine Beschädigung des Gas führenden Quarzrohres zu vermeiden. In einer weiteren Simulation wird das Plasma mit Hilfe des Drude-Modells beschrieben. Hierbei werden dem Plasma eine Permittivität und eine Leitfähigkeit zugewiesen. Eine Erweiterung erfolgt durch das Fluid-Modell, das Bilanzgleichungen für die Elektronendichte sowie Reaktionsmechanismen für ein Argon-Plasma enthält. Die Simulationsergebnisse werden durch den Vergleich mit experimentellen Ergebnissen verifiziert. Dazu wird zum einen die räumliche Lage des Plasmas mit Hilfe von Kameraaufnahmen qualitativ untersucht. Zum anderen stehen Messwerte aus der optischen Emissionsspektroskopie zur Verfügung.Item Open Access Barrier properties and analysis of defects of plasma polymerized hexamethyldisilazane-based films(2019) Troia, Mariagrazia; Hirth, Thomas (Prof. Dr.)A great variety of commercially available goods, e. g. food products, require a degree of protection against gases and vapors. Electronic devices whose active layers are based on organic materials in particular demand extremely low oxygen transmission rates in order to attain adequate lifetimes. In order to do so, an encapsulation of the device by means of a barrier becomes necessary. In case of flexible devices, such as organic light emitting devices (OLEDs), conventional encapsulation methods relying on stiff glass lids cannot be employed. Plasma-enhanced chemical vapor deposition (PECVD) methods on the other hand have been proven to be successful in obtaining thin films (in the range of tens or hundreds of nanometers) which combine good barrier performances with flexibility and other favorable mechanical properties. In the current work, thin silica-like (SiOx) films have been deposited on polyethylene terephthalate (PET) through a low-pressure microwave plasma and a gaseous feed consisting of hexa-methyldisilazane (HMDSN) and oxygen, with the aim of providing flexible oxygen barrier layers with additional properties as transparency, colorlessness, good adhesion to the substrate and resilience. Operational parameters such as the gas feed composition, microwave power and deposition time have been investigated and optimized, thus obtaining inorganic barriers with an optimal thickness in the 50 to 100 nm range and with a barrier improvement, when compared to the uncoated substrates, up to a factor of 100. The defects in the barriers have been investigated by means of a concurrently developed non-destructive method for their localization and identification, based on the precipitation of calcium carbonate crystallites on top of them, which allows the defect to be later retrieved and investigated by means of microscopy methods. Further analyses of the transmission rates have been carried out at different temperatures in order to investigate the permeation mechanisms through the bulk and the defects. The films, when compared to barriers deposited via the common precursor hexamethyldisiloxane (HMDSO), obtained in the same experimental setup, showed consistently better properties in a wider range of conditions, proving HMDSN to be a better precursor for thin films with barrier applications. Multilayer systems, based on the combination of SiOx films and an intermediate organic layer optimized in parallel to the barriers, have been developed, tested and used successfully for the encapsulation of flexible Organic Light Emitting Device (OLED) prototypes printed on polymers.Item Open Access Experimental and numerical study of turbulence in fusion plasmas using reflectometry synthetic diagnostics(2018) Zadvitskiy, Georgiy; Tovar, Günter (Prof. Dr.)Anomalous energy and particle transport is closely related to micro-turbulence. Therefore plasma turbulence studies are essential for successful operation of magnetic confinement fusion devices. This thesis deals with the development of interpretative models for Ultra-Fast Swept Reflectometry (USFR), a diagnostic used for the measurement of turbulence radial wave-number spectra in fusion devices. While the interpretation of reflectometry data is quite straightforward for small levels of turbulence, it becomes much trickier for larger levels as the reflectometer answer is no longer linear with the turbulence level. It has been shown for instance that resonances due to probing field trapping can appear in turbulent plasma and produce jumps of the signal phase. In the plasma edge region the turbulence level is usually high and can lead to a non-linear regime of the reflectometer response. The loss of probing beam coherency and beam widening when the probing beam crosses the edge turbulence layer can affect USFR core measurements. Edge turbulence with a long correlation length leads to small beam widening and strong distortion of the probing wave phase. However backscattering effects from turbulence with short correlation lengths are also able to cause reflectometer signal change. To study turbulence wave-number spectra as well as reflectometer signal phase variations, signal amplitude variations can be analized. Unlike signal phase variation, amplitude does not suffer from resonant jumps, and can give more clear qualitative evaluation of turbulence structure. In the case when the turbulence amplitude peaked in the edge region, it can be detected as spectral peak near local Bragg resonance wave-number. USFR with a set of receiving antennas arranged poloidally was proposed to obtain more information on the edge turbulence properties. A displacement of the spectral peak appears when the receiving antenna is misaligned with the emitting one. Peak displacement measurements could provide additional information on probing beam shaping and turbulence properties and help in coherent mode observation as well. A 2D full wave code was applied as a synthetic diagnostic to Gysela gyro-kinetic code data to study Tore-Supra tokamak core turbulence. Radial correlation lengths computed from the amplitude of multi-channel fixed frequency reflectometry signals 5have shown good agreement with the turbulence correlation length directly computed from the simulation. The synthetic diagnostic was then applied to analyse the correlation length and wave-number spectra obtained by USFR in the ASDEX-Upgrade tokamak. A comparison between 1D and 2D results have shown different behaviour. However correlation lengths measured with UFSR signals are in the same order with turbulence ones.Item Open Access Investigation into the influence of magnetic field structure on the dynamical and spatial properties of plasma edge turbulence in the stellarator TJ-K(2019) Garland, Stephen; Hirth, Thomas (Prof. Dr.)Nuclear fusion could provide the solution to our rising energy demands in a world where greenhouse gas emissions must be rapidly reduced (Germany plans a 55 % reduction by 2030, compared to 1990 levels). In order to have sufficient rates of fusion a high-temperature, relatively dense plasma is required. Containing such a plasma for long enough for fusion to occur at sufficient rates is challenging. One solution is to confine the plasma with strong toroidal magnetic fields. Whilst this drastically improves the confinement, particles and heat are still transported towards the reactor walls, reducing the temperature and density, and posing a threat to wall components. The main contribution to outward transport in fusion-relevant reactors comes from turbulent fluctuations in the plasma potential and density. The aim of this thesis is to investigate the effect of magnetic field geometry on the spatial, statistical and dynamical properties of turbulence in the confined region of the plasma, dominated by drift-wave turbulence, and the region close to the reactor wall (scrape-off layer), where the turbulence has an intermittent character due to outward-travelling high-amplitude pressure perturbations, often called blobs. A high proportion of scrape-off layer transport towards the reactor wall is due to blob filaments. The generation of blobs is known to be linked to drift-wave turbulence, and so the intermittent nature of scrape-off layer turbulence could have its origin in the confined plasma. To gain an understanding of the intermittent properties of drift-wave turbulence, simulations were carried out with a simple slab geometry model and compared to experimental measurements at the stellarator TJ-K. It was found that the density fluctuations become more intermittent with increasing plasma collisionality, due to a progressive decoupling of density and potential fluctuations. An extended version of the model, accounting for magnetic curvature, predicted more intermittent density fluctuations on the outboard side of the reactor, where the normal curvature is negative. Experiments showed that the most intermittent fluctuations are in fact shifted into the region where the normal curvature is negative but the geodesic curvature is positive. This shift could be understood by considering the spatial properties of the turbulence, which enter into the density-potential coupling terms in the model. Furthermore, the local magnetic shear was found to have a damping effect on drift-wave turbulence, which locally reduces the cross-sectional areas of turbulent structures. Blob dynamics were studied using a three-dimensional gyrofluid model, in which blob filaments are generated self-consistently. An effect of the magnetic curvature was found not only on the radial blob speeds, which is well known, but also on the binormal velocity component. This result was also found in experiments at TJ-K, where the geodesic curvature drive was shown to contribute significantly to poloidal blob speeds. In addition, the structure of blob filaments was studied in the experiment. It was found that the magnetic shear does not have a deforming effect, and that blobs retain the filamentary form that they have near their generation region.Item Open Access Investigation of geodesic acoustic mode flow oscillations using Doppler reflectometry in ASDEX Upgrade(2017) Simon, Patrick; Tovar, Günter (Prof. Dr.)Magnetic confinement fusion is a promising candidate for a future energy source. Its efficiency is limited by particle and heat transport due to plasma turbulence. A thorough understanding of the turbulence and turbulence moderation mechanisms, is therefore needed. The geodesic acoustic mode (GAM) is a radially localised plasma flow oscillation which contributes to the reduction of turbulent transport through velocity shearing. This thesis investigates the fundamental behaviour of the GAM through a systematic experimental study of its properties in the ASDEX Upgrade tokamak. In particular, the role of the plasma geometry on the scaling of the GAM frequency and amplitude, as well as the GAM radial structure are investigated in detail. The experimental data was obtained with the aid of the microwave Doppler reflectometry diagnostic. The GAM frequency scaling is compared with multiple models which reproduce the expected fundamental scaling behaviour, but do not give a satisfyingly accurate prediction. The GAM amplitude is studied in connection with damping rates predicted by models for collisional and collisionless Landau damping processes. It is found that finite orbit width effects need to be considered and that collisional damping effects cannot be neglected. In studying the GAM radial structure, three distinct states are identified for different plasma conditions. Transitions between these states are observed under variations of the plasma geometry.Item Open Access Investigation of tungsten exposed to fusion relevant intense H/He particle fluxes and thermal loads(2016) Lemahieu, Nathan; Tovar, Günter (Prof. Dr.)