Universität Stuttgart
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Item Open Access PFG-NMR studies of ATP diffusion in PEG-DA hydrogels and aqueous solutions of PEG-DA polymers(2018) Majer, Günter; Southan, AlexanderAdenosine triphosphate (ATP) is the major carrier of chemical energy in cells. The diffusion of ATP in hydrogels, which have a structural resemblance to the natural extracellular matrix, is therefore of great importance to understand many biological processes. In continuation of our recent studies of ATP diffusion in poly(ethylene glycol) diacrylate (PEG-DA) hydrogels by pulsed field gradient nuclear magnetic resonance (PFG-NMR), we present precise diffusion measurements of ATP in aqueous solutions of PEG-DA polymers, which are not cross-linked to a three-dimensional network. The dependence of the ATP diffusion on the polymer volume fraction in the hydrogels, φ, was found to be consistent with the predictions of a modified obstruction model or the free volume theory in combination with the sieving behavior of the polymer chains. The present measurements of ATP diffusion in aqueous solutions of the polymers revealed that the diffusion coefficient is determined by φ only, regardless of whether the polymers are cross-linked or not. These results seem to be inconsistent with the free volume model, according to which voids are formed by a statistical redistribution of surrounding molecules, which is expected to occur more frequently in the case of not cross-linked polymers. The present results indicate that ATP diffusion takes place only in the aqueous regions of the systems, with the volume fraction of the polymers, including a solvating water layer, being blocked for the ATP molecules. The solvating water layer increases the effective volume of the polymers by 66%. This modified obstruction model is most appropriate to correctly describe the ATP diffusion in PEG-DA hydrogels.Item Open Access Simulation of microwave beams with PROFUSION(2019) Plaum, BurkhardItem 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 Charakterisierung der 2. Harmonischen EBW-Heizung(2013) Höfel, UdoElektron-Bernstein-Wellen (EBW) können dazu benutzt werden ein überdichtes Plasma effektiv zu heizen, da für für ihr Eindringen ins Plasma kein oberes Limit in der Elektronendichte existiert, sie allerdings sehr gut an der Elektronzyklotronresonanz (ECR) absorbiert werden. Dies gilt nicht nur für die direkte Absorption an der ECR, sondern auch an deren Harmonischen. Die EBW muss dazu allerdings durch Modenkonversionsprozesse aus einer von außen eingestrahlten Mikrowelle erzeugt werden, da sie im Vakuum nicht ausbreitungsfähig ist. Im Stellarator TJ-K der Universität Stuttgart konnten erstmals Plasmen durch EBW-Heizung an der zweiten Harmonischen stabil erzeugt und somit gezielt untersucht werden. Hierzu wird eine Mikrowelle mit einer Frequenz von 8 GHz und einer Leistung von 2,7 kW in ein Plasma mit einer Magnetfeldstärke von ungefähr 220 mT eingestrahlt. Umfangreiche Studien der Plasmaparameter, wie zum Beispiel der Elektronentemperatur und der Plasmadichte mithilfe von Langmuir-Sonden deuten auf eine gesteigerte Heizeffizienz im Vergleich mit bisherigen Operationsbereichen in TJ-K hin.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 Dynamics and structure analysis of coherent turbulent structures at the boundary of toroidally confined plasmas(2013) Fuchert, Golo; Stroth, Ulrich (Prof. Dr.)Die sichere und finanzierbare Deckung des steigenden Energiebedarfs ist eine der größten Herausforderungen unseres Jahrhunderts. Kernfusionskraftwerke nach dem Prinzip des magnetischen Einschlusses können möglicherweise einen entscheidenden Beitrag leisten. Derzeit verhindern Energieverluste des Fusionsplasmas durch Turbulenz einen effizienten Betrieb und erhöhen die Erosion der Innenwand des Fusionsreaktors. Nahe der Wand, in der sogenannten Abschälschicht, wird der Transport dominiert von Blobs oder Filamenten: lokalisierte Strukturen erhöhten Drucks, die Energie und Teilchen in Richtung der Wand transportieren. Der Transport hängt unter anderem ab von der Größe, Geschwindigkeit und Entstehungsrate der Blobs. Für einfache Geometrien des einschließenden Magnetfelds sagt ein analytisches Modell die Größe und Geschwindigkeit der Blobs voraus, nicht aber die Entstehungsrate. Experimentelle Beobachtungen deuten auf eine Beteiligung der Randschichtturbulenz in der Nähe der letzten geschlossenen Flussfläche (dem Beginn der Abschälschicht) bei der Blobentstehung hin, was sich in der Entstehungsrate widerspiegeln sollte. Diese Arbeit beantwortet vorrangig zwei Fragen: Beschreiben die einfachen Modelle die Blobeigenschaften auch in Magnetfeldgeometrien tatsächlicher Fusionsexperimente und welchen Einfluss hat die Randschichtturbulenz auf diese Eigenschaften? Mit einer Hochgeschwindigkeitskamera wurden Größe, Geschwindigkeit und Entstehungsrate der Blobs im Stellarator TJ-K und dem Tokamak ASDEX Upgrade untersucht. Während eine grundsätzliche Übereinstimmung mit den Vorhersagen besteht, konnte zum ersten Mal gezeigt werden, dass die Randschichtturbulenz die untersuchten Eigenschaften beeinflusst. Die Messungen beinhalten den ersten systematischen Vergleich der Strukturgrößen inner- und außerhalb der letzten geschlossenen Flussfläche. Darüber hinaus wird mit Sondenmessungen die dreidimensionale Struktur der Blobs in einem Stellarator vermessen und gezeigt, dass die Blobs mehr als 50 % des lokalen und mehr als 20 % des totalen Transports in der Abschälschicht ausmachen. Messungen eines Stroms entlang der Filamente bestätigen, dass das analytischen Modell die relevanten physikalischen Prozesse behinhaltet. In ASDEX Upgrade werden Blobeigenschaften bestimmt und in zwei Einschlussregimen, der sogenannten L- und H-Mode, verglichen. Wie schon in TJ-K zeigt sich eine weitgehende Übereinstimmung mit den analytischen Vorhersagen. Größenmessungen deuten einen Einfluss der hohen Ionentemperatur auf die Blobdynamik hin. Außerdem wird eine überraschend geringe Variation der Blobeigenschaften zwischen L- und H-Mode beobachtet.Item Open Access Microwave heating of plasmas with the new 14 GHz system at the stellarator TJ-K(2013) Loiten, MichaelThe aim of this thesis has been to investigate the plasmas generated by the newly installed 14 GHz microwave heating system at TJ-K in the equilibrium state. The new heating system has been installed in order to operate TJ-K at a wider range of controllable parameters. Several diagnostics have been used to investigate the plasma: An interferometer was used to obtain the line averaged density. A radially movable device with three Langmuir probes was used to obtain the radial profiles of the electron density and the electron temperature. An optical diode was used to obtain the radiation mainly in the visible range, whereas a bolometer with eight channels was used in order to obtain the poloidal radiation profiles. In addition, the neutral gas pressure, the magnetic field (based on the current running through the coils), and the injected and reflected microwave power was measured. Magnetic and pressure scans in the new regime have been performed, meaning that the scanned parameter has been varied on a shot to shot basis, whereas the other parameters have been kept constant. In addition to increase the parameter space, the magnetic field has been varied in order to vary the power deposition in the plasmas. The pressure has been varied in order to approach regimes where neoclassical effects become important. When lowering the collisionality, collisional regimes where neoclassical effects dominates can be reached. Lower collisional regimes were found for low pressures in hydrogen. However, operation at these collisional regimes is not readily available as it was found that the plasmas become increasingly unstable when closing in on these regimes. With this heating system one can operate at higher magnetic fields, and thus increase the confinement of the plasma. It has been found that plasmas in this regime have higher densities than the previously installed heating systems. This makes the new heating system a good candidate in studying over-dense plasmas.Item Open Access Silicon integrated dual-mode interferometer with differential outputs(2017) Hoppe, Niklas; Scheck, Pascal; Sweidan, Rami; Diersing, Philipp; Rathgeber, Lotte; Vogel, Wolfgang; Riegger, Benjamin R.; Southan, Alexander; Berroth, ManfredThe dual-mode interferometer (DMI) is an attractive alternative to Mach-Zehnder interferometers for sensor purposes, achieving sensitivities to refractive index changes close to state-of-the-art. Modern designs on silicon-on-insulator (SOI) platforms offer thermally stable and compact devices with insertion losses of less than 1 dB and high extinction ratios. Compact arrays of multiple DMIs in parallel are easy to fabricate due to the simple structure of the DMI. In this work, the principle of operation of an integrated DMI with differential outputs is presented which allows the unambiguous phase shift detection with a single wavelength measurement, rather than using a wavelength sweep and evaluating the optical output power spectrum. Fluctuating optical input power or varying attenuation due to different analyte concentrations can be compensated by observing the sum of the optical powers at the differential outputs. DMIs with two differential single-mode outputs are fabricated in a 250 nm SOI platform, and corresponding measurements are shown to explain the principle of operation in detail. A comparison of DMIs with the conventional Mach-Zehnder interferometer using the same technology concludes this work.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.