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    ItemOpen Access
    Influence of the ion energy on generation and properties of thin barrier layers deposited in a microwave plasma process
    (2012) Ramisch, Evelyn Christine; Stroth, Ulrich (Prof. Dr.)
    The demand for environment-friendly energy sources increases more and more, which is not only caused by the energy turnaround initialized by the Federal Government. In this context, the focus is set mainly on the development of wind power and solar energy with competitive production costs. Above all, this is a problem for solar cells, which, today, are mainly fabricated out of crystalline silicon and, therefore, are in competition with semiconductor industry. Hence, the development of solar cells based on alternative materials like e.g. copper-indium-gallium-diselenide (CIGS) is of great interest. Because of the lower layer thickness needed for this material, these solar cells can be fabricated on flexible substrates like metal foils. This possibility offers a broader spectrum of applications. For reaching low production costs, the applicability of unpolished steel foil, which exhibits scratches on the µm scale, is investigated as substrate for the solar cells in this work. The use of any metal as substrate requires a barrier layer between the substrate and the solar cells to prevent short-circuits between the separate cells of a solar module and to prevent the diffusion of undesired substrate elements into the solar cells. In this work, siliconoxide and silicon-nitride coatings are deposited as barrier layers in a microwaveplasma process in a gas mixture of HMDSO (hexamethyldisiloxane) and oxygen or monosilane and ammonia. To have the opportunity of influencing the layer growth by high-energetic ions, an additional substrate bias is applied during the deposition, which leads to a capacitive discharge superimposing the microwave one. The high-energetic ions impinging on the layer surface lead to a layer smoothing and melting, especially at positions of indentations in the substrate surface. Hence, the barrier properties of the coating are improved clearly, which was identified by insulation measurements of the deposited film. The layer growth modification is analyzed on the basis of substrates with a well-defined rough surface structure in the µm range experimentally as well as by simulations with the Monte-Carlo Code SDTrimSP-2D, which allows a detailed analysis of the local layer growth mechanisms contributing to the deposition. Additionally, the impinge of the energetic ions affects the molecular structure and composition of the coatings as well. These parameters are an important indicator for the layer material properties like adhesion, hardness and diffusion properties. The molecular composition of the deposited layers is analyzed in detail by Fourier- ransform infrared (FTIR) spectroscopy. From the layer composition and their refractive index, conclusions on the diffusion behavior of the coatings are drawn. In case of applying the substrate bias, the spectra indicate a denser and harder film in case of silicon oxide. Hence, these layers are more diffusion preventing compared to the unbiased ones. On the other hand, the silicon-nitride coatings show contrary properties: They offer more porous layers, when the substrate bias is applied, and, therefore, they assist diffusion.
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    Particle dynamics simulation and diagnostics of the PECVD processes in fluorocarbon rf discharges
    (2010) Barz, Jakob Philipp; Lunk, Achim (Prof. Dr. rer. nat. habil.)
    The present work deals with the investigation of fluorocarbon plasmas by different experimental methods and supporting numerical analysis of the plasma with an emphasis on plasma-chemical interactions. Several insights could be gained from the combined experimental and numerical approaches, especially concerning the conclusiveness of the results and previous observations from the literature. Plasma diagnostics were performed with non-invasive methods, such as UI probe measurements, microwave interferometry, laser-induced fluorescence, UV absorption measurements, and mass spectrometry. The complementary numerical simulations accounted for the electron-neutral interactions, discharge dynamics, and chemical reactions. From the excitation and ionization cross sections of argon as well as the dissociation, ionization, and attachment cross sections of trifluoromethane, the field-dependence of transport parameters were obtained. These transport parameters were used as input data for fluid-modeling of the discharge. For the plasma dynamics simulation, the Boltzmann-equation was solved numerically for transport of mass, momentum, and energy in a time-dependent two-term approach. The so-obtained electron density and the power-voltage characteristics were compared to measurements with microwave interferometry and the UI probe, respectively. An overall good agreement of the numerical and measured electron densities was obtained over a large variation range of plasma power, gas composition, and pressure. The power-voltage characteristics showed a good agreement between numerical results and data obtained right after ignition of plasma. It was further found that the measured data showed time-dependent developments from which strong deviations resulted. The time scales of changes were typically in the range of milliseconds to seconds after ignition. It was concluded that compositional changes in the gas phase were the reason. The high abundance of oligomers as well as small molecules like HF in the gas phase on one hand, and the loss of molecules by polymer deposition on the other hand affect the charge carrier mobilities and the ionic composition, such result in the changes observed. Furthermore, from this investigation, the major fragmentation processes were identified. For the investigation of the reaction-diffusion processes, investigations by laser-induced fluorescence were carried out. In order to obtain best resolution along the axial direction of the plasma reactor, the conventional crossed-beam technique was modified. Such, a resolution of up to 60 micrometers became possible. Thus, highly-resolved axial densities of two plasma abundant intermediates, fluoromethylidine and difluorocarbene, were obtained. For the analysis of the gas phase kinetics, a numerical chemical-diffusion model was set up. To complete the analysis of the plasma dynamics, the deposition of plasma polymer onto substrates was examined. The deposition rate was determined, and changes in the surface chemistry at the transition form uncovered substrates to closed films were revealed. For the identification of the deposition precursors, results from the chemical-diffusion model were adopted for the analysis. The oligomer molecules, which are produced at high results according to the simulation, were shown to correlate well with the polymer deposition rate. It was found by electron spin resonance (ESR) that chemical reactions took place within the deposited polymer films. The restructuring of the polymer by these reactions resulted in highly cross-linked films according to x-ray photoelectron spectroscopy (XPS). Further, it was found that the amount of fluorine in the polymer was lower than could be expected from the oligomers formed according to the chemical model. Such, it was suggested that ejection of fluorine containing species was taking place especially during the plasma glow, promoted by electron and ion bombardment, and radiation. Moreover, the ejection of fluorine containing species was tentatively ascribed to the production of difluorocarbene at the surface of the plasma chamber as observed by LIF. Concluding, radical and metastable fluxes from the electrodes, combined with isotropic gas phase reactions, determine the density profiles of several species from trifluoromethane plasmas. They strongly feed back the plasma chemistry, which itself feeds back the plasma particle dynamics. According to models, the deposition occurs via formation of oligomers in the gas phase, which deposit on the surface either as neutrals or ions, and become crosslinked by subsequent reactions. The origin of the particle fluxes at the electrodes is not yet identified, but indications were found for the chemical cross-linking processes being the cause.
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    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.
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    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.
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    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.
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    Experimentelle Untersuchungen zur Struktur und Dynamik von Driftwellenturbulenz in Stellaratorgeometrie
    (2012) Birkenmeier, Gregor; Stroth, Ulrich (Prof. Dr.)
    Seit über 60 Jahren versucht man in der Fusionsforschung ein Plasma mit Hilfe von Magnetfeldern einzuschliesen, so dass die erforderlichen hohen Dichten und Temperaturen für die Zündung der Kernfusion erreicht werden können. Trotz großartiger Fortschritte bewährter Einschlusskonzepte, die Energieeinschlusszeiten an der Zündschwelle der Kernfusion in Bälde erwarten lassen, wird neuartigen Magnetfeldgeometrien von Seiten der theoretischen Plasmaphysik ein enormes zusätzliches Potential an Einschlussverbesserung zugesprochen. Der Schlüssel dafür liegt in der Minimierung des turbulenten Transports durch geeignete Wahl der Magnetfeldgeometrie, wofür ein grundlegendes Verständnis des Einflusses der Magnetfeldgeometrie auf die Plasmaturbulenz essenziell ist. Neben einer stattlichen Anzahl von theoretischen Arbeiten über die turbulente Plasmadynamik in dreidimensionalen Geometrien gibt es nur wenige experimentelle Studien zur Überprüfung der theoretischen Resultate. Das Ziel der vorliegenden Arbeit ist daher, experimentelle Daten zu liefern, die für den Vergleich mit der Theorie und für tiefere Einblicke in das Wechselspiel zwischen Driftwellenturbulenz und Magnetfeldgeometrie dienen. Dafür werden mit Hilfe zweier Multi-Sondenanordnungen an 128 Stellen auf einer Flussfläche des Stellarators TJ-K in Niedertemperaturplasmen lokale Dichte- und Potentialfluktuationen mit hoher zeitlicher Auflösung gemessen. Daraus bestimmte senkrechte Strukturgrößen sind in Bereichen hoher absoluter lokaler Magnetfeldverscherung reduziert. Zudem wird ein poloidaler Versatz relativ zu den Magnetfeldlinien und ein komplexes Propagationsmuster der parallel ausgedehnten Turbulenzstrukturen gefunden. Aus den Sondendaten können auch Poloidalprofile des turbulenten Transports bestimmt werden. Die Transportmaxima werden dabei poloidal lokalisiert im Bereich negativer Normalenkrümmung (ungünstiger Krümmung) gefunden. Darüber hinaus gibt es Hinweise, dass auch die geodätische Krümmung eine Rolle für den Transport spielen könnte. Die transportverursachenden Bereiche sind parallel entlang einer Magnetfeldlinie auf der Flussfläche ausgedehnt. Die Sondenanordnungen erlauben erstmals auch globale Messungen von Zonalströmungen. Diese deuten auf ein Räuber-Beute-Schema zwischen Zonalströmung und Turbulenz hin, wobei eine signifikante Reduktion des turbulenten Transports um 30 % durch die Zonalströmungen nachgewiesen werden kann. Dabei wirkt die Zonalströmung zunächst auf die Kreuzphase ƒzwischen Dichte und elektrischem Feld, danach erst auf die Fluktuationsamplituden.
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    Investigation of microwave heating scenarios in the magnetically confined low-temperature plasma of the stellarator TJ-K
    (2010) Köhn, Alf; Stroth, Ulrich (Prof. Dr.)
    The generation and heating of plasmas by means of microwaves is a widely-used method. This is the case for high-temperature fusion plasmas as well as for low-temperature plasmas. In fusion plasmas, the absorption of the microwave is well understood: The wave couples resonantly to the cyclotron motion of electrons around the magnetic field lines. The efficiency of the heating depends strongly on the temperature of the electrons. In low-temperature plasmas, the electrons have temperatures in the range of 1-10 eV. At these temperatures, which are low compared to those in fusion plasmas, the cyclotron resonance only plays a role for the plasma breakdown. Hence, other mechanisms must be used for plasma heating. One possibility is heating by electron Bernstein waves. They must be excited by mode conversion processes in the plasma, because they cannot propagate in vacuum. Another candidate is heating at the upper-hybrid resonance. The stellarator TJ-K is a low-temperature experiment at which microwave heating can be carried out at two different frequencies: at 2.45 GHz and in the range around 8 GHz. The thesis presented here, investigates the possible heating scenarios in TJ-K. To numerically study the interaction of the microwave with the plasma, the full-wave code IPF-FDMC was developed. With this code, the efficiency of the conversion process of an electromagnetic wave into the electrostatic electron Bernstein wave could be investigated in detail for different fusion-relevant experiments in Europe. Both the experimental and the numerical results show that, in TJ-K, most of the microwave power is absorbed at the upper-hybrid resonance. To understand the high absorption coefficient, the reflecting vacuum vessel walls are of vital importance. In the present experimental configuration of TJ-K, heating by Bernstein waves does not play an important role. In the course of these investigations, a new operational regime was discovered in which it is possible to efficiently heat plasmas, albeit there is no resonance for the injected microwave in the plasma.
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    Entwicklung und spektroskopische Untersuchung eines Mikrowellen-Plasmabrenners für die Schichtabscheidung aus Pulvern
    (2012) Kopecki, Jochen; Stroth, Ulrich (Prof. Dr.)
    Nachhaltige Energiekonzepte, wie die Verwendung von regenerativen Energien, spielen in Zeiten von immer größer werdendem Energiebedarf eine entscheidende Rolle. Insbesondere im Bereich der Photovoltaik hat Deutschland seit jeher eine Vorreiterrolle eingenommen. Damit ist Deutschland der zentrale Standort für Photovoltaikforschung. In der vorliegenden Arbeit wird eine Möglichkeit zur plasmagestützten Abscheidung von amorphem Silizium aus Pulver entwickelt und untersucht, um eine kostengünstige Alternative zu den bestehenden Verfahren zu finden. Die Plasmaquelle hierfür basiert auf einem Mikrowellenresonator, welcher mit Hilfe von numerischen Simulationen mit CST Microwave Studio dimensioniert wurde und für den Betrieb bei Atmosphärendruck ausgelegt ist. Mit diesem Plasmabrenner ist es möglich ein linear ausgedehntes, freistehendes Plasma zu erzeugen, in dem Si-Partikel verdampft werden können. Die Partikel werden hierfür über einen Trägergasstrom eingeblasen und müssen während ihrer Verweilzeit im Plasma die benötigte Energie zum Verdampfen aufnehmen. Dieser Prozess wird im Detail untersucht, da sich über die Plasmalänge und den Gasfluss die maximal verwendbare Partikelgröße einstellt und für die Abscheidung von qualitativ hochwertigem amorphen Silizium der Schichtbildner vollständig gasförmig sein muss. Die Plasmaparameter T_gas, T_e und n_e, welche ebenfalls ausschlaggebend für den Beschichtungsprozess sind und in die verwendeten Verdampfungsmodelle eingehen, werden mittels optischer Emissionsspektroskopie in Abhängigkeit der Gaszusammensetzung ermittelt. Hierfür werden sowohl die relativen Intensitäten sowie die Linienprofile der Atomlinien der Balmerserie gemessen und ausgewertet. Die abgeschiedenen Schichten wurden mittels REM-, FTIR- und XPS-Analyse sowie der Photospektroskopie analysiert, wobei eine Verunreinigung der Schichten mit Sauerstoff ermittelt wurde, welche negative Auswirkungen auf die Leitfähigkeit der Schicht hat. Dennoch ist die Morphologie sowie die optische Qualtität der Schichten vergleichbar mit den Ergebnissen gängiger PECVD-Verfahren.
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    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.
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    Ion-acoustic solitons : analytical, experimental and numerical studies
    (2011) Aziz, Farah; Stroth, Ulrich (Prof. Dr. rer. nat.)
    Plasma is a nonlinear and dispersive medium that supports the propagation of several types of electrostatic and electromagnetic waves. Ion-acoustic waves are very simple kind of waves that take the form of solitary waves, if the effects of nonlinearity and dispersion are balanced with each other in the plasma. A solitary wave is called a soliton if it retains its shape during propagation and after collision with another solitary wave. In the present thesis, the research work is mainly focused on the theoretical, experimental and numerical analyses of ion-acoustic solitons. The analytical part deals with the soliton propagation, reflection and transmission in an inhomogeneous plasma having electrons being trapped in the soliton potential. The experimental and simulation parts emphasize on the soliton evolution mechanisms and their propagation in a Double-Plasma (DP) device. One-dimensional propagation of the solitons is analyzed under the effects of ion temperature, density inhomogeneity and temperature and concentration of trapped electrons. Here, the usual KdV equation is found to be modified by variable coefficients and an additional term appearing due to the density gradient present in the plasma. This modified KdV (mKdV) equation is solved by using a novel technique, called sine-cosine method. The linear and nonlinear analyses lead us to infer that the soliton propagation characteristics are significantly modified in the presence of even a small population electrons trapped by the wave potential and hence interact strongly with the wave during its propagation. Apart from the one dimensional propagation of mKdV solitons, oblique reflection of the solitons from a density gradient is investigated in the plasma. In relation to the transmission and reflection of the solitons from a semi-transparent grid, conditions are obtained for the obliqueness of the propagation and maximum drift velocity of ions. Also, a transmission-reflection conservation law is derived, based on which the mechanism of soliton reflection and transmission is explored in detail. The contribution of trapped electrons to the solitons’ propagation, reflection and transmission is examined through energy, amplitude and width of the solitons, in addition to the effects of temperature and drift of the ions. As mentioned, the experimental and simulation studies are conducted in a DP device. This device consists of two plasma regions, the source chamber and a target chamber, both housed in a common vacuum chamber. Here, the excitation of linear and nonlinear ion-acoustic waves is carried out by applying bursts of sinusoidal signals on the grid that separates the source and the target chambers. The soliton generation mechanism in the target chamber is explored by carrying out diagnostic measurements using a Langmuir probe. It is observed that the soliton profiles are accompanied by a burst of fast ions and a depression of ions, when electron temperature Te remains much larger than the ion temperature Ti, i.e. Te >> Ti. Soliton profiles are investigated for different peak-to-peak amplitudes, durations and frequencies of the applied grid signal. Particle-In-Cell (PIC) simulations are carried out in order to study in detail the evolution and propagation mechanism of the solitons. The simulation results show similar features as observed in the experiment for Te/Ti > 10. A detailed insight into the soliton evolution mechanism is obtained based on the ion phase- space distributions obtained from the simulations. Also, the effect of the amplitude, duration and frequency of the excitation signal on the soliton evolution is simulated. The simulated soliton is found to behave in a consistent manner under the effect of the parameters and it acquires a saturation in its amplitude after undergoing an initial enhancement. However, the simulations with Te/Ti < 10 having higher concentrations of resonant ions show strong interaction of the waves with the ions, producing another soliton through energy exchange mechanism. Finally, the generation mechanism of this second soliton is discussed based on the simulation studies.