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<p dir="ltr">This dissertation reports experiments and simulations of micro-/nanoscale electrical breakdown, connects them to the microscale breakdown theories, relates them to field emission and space-charge-limited conditions, and demonstrates the modification of the approach to microwave fields. It provides the first comprehensive experimental assessment of the transitions between electron emission and gas breakdown mechanisms at microscale and nanoscale and extension of semi-empirical laws for ionization process in DC and microwave. These findings will be valuable in developing theories to predict electron emission and gas breakdown mechanisms, which provides guidance for nanoscale device design.</p>

Σκοπός της παρούσας διπλωματικής εργασίας είναι η πειραματική μελέτη των κυμάτων ιονισμού που παράγονται από ηλεκτρικές εκκενώσεις σε ανομοιογενές ηλεκτρικό πεδίο. Συγκεκριμένα, εξετάζουμε τη δημιουργία και διάδοση των streamer στις ηλεκτρικές εκκενώσεις του αζώτου και του ατμοσφαιρικού αέρα. Οι παράμετροι που καθορίζουν την εξέλιξη της εκκένωσης είναι η κατανομή του πεδίου, η πίεση και η φύση του αερίου το οποίο μελετάμε. Στο κεφάλαιο 1 γίνεται μια εισαγωγή στους φυσικούς μηχανισμούς των ηλεκτρικών εκκενώσεων καθώς και στις χαρακτηριστικές V-I αυτών και θα παρουσιαστούν συνοπτικά τα «φωτεινά-οπτικά» χαρακτηριστικά τους. Βάση για όλες τις θεωρίες που πραγματεύονται την παραγωγή πλάσματος συνιστά η θεωρία Townswed. Σύμφωνα με αυτή, τα αέρια κατά την εφαρμογή μιας κρίσιμης τιμής τάσης παύουν να είναι μονωτές, υφίστανται ηλεκτρική διάσπαση και μετατρέπονται σε αγωγούς. Προτείνεται έτσι μια πολύ καλή εξήγηση των μηχανισμών των ηλεκτρικών εκκενώσεων που αφορά όμως, μόνο τα ομογενή πεδία. Η πλήρης ερμηνεία τους επιτυγχάνεται με τη θεωρία των κυμάτων ιονισμού (streamer) που λαμβάνει υπόψην τα μη αμελητέα φορτία χώρου στα οποία εξάλλου και αποδίδει τη μεγάλη ταχύτητα διάδοσης του φαινομένου. Συμπληρωματικά, παρουσιάζεται συνοπτικά η εκκένωση αίγλης που συνιστά κατηγορία φαινομένων που αναπτύσσονται όταν το ρεύμα που διαρρέει το διάκενο γίνεται σημαντικό (Ι>10 μΑ), δηλαδή όταν το κύριο χαρακτηριστικό της εκκένωσης είναι η έντονη παραμόρφωση του ηλεκτρικού πεδίου που προκαλείται από το φορτίο χώρου που συσσωρεύεται στο διάκενο. Στο κεφάλαιο 2 περιγράφεται πλήρως το εργαστήριο, η πειραματική διάταξη που χρησιμοποιήθηκε, τα όργανα των μετρήσεων καθώς και τα αέρια που εξετάζουμε. Κατόπιν, αναφέρονται συνοπτικά τα στάδια που πειράματος καθώς οι δυσκολίες που συναντήθηκαν. Επιπλέον, διερευνάται η ευστάθεια της ηλεκτρικής εκκένωσης που εξαρτάται κυρίως από την επιλογή της αντίστασης φορτίου . Στο κεφάλαιο 3, παρουσιάζονται τα πειραματικά αποτελέσματα για τις ηλεκτρικές εκκενώσεις του αζώτου και του ατμοσφαιρικού αέρα για πιέσεις 1-100mbar. Μελετάται η συμπεριφορά των εκκενώσεων για μεταβολές του διακένου, της ανόδου και της καθόδου όπως αυτά αναδεικνύονται από τις χαρακτηριστικές καμπύλες V-I αλλά και τα αντίστοιχα παλμογραφήματα. Συμπληρωματικά, σχολιάζονται τα ηλεκτρικά και τα οπτικά χαρακτηριστικά τους και επιχειρείται σύγκριση μεταξύ των δύο αερίων. Καθοριστική για την εξέλιξη της εκκένωσης επιβεβαιώνεται ότι είναι η φύση, εν προκειμένω η ηλεκτραρνητικότητα ή μη, του κάθε αερίου καθώς και το υλικό της καθόδου και η πίεση, φυσικά. Στο κεφάλαιο 4 γίνεται μια ανακεφαλαίωση των παρατηρήσεων που προέκυψαν από το πείραμα και παρουσιάζονται κάποιες σκέψεις. Γίνεται προσπάθεια να αντιστοιχεί κάθε μια περιοχή της εκκένωσης στην αντίστοιχη που προβλέπεται από τη θεωρία. Στο κεφάλαιο 5, παρουσιάζεται η αρχή λειτουργίας του φωτοπολλαπλασιαστή. Τέλος, παρουσιάζεται η βιβλιογραφία. / The purpose of the present assignment is the experimental study of the streamers which are produced by electrical discharges at inhomogeneous electrical fields. Specifically, we examine the creation and spreading of the streamers at the electrical discharges of pure nitrogen and atmospheric air. The parameters which define the discharge’s evolution are the field’s allocation, the pressure and the nature of the gas. In chapter 1, an introduction to the physic mechanism of the electrical discharges and the characteristic curves V-I takes place. Their light and optical characteristics are presented, as well. The basis for all the theories that deal with plasma’s production is Townsed’s theory. According to this, gases subsisting a crucial value of voltage stop being insulators, incur an electrical disruption and become conductors. Thus, a very nice explanation of the mechanisms of the electrical discharges is suggested but it refers only to the homogeneous fields. Full interpretation is achieved through the streamers’ theory which takes the space charges into consideration and attributes to them the great spreading’s velocity of the phenomenon. Additionally, the glow discharges are presented. Glow discharges constitute a category of phenomena which evolve when the current in the gap becomes significant. In other words, they evolve when the discharge’s main characteristic is the intense distortion of the electrical field because of the space charges. In chapter 2, the lab, the experimental set-up, the machinery used and the gases are described. Moreover, the experiment’s steps and the difficulties we met are briefly reported. Furthermore, the stability of the discharge that depends on the load resistance is examined. In chapter 3, we present the experimental results concerning the electrical discharges of nitrogen and atmospheric air for pressures 1-100 mbar. The behavior of the discharges is studied while changing the gap, the anode, the cathode and is highlighted at the curves V-I and the oscillograph. In addition, we comment on the electrical and optical characteristics of the discharges and a comparison between the two gases is attempted. The nature of the gas turns out to be significant to the evolution of the discharge (the existence of electronegativity makes a difference). The same thing happens with the cathode’s material and the pressure, too. In chapter 4, we sum up the remarks on the experiment and present some thoughts and questionings. An effort to match the discharge’s regions to the counterpart ones predicted by the theory also takes place. Finally, in chapter 5, the principles of the photomultiplier are explained. Last but not least, the bibliography that has been used is presented.

<p dir="ltr">Calculating space-charge limited current (SCLC) is a critical problem in plasma physics and intense particle beams. Accurate calculations are important for validation and verification of particle-in-cell (PIC) simulations. The theoretical assessment of SCLC is complicated by the nonlinearity of the Poisson equation when combined with the energy balance and continuity equations. This dissertation provides several theoretical tools to convert the nonlinear Poisson equation into a corresponding linear differential equation, which is then solved for numerous geometries of practical interest.</p><p dir="ltr">The first and second chapters briefly summarize the application of variational calculus (VC) to solve for one-dimensional (1D) SCLC in cylindrical and spherical diode geometries by extremizing the current in the gap. Next, conformal mapping (CM) is presented to convert the concentric cylindrical diode geometry into a planar geometry to obtain the same SCLC solution as VC. In the next chapter, SCLC is determined for several geometries with curvilinear electron flow that cannot be solved using VC because the Poisson equation cannot be written easily. We then map a hyperboloid tip onto a plane to form a non-Euclidean disk (Poincaré disk). These mappings on to Poincaré disk are utilized to solve for SCLC in tip-to-tip and tip-to-plane geometries. Lie symmetries are then introduced to solve for SCLC with nonzero monoenergetic injection velocity, recovering the solutions for concentric cylinders, concentric spheres, tip-to-plane, and tip-to-tip for zero injection velocity. We then extend the SCLC calculations to account for any geometry in multiple dimensions by using VC and vacuum capacitance. First, we derive a relationship between the space-charge limited (SCL) potential and vacuum potential that holds for any geometry. This relationship is utilized to obtain exact closed-form solutions for SCLC in two-dimensional (2D) and three-dimensional (3D) planar geometries considering emission from the full surface of the cathode. PIC simulations using VSim were performed that agreed with the SCLC in 2D diode with a maximum error of 13%. In the final chapters, we extend these multidimensional SCLC calculations to nonzero monoenergetic emission. The SCLC in any orthogonal diode in any number of dimensions is obtained by relating it to the vacuum capacitance. The current in the bifurcation regime is also derived from first-principles from vacuum capacitance. The simulations performed in VSim agreed with the theory with a maximum error of 7%.</p><p dir="ltr">These mathematical techniques form a set of powerful tools that extend prior studies by yielding exact and approximate SCLC in numerous nonplanar and multidimensional diode geometries, thereby not requiring expensive and time-consuming PIC simulations. While more experiments are required to benchmark the validity of these calculations, these results may ultimately prove useful by providing a rapid first-principles approach to determine SCLC for many geometries that can be used to assess the validity of PIC simulations and facilitate multiphysics simulations.</p>

The study presented in this thesis was motivated by the large uncertainty on the concentration of atmospheric electrical discharges to the global nitrogen budget. This uncertainty is partly due to the fact that information concerning the NOx production efficiency of electrical discharges having current signatures similar to those of lightning flashes is not available in the literature. Another reason for this uncertainty is the fact that energy is used as a figure of merit in evaluating NOx production from lightning flashes even though insufficient knowledge is available concerning the energy dissipation in lightning flashes. The third reason for this uncertainty is the lack of knowledge concerning the contribution of discharge processes other than return strokes to the NOx production in the atmosphere. Lightning is not the only process in the atmosphere that causes ionisation and dissociation of atmospheric air. Cosmic rays continuously bombard the Earth with high energetic particles and radiation causing ionization and dissociation of air leading to the production of NOx in the atmosphere. The work carried out in this thesis is an attempt to improve the current knowledge on the way in which these processes contribute to the global NOx production. Experiments have been conducted in this thesis to estimate the NOx production efficiency of streamer discharges, laser-induced plasma, laboratory sparks having current signatures similar to those of lightning flashes, alpha particle impact in air and finally with the lightning flash itself. The results obtained from laboratory electrical discharges show the following: (a) The NOx production efficiency, in terms of energy, of positive streamer discharges is more or less similar to those of hot discharges. (b) The NOx production efficiency of an electrical discharge depends not only on the energy but also on the peak and the shape of the current waveform. (c) The current signature is a better figure of merit in evaluating the NOx yield of electrical discharges. As a part of this thesis work a direct measurement of NOx generated by lightning flashes was conducted and the results show that slow discharge processes such as continuing currents could be the main source of NOx in lightning flashes. Concerning NOx production by other ionisation processes such as alpha particle impacts in the atmosphere, the data gathered in this thesis show that each ionising event in air leads to the creation of one NOx molecule. In terms of energy the NOx production efficiency of alpha particles is similar to that of electrical discharges. The theoretical studies conducted within this thesis indicate that M-components contribute more than the return strokes to the NOx production. The calculations also show that the contribution to the global NOx budget by return stroke is not as high as that assumed in the current literature.

This work presents information obtained from high-speed video and electrical monitoring of electrical breakdown (discharge) events during plasma electrolytic oxidation (PEO) of aluminium alloy substrates. Discharges were found to occur in extended sequences termed "cascades" at particular locations. This was a feature common to all the substrates and processing frequencies investigated. As the coating thickness increases, the characteristics remained broadly similar, although discharges become more energetic and longer-lived. Short PEO treatments were applied to existing PEO coatings in order to investigate the microstructural effects of discharge cascades. It was found that cascades persist at particular locations due to the residual deep pore channel left by previous discharges in the cascade. Observations were made of the way the coating was restructured around a cascade location. Samples were illuminated with very high intensity flashes during PEO processing, revealing that relatively large (1 mm diameter) bubbles form where a discharge emerges from the surface of a coating. Analysis of the overall energy consumption, as well as the energetic processes occurring within an individual discharge, indicate that the bubble growth occurs due to rapid volatilisation of water originating from the electrolyte. It is postulated that the growth of this bubble causes the electrical resistance to rise and is responsible for the termination of the discharge current. Investigations of high frequency (2,500 Hz) processing lead to the discovery of discharges occurring during the cathodic half-cycle, after a certain coating thickness had been achieved. Cathodic discharges were more energetic than anodic discharges, and created large craters in the coatings. Gas evolution was found to exceed the electrochemical Faraday yield, and was similar at low and high frequency initially. Once cathodic discharges began, the gas evolution rate increased and the coating mass gain levelled off.

O presente trabalho teve como objetivo estudar diferentes tecnologias na extração de óleo da semente de gergelim e de compostos fenólicos e proteínas da torta de gergelim. Este estudo está dividido em quatro partes. O objetivo da primeira parte do trabalho foi extrair compostos fenólicos de diferentes tortas de nozes e sementes nas mesmas condições e comparar o teor de tais compostos e a atividade antioxidante dos extratos. Nessa fase, foram utilizadas nos experimentos tortas das sementes de girassol, linhaça e gergelim, e das nozes amêndoa, pecã, macadâmia e avelã. O extrato da torta de noz pecã apresentou o maior teor de todos os compostos fenólicos analisados, seguido pelo extrato da torta de semente de girassol e de avelã. Essas amostras também apresentaram as maiores atividades antioxidantes. As etapas seguintes do trabalho focaram-se no gergelim. A segunda parte do trabalho teve como objetivo a otimização da extração, pela metodologia convencional, de fenólicos totais e lignanas da torta de gergelim. Inicialmente, um modelo polinomial de segunda ordem foi utilizado para predição dos resultados, mediante a variação da temperatura, concentração de etanol e razão, sólido/solvente. As variáveis de resposta foram as concentrações de fenólicos totais, de sesamina e de sesaminol triglicosídeo e a atividade antioxidante dos extratos obtidos. Entre os compostos analisados, o sesaminol triglicosídeo está presente em maior quantidade na torta de gergelim. A razão sólido/solvente e a concentração de etanol foram os fatores que mais afetaram a extração, enquanto a temperatura demonstrou uma influência reduzida. Na terceira etapa, o escopo da pesquisa foi a avaliação de metodologias alternativas na extração desses mesmos compostos e, também, de proteínas. As tecnologias usadas foram as de campo elétrico pulsado (CEP) e de descargas elétricas de alta tensão (DEAT). A análise da aplicação de CEP e de DEAT foi realizada usando essas tecnologias como pré-tratamentos ao processo de extração com solvente. Os resultados demonstraram que as técnicas foram eficazes e aumentaram os rendimentos do processo para fenólicos totais, lignanas e proteínas da torta. O uso de diferentes porcentagens de etanol também se mostrou significativo nessa etapa, entretanto, esse efeito foi reduzido quando utilizadas as tecnologias elétricas. Da mesma forma, o efeito da temperatura na etapa difusiva foi menor quando os pré-tratamento foram utilizados. Os comportamentos observados sugerem que a aplicação de CEP e DEAT aumenta a eficiência da extração de compostos de interesse. Por fim, na quarta parte do trabalho, objetivou-se melhorar a eficiência do processo de extração do óleo de gergelim aplicando as tecnologias previamente citadas. Esses experimentos demonstraram um efeito significativo dos tratamentos de CEP e DEAT e um aumento na quantidade de óleo extraído com o aumento da energia aplicada às sementes. O uso de DEAT gerou um aumento maior na quantidade de óleo extraído, se comparado à tecnologia de CEP. / The goal of the present work was to study different technologies in the extraction of oil from sesame seed and phenolic compounds and proteins from sesame cake. This study is divided in four parts. The first part aimed to extract water-soluble compounds from different seed and nut cakes under the same conditions and compare the phenolic content and antioxidant activity of the extracts. For the first portion of the study, seed cakes of sunflower, pumpkin, flaxseed and defatted sesame, and nut cakes of almond, pecan, macadamia and hazelnut were used in the experiments. The extract from pecan nut cake presented the highest amounts of all compounds analyzed, followed by sunflower seed and hazelnut cake extracts. These samples also had the highest antioxidant activities. The following steps of the work focused on sesame only. The second part of the work aimed to optimize the extraction of total phenolics and lignans from sesame seed cake. Initially, a second-order polynomial model was set up to predict the responses in different temperatures, solid/solvent ratios and ethanol concentrations. The response variables were the concentrations of total phenolics, sesamin, sesaminol triglucoside and antioxidant activity of the extracts. Among the analyzed compounds, ST is presented in the highest quantity in sesame cake. Solid to liquid ratio and ethanol concentration where the most important factors affecting extraction, whereas temperature showed reduced influence. In the third part of this work, the aim was to evaluate alternative methodologies in the extraction of phenolics and proteins. The technologies used were pulsed electric fields (PEF) and high voltage electric discharges (HVED). These methods were used as pre-treatments, prior to diffusion. Result show that PEF and HVED were efficient and increased the extraction yield for phenolic compounds, lignans and proteins from the cake. The use of different percentages of ethanol was also significant in this stage; however, the effect of this parameter was reduced when the electrical treatments were used. In the same way, temperature also showed a smaller influence on the results when the pre-treatments were used. The observed behaviors suggest that the use of PEF and HVED increases extraction efficiency. Finally, the goal of the last part of the work was to improve oil expression from sesame seeds, using the aforementioned technologies. These experiments show a significant effect of both PEF and HVED. It was observed an increase of the amount of oil extracted with the energy input applied to the seeds. When compared both technologies, HVED showed a more expressive effect then PEF.

<p>The study presented in this thesis was motivated by the large uncertainty on the concentration of atmospheric electrical discharges to the global nitrogen budget. This uncertainty is partly due to the fact that information concerning the <i>NO</i><i>x</i> production efficiency of electrical discharges having current signatures similar to those of lightning flashes is not available in the literature. Another reason for this uncertainty is the fact that energy is used as a figure of merit in evaluating <i>NO</i><i>x</i> production from lightning flashes even though insufficient knowledge is available concerning the energy dissipation in lightning flashes. The third reason for this uncertainty is the lack of knowledge concerning the contribution of discharge processes other than return strokes to the <i>NO</i><i>x</i> production in the atmosphere. Lightning is not the only process in the atmosphere that causes ionisation and dissociation of atmospheric air. Cosmic rays continuously bombard the Earth with high energetic particles and radiation causing ionization and dissociation of air leading to the production of <i>NO</i><i>x</i> in the atmosphere. The work carried out in this thesis is an attempt to improve the current knowledge on the way in which these processes contribute to the global <i>NO</i><i>x</i> production. Experiments have been conducted in this thesis to estimate the <i>NO</i><i>x</i> production efficiency of streamer discharges, laser-induced plasma, laboratory sparks having current signatures similar to those of lightning flashes, alpha particle impact in air and finally with the lightning flash itself. The results obtained from laboratory electrical discharges show the following: (a) The <i>NO</i><i>x</i> production efficiency, in terms of energy, of positive streamer discharges is more or less similar to those of hot discharges. (b) The <i>NO</i><i>x</i> production efficiency of an electrical discharge depends not only on the energy but also on the peak and the shape of the current waveform. (c) The current signature is a better figure of merit in evaluating the <i>NO</i><i>x</i> yield of electrical discharges. As a part of this thesis work a direct measurement of <i>NO</i><i>x</i> generated by lightning flashes was conducted and the results show that slow discharge processes such as continuing currents could be the main source of <i>NO</i><i>x</i> in lightning flashes. Concerning <i>NO</i><i>x</i> production by other ionisation processes such as alpha particle impacts in the atmosphere, the data gathered in this thesis show that each ionising event in air leads to the creation of one <i>NO</i><i>x</i> molecule. In terms of energy the <i>NO</i><i>x</i> production efficiency of alpha particles is similar to that of electrical discharges. The theoretical studies conducted within this thesis indicate that M-components contribute more than the return strokes to the <i>NO</i><i>x</i> production. The calculations also show that the contribution to the global <i>NO</i><i>x</i> budget by return stroke is not as high as that assumed in the current literature.</p>

Nanosecond Repetitively Pulsed (NRP) discharges in atmospheric pressure air have many potential applications. Spark NRP discharges have applications in plasma assisted combustion. These discharges tend to stabilize lean flames which produce less NOx. Furthermore, an increase of several hundreds of Kelvins in less than 20 ns has been observed following NRP spark discharges, which could be used to create nanomaterials. NRP glow discharges, while creating an important number of actives species such as atomic oxygen, do not heat the ambient gas, which allows them to be used in temperature-sensitive applications such as bio-decontamination. In the first part of this thesis, we validate experimentally the mechanism that was proposed to explain the ultrafast heating observed. Time-resolved measurements of the absolute densities of two excited states of nitrogen and of the gas temperature have been performed with calibrated Optical Emission Spectroscopy. The second part of the thesis deals with the NRP glow regime. We have shown that its existence depends on several parameters, gas temperature and pressure, voltage across the electrodes, inter-electrode distance, pulse duration, radius of curvature of the electrodes. This regime had not been observed for temperatures lower than 750 K so far. Thanks to a detailed parametrical experimental study and the analysis of the obtained results, we have succeeded in identifying the NRP glow regime at ambient temperature and we observe a new type of "multi-channel" glow regime.