This thesis deals with the study of parameters of diaphragm discharge in liquids. NaCl solution of different conductivity was used as a conductive medium. Conductivities were adjusted in the range from 220 to 1000 µS cm-1. Two diagnostic methods were used for the study of plasma parameters. The first one was employed in the laboratory of plasma chemistry at Faculty of Chemistry, Brno University of Technology, namely the optical emission spectroscopy. The second method used for plasma diagnostics was the time resolved ICCD camera at the Laboratoire de Physique des Plasmas at the École Polytechnique in Paris. The reactor for the diagnostics by optical emission spectroscopy had the volume of 4 l, and it was made of polycarbonate. PET diaphragm was placed in the barrier separating the cathode and the anode space. Electrodes were made of titanium coated with platinum. Electric power source supplied a constant DC voltage of maximum 5 kV and electric current up to 300 mA. Spectrometer Jobin Yvon TRIAX 550 with CCD detector was used during the experiments in order to measure overview spectra within the range from 200 to 900 nm as well as OH molecular spectra and Hß line spectra. All spectra were scanned in both discharge polarities, i.e. at the cathode and the anode part of reactor. The basic parameters of the discharge plasma were calculated from the spectra, that means rotational and electron temperature and electron density. Another part of experiment consisted of measurements by the ICCD camera iStar 734. Two types of reactors were used. The first one was the same as the reactor for the measurements by the optical emission spectroscopy. The second one was also made of polycarbonate, but the volume of conductive solution was 110 ml, only. HV electrodes made of stainless steel were placed in this reactor. Ceramic diaphragm (Shapal-MTM) was used in both reactors. Diaphragms had different thickness and diameter of holes. ICCD camera acquired photographs with details of processes of the bubbles generation and discharge operation (propagation of plasma channels), depending on solution conductivity, dimensions of the diaphragm, and with respect to the electrode part of the reactor.

Clean post-discharge nitrogen plasma and nitrogen plasma with different traces have been focus of scientists for more than 50 years and there were published many articles on theme active discharge, post-discharge, processes and reactions. It is possible to create kinetic models from all these information and then calculate concentrations of elements in atomic form. This diploma thesis is focused on measuring of concentration of atomic nitrogen for different conditions (decay time, pressure, admixture). The titration method by nitric oxide in post-discharge was used to determinate of concentration of atomic nitrogen. All experimental results were obtained by the optical emission spectroscopy. Optical emission spectra were taken in the range of 300-600 nm. DC discharge was created in a quartz tube in a flowing regime. The flowing regime was chosen for this experiment because of better time resolution of decay time, order in milliseconds. Decay time was in the range of 16 – 82 ms for individual experiments. Nitrogen flow was 400 mln/min. Nitrogen oxide flow was in the range of 0-10 mln/min and it was added at the selected post-discharge time. Trace of methane was 0,006 % of the whole volume. Total gas pressure was set on values from 500 to 4000 Pa. The output of discharge was set on constant value of current 150 mA and the output has changed according to the amount of pressure. Nitrogen first positive, second positive and first negative spectral systems, NO spectral system and NO2* spectral system were recognized in all measured spectra. Absolute concentration of atomic nitrogen was specified by the method of titration of NO. Traces of methane increase dissociation of molecular nitrogen and therefore increase the concentration of atomic nitrogen. This thesis brings new results into longtime research of moon Titan and new results into study of processes in nitrogen-methane plasma.

Presented thesis gives results obtained during the spectroscopic observations of post –discharges of the pure nitrogen plasma with small oxygen admixture and in the nitrogen – argon mixture and the effect of the pink afterglow in it. The DC discharge in the flowing regime has been used for the plasma generation. The decaying plasma was study by optical emission spectroscopy, mainly in the range of 300–800 nm. The first positive, second positive, first negative nitrogen spectral system and NO spectral systems were observed in measured spectra. The band head intensities of these bands have been studied in the dependencies on experimental conditions. Simultaneously, the relative vibrational populations on the given nitrogen states have been calculated. Two discharge tubes made from different materials (PYREX glass and QUARTZ glass) were used in the case of nitrogen plasma containing low oxygen traces (up to 0.2 %). These experiments have been carried out at two wall temperatures for the determination of the temperature effect on the post-discharge. The discharge tube around the observation point was kept at the ambient temperature (300 K) or it was cooled down to 77 K by liquid nitrogen vapor. The total gas pressure of 1 000 Pa and the discharge current of 200 mA were conserved for all these experiments. The relative populations of electronic states were calculated in the dependence on the post-discharge time. The dependencies on oxygen concentration were given, too. The results showed no simple dependence of vibrational populations on oxygen concentration. Generally, slight increase of neutral nitrogen states populations was observed with the increase of oxygen concentration. These observations were well visible due to the intensity of nitrogen pink afterglow effect that was well visible at all oxygen concentrations. The pink afterglow maximal intensity was reached at about 5–10 ms at the wall temperature of 300 K in the PYREX tube. The molecular ion emission was strongly quenched by the oxygen and as this was dominant process for the pink afterglow emission the pink afterglow effect disappears at oxygen concentration of about 2000 ppm. The temperature and wall material influences were observed, too. The post-discharge in nitrogen argon mixtures was studied only in the PYREX tube at the ambient wall temperature of 300 K. The power dissipated in an active discharge was constant of 290 kW. The experimental studies had two new parameters – total gas pressure (500 Pa – 5 000 Pa) and the argon concentrations that were varied in the range of 0–83 %. Also in this case the dependencies of relative intensities of the bands given above were obtained and further the relative populations of electronic states as a function of decay time, total gas pressure and on argon concentration were obtained. The pink afterglow effect was observed at all applied discharge powers and total gas pressures. At the highest argon concentrations, especially at lower pressure, the pink afterglow effect disappeared. The presented experimental work is one of the hugest sets of experiments in the nitrogen with oxygen traces and in nitrogen-argon mixtures. These data can be used as a very good fundament for the further studies using wide numeric modeling of the post-discharge kinetic processes.

<p>Opisani&nbsp; su&nbsp; detalji&nbsp; konstrukcije&nbsp; novog&nbsp; izvora&nbsp; plazme, u impulsnom režimu, konstruisanog za&nbsp; potrebe ekscitacija linija berilijuma u&nbsp; prisustvu berilijumske&nbsp; pra&scaron;ine.&nbsp; Konstrukcija&nbsp; izvora&nbsp; je ostvarena&nbsp; na&nbsp; takav&nbsp; način&nbsp; da&nbsp; je&nbsp; sprečeno prodiranje&nbsp; čestica&nbsp; pra&scaron;ine&nbsp; u&nbsp; atmosferu&nbsp; laboratorije.&nbsp; Opisane&nbsp; su&nbsp; dodatne&nbsp; 2&nbsp; cevi&nbsp; za pražnjenje&nbsp; konstruisane&nbsp; od&nbsp; Al2O3 i&nbsp; SiO 2 . Pronađeni&nbsp; su&nbsp; i&nbsp; opisani&nbsp; optimalni&nbsp; uslovi&nbsp; za&nbsp; rad<br />izvora&nbsp; plazme.&nbsp; Vrednosti&nbsp; elektronske&nbsp; koncentracije,&nbsp; određene&nbsp; nakon&nbsp; maksimuma<br />struje,&nbsp; kori&scaron;ćenjem&nbsp; vodonikove&nbsp; balmer&nbsp; beta linije,&nbsp; kreću&nbsp; se&nbsp; u&nbsp; opsegu&nbsp; 1,16-9,2&nbsp; ∙10<br />22&nbsp; m -3 . Elektronska temperatura je određena&nbsp; na&nbsp; osnovu relativnih&nbsp; intenziteta&nbsp; linija&nbsp; dva&nbsp; uzastopna jonizaciona&nbsp; stanja&nbsp; istog&nbsp; elementa&nbsp; i&nbsp; kreće&nbsp; se&nbsp; u opsegu&nbsp; 10&nbsp; 500-15&nbsp; 500&nbsp; K.&nbsp; Prikazane&nbsp; su snimljene&nbsp; linije&nbsp; berilijuma,&nbsp; osim&nbsp; rezonantnih. Dato&nbsp; je&nbsp; poređenje&nbsp; snimljenih&nbsp; linija&nbsp; sa postojećim&nbsp; teorisjkim&nbsp; podacima.&nbsp; Dve&nbsp; linije berilijuma&nbsp; koje&nbsp; se&nbsp; pojavljuju&nbsp; sa&nbsp; zabranjenom komponentom su prikazane prvi put. Pokazano je&nbsp; da&nbsp; postoji&nbsp; tipičan&nbsp; trend&nbsp; zavisnosti&nbsp; odnosa dozvoljene&nbsp; i&nbsp; zabranjene&nbsp; komponente,&nbsp; kao&nbsp; i rastojanja&nbsp; između&nbsp; položaja&nbsp; maksimuma intenziteta ove dve komponente, od elektronske koncentracije,&nbsp; koji&nbsp; se&nbsp; javlja&nbsp; kod&nbsp; linija&nbsp; sa zabranjenim&nbsp; komponentama,&nbsp;&nbsp;&nbsp; &scaron;to&nbsp; govori&nbsp; o<br />mogućnosti ove linije za primenu u dijagnostici plazme.</p> / <p>Construction&nbsp; details&nbsp; of&nbsp; new&nbsp; plasma&nbsp; source,&nbsp; running in pulsed regime,&nbsp; for beryllium spectral line&nbsp; studies,&nbsp; in&nbsp; the&nbsp; presence&nbsp; of&nbsp; beryllium&nbsp; dust particles are presented.&nbsp; The construction of the source&nbsp; was&nbsp; realised&nbsp; in&nbsp; such&nbsp; a&nbsp; way&nbsp; that&nbsp; it prevented&nbsp; the&nbsp; ingress&nbsp; of&nbsp; dust&nbsp; particles&nbsp; into&nbsp; the laboratory&nbsp; atmospher.&nbsp; Construction&nbsp; details&nbsp; and<br />testing&nbsp; of&nbsp; BeO&nbsp; discharge&nbsp; tube&nbsp; in&nbsp; comparison with&nbsp; SiO2 and&nbsp; Al2O3 discharge&nbsp; tubes&nbsp; are&nbsp; presented,&nbsp; also.&nbsp; Optimal&nbsp; conditions&nbsp; for&nbsp; plasma source operation&nbsp; and beryllium line studies are found.&nbsp; The&nbsp; electron&nbsp; density&nbsp; measured&nbsp; after discharge current maximum is determined from&nbsp; the peak separation of the hydrogen Balmer beta<br />spectral&nbsp; line,&nbsp; and&nbsp; the&nbsp; electron&nbsp; temperature&nbsp; is&nbsp; determined&nbsp; from&nbsp; the&nbsp; ratios&nbsp; of&nbsp; the&nbsp; relative&nbsp; intensities&nbsp; of&nbsp; Be&nbsp; spectral&nbsp; lines&nbsp; emitted&nbsp; from successive&nbsp; ionized&nbsp; stages&nbsp; of&nbsp; atoms.&nbsp; Maximum values&nbsp; of&nbsp; electron&nbsp; density&nbsp; and&nbsp; temperature&nbsp; are measured&nbsp; to&nbsp; be&nbsp; 9.3∙1022 m -3 and&nbsp; 16&nbsp; 800&nbsp; K, respectively.&nbsp; The&nbsp; recorded&nbsp; spectral&nbsp; lines&nbsp; of beryllium,&nbsp; other&nbsp; then&nbsp; resonant&nbsp; lines,&nbsp; are&nbsp; presented. The lines&nbsp; with forbidden component are&nbsp; described&nbsp; for&nbsp; the&nbsp; first&nbsp; time.&nbsp; The&nbsp; functional dependence of the wavelength separation range and&nbsp; peak&nbsp; intensity&nbsp; ratio&nbsp; of&nbsp; these&nbsp; lines&nbsp; upon<br />electron&nbsp; number&nbsp; density&nbsp; suggests&nbsp; the&nbsp; complex profile of the forbidden and allowed line, which can be used for diagnostics of low-temperature beryllium containing plasmas.</p>

Under high irradiation, a fourth state of matter named plasma can be obtained. Plasmas emit electromagnetic radiation that can be recorded in the form of spectra for spectroscopic elemental analysis. With the advent of lasers in the 1960s, spectroscopists realized that lasers could be used simultaneously as a source of energy and excitation to create plasmas. The use of a laser to ignite a plasma subsequently led to laser-induced breakdown spectroscopy (LIBS), an optical emission spectroscopy capable of analyzing samples in various states (solids, liquids, gases) with minimal sample preparation, rapid feedback, and endowed with in situ capability. In this dissertation, studies of LIBS for multi-elemental analysis and geological applications are reported. LIBS was applied to cosmetic powders for elemental analysis, screening and classification based on the raw material used. Principal component analysis (PCA) and internal standardization were used. The intensity ratios of Mg/Si and Fe/Si observed in talcum powder show that these two ratios could be used as indicators of the potential presence of asbestos. The feasibility of LIBS for the analysis of gasification slags was investigated and results compared with those of inductively-coupled plasma−optical emission spectrometry (ICP-OES). The limits of detection for Al, Ca, Fe, Si and V were determined. The matrix effect was studied using an internal standard and PLS-R. Apart from V, prediction results were closed to those of ICP-OES with accuracy within 10%. Elemental characterization of outcrop geological samples from the Marcellus Shale Formation was also carried out. The matrix effect was substantially reduced. The limits of detection obtained for Si, Al, Ti, Mg, Ca and C were determined. The relative errors of LIBS measurements are in the range of 1.7 to 12.6%. Gate delay and laser pulse energy, have been investigated in view of quantitative analysis of variation of trace elements in a high-pressure environment. Optimization of these parameters permits obtaining underwater plasma emission of calcium with quantitative results on the order of 30 ppm within a certain limit of increased pressure. Monitoring the variation of the trace elements can predict changes in the chemical composition in carbon sequestration reservoir.

<p>As the small satellite market has grown from a niche of the space economy to a full commercial force,  microthrusters remain an area of significant growth in the space industry as new technologies mature. The \textit{Film-Evaporation Microelectricalmechanical Tunable Array} (FEMTA) is one such device. FEMTA is \textit{microelectricalmechanical system} (MEMS) device that harnesses the microcapillary action of water and vacuum boiling to generate thrust. The water propellant is not chemically altered at all by the process; it is simply evaporated. This technology has been tested in relevant laboratory environments, and a suborbital flight opportunity in 2023 as a payload on a Blue Origin New Shepard rocket  will grant FEMTA a demonstration in a space environment. The flight will provide 150 seconds of weightlessness at the zenith of the suborbital flight path before the booster returns to land. During weightlessness, the experiment will be exposed to the ambient environment allowing for a full capability test of the thruster. The experiment is meant to demonstrate the propellant management system for FEMTA in 0G and measure the thrust produced by a FEMTA thruster.</p> <p><br></p> <p>The propellant management system portion of the experiment consists of an oversized version of the subsystem intended for use in the thruster. The propellant management system uses a hydrofluoroether to inflate a diaphragm to ensure constant wetting of the propellant tank exit and nozzle inlet. The experiment will take tank pressure data and flow sensor data to understand the system's behavior. The system is duplicated for redundancy and to double the possible data. This system requires further testing before being prepared for launch, vibrational testing, thermal testing, and vacuum testing. </p> <p><br></p> <p>The 0G thrust experiment and plume analysis portion of the experiment consists of numerical modeling and a novel thrust measurement approach. \textit{Direct Simulation Monte Carlo} (DSMC) is being applied to understand the pressure, density, and temperature distributions of the plume of water vapor produced by the FEMTA thruster. The FEMTA nozzle environment is challenging to simulate with computational fluid dynamics  or DSMC due to chaotic transient effects and because both the continuum and molecular regimes must be considered. The current analysis consisted of a two-dimensional model and investigated the effect of meniscus location and contact angle on thrust generated.</p> <p><br></p> <p>It is not possible to use traditional thrust measurement devices (sensitive torsional thrust stands or microsensors intended for use on small satellites) for microthrusters on a rocket booster. Two  novel approaches for performing thrust measurement in the range of 100 microNewtons have been investigated. The first approach ionizes the FEMTA thruster plume and analyzes the plasma by optical emission spectroscopy. The theory states that the relative intensity of a given wavelength observed correlates to the density of the species in the plasma. The density of water would be directly correlated to the thrust generated by FEMTA during the experiment, as more water is evaporated as thrust is increased. This method is no longer being considered for the suborbital experiment but did yield promising results. </p> <p><br></p> <p>The second approach employs a d'Arsonval meter, a photo-interrupt, and an Arduino controller. The d'Arsonval meter consists of a stationary permanent magnet with a moving coil and a pointer. Increasing the voltage in the coil causes a torque on the system due to the magnetic field induced by the permanent magnet. This torque causes a deflection of the pointer that is proportional to the voltage applied. The flag of the sensor will be placed in the path of the gas jet from the thruster. The force caused by the jet pressure will move the flag. An Arduino controller will vary the voltage to hold the flag in place. As the mass flow rate increases, the reaction force required to hold the flag in place will increase. This sensor can be calibrated using an analog cold gas system that passes various gases (air nitrogen, argon, etc.) through an orifice nozzle at mass flow rates that are set by a mass flow rate controller. DSMC analysis has been performed to understand the flow field and flow properties and how they directly relate to the force experienced by the flag sensor. </p> <p>An undergraduate course has supported parts of the work described in this dissertation. This course has applied the Vertically Integrated Projects approach to project-based learning. This method and its results were analyzed and lessons learned as well as a blueprint for future application of this method to other small satellite projects are discussed.</p>

Es wurde eine Elektron-Zyklotron-Resonanz-Ionenquelle mit einer Mikrowellenfrequenz von2,45 GHz für die Produktion intensiver Ströme einfach geladener Metallionen entwickelt. Deren Beladung mit Metalldampf erfolgt über ein integriertes zylindrisches Sputtermagnetron, welches speziell für diese Aufgabe entworfen wurde. Die entstandene MECRIS, engl. Magnetron Electron Cyclotron Resonance Ion Source, vereinigt die ECR-Ionenquellentechnologie mit der Magnetron-Sputtertechnologie auf bisher einzigartige Weise und verkörpert so ein neues Metallionen-Quellenkonzept. Unter Verwendung eines Al-Sputtertargets konnte die Funktionsfähigkeit der MECRIS an dem Beispiel der Al+-Ionenerzeugung erfolgreich demonstriert werden. Der extrahierbare Al+-Ionenstrom wurde über einen neuartigen, im Rahmen der Arbeit entwickelten, Hochstrom-Faraday-Cup gemessen. Auf Basis numerischer Berechnungen wurde das Gesamtmagnetfeld so ausgelegt, dass die Permanentmagnete des Magnetrons und die Spulen der ECR-Quelle eine Minimum-B-Struktur erzeugen, welche einen effektiven Elektroneneinschluss nach dem magnetischen Spiegelprinzip ermöglicht. Gleichzeitig wird durch eine geschlossene ECR-Fläche, mit der magnetischen Resonanzflussdichte von 87,5 mT, eine optimale Heizung der Plasmaelektronen realisiert. Die mithilfe einer Doppel-Langmuir-Sonde gemessene Elektronentemperatur steigt in Richtung Quellenmitte an und beträgt maximal 11 eV. Geheizte Elektronen erlauben die effiziente Stoßionisation der Al-Atome, welche mit einer Rate von über 1E18 Al-Atome/s eingespeist werden und eine höchstmögliche Dichte von 2E10 1/cm³ aufweisen. Die MECRIS erzeugt hauptsächlich einfach geladene Ionen des gesputterten Materials (Al+) und des Prozessgases (Ar+). Der Al+-Ionenextraktionsstrom ist über die Erhöhung der Prozessparameter Sputterleistung, Mikrowellenleistung, Spulenstrom und Extraktionsspannung um eine Größenordnung bis auf maximal 135 μA steigerbar, was einer Stromdichte von 270 μA/cm² über die Extraktionsfläche von rund 0,5 cm² entspricht. Dies steht im Einklang mit der Prozessparameterabhängigkeit der anhand der Sonde bestimmten Plasmadichte, welche einen größtmöglichen Wert von etwa 6E11 1/cm³ annimmt. Das Verhältnis von extrahiertem Al+- zu Ar+-Ionenstrom kann durch Optimierung der Prozessparameter von 0,3 auf maximal 2 angehoben werden. Sondenmessungen des entsprechenden Ionendichteverhältnisses bestätigen diesen Sachverhalt. Um möglichst große Extraktionsströme und Al+/Ar+-Verhältnisse zu generieren, muss die ECR-Fläche demnach in dem Bereich der höchsten Al-Atomdichte in der Targetebene lokalisiert sein. Gegenüber dem alleinigen Magnetronplasma (ohne Mikrowelleneinspeisung) können mit dem MECRIS-Plasma um bis zu 140 % höhere Al+-Ionenströme produziert werden. Aus Sondenuntersuchungen geht hervor, dass dies eine Folge der um etwa eine Größenordnung gesteigerten Plasmadichte und der um rund 7 eV größeren Elektronentemperatur des MECRIS-Plasmas ist. Das MECRIS-Plasma wurde außerdem mittels optischer Emissionsspektroskopie charakterisiert und durch ein globales sowie ein zweidimensionales Modell simuliert. Die gewonnenen Prozessparameterabhängigkeiten der Plasmadichte, Elektronentemperatur sowie Al+- und Ar+-Ionendichte stimmen mit den Sondenergebnissen überein. Teilweise treten jedoch Absolutwertunterschiede von bis zu zwei Größenordnungen auf. Die Erhöhung der Sputterleistung und Extraktionsspannung über die derzeitigen Grenzen von 10 kW bzw. 30 kV sowie die Optimierung der Extraktionseinheit hinsichtlich minimaler Elektrodenblindströme bietet das Potential, den Al+-Ionenstrom bis in den mA-Bereich zu steigern. / An electron cyclotron resonance ion source working at a microwave frequency of 2.45 GHz has been developed in order to generate an intense current of singly charged metal ions. It is loaded with metal vapor by an integrated cylindrical sputter magnetron, which was especially designed for this purpose. The MECRIS (Magnetron Electron Cyclotron Resonance Ion Source) merges ECR ion source technology with sputter magnetron technology in a unique manner representing a new metal ion source concept. By using an Al sputter target, the efficiency of the MECRIS was demonstrated successfully for the example of Al+ ion production. The extractable ion current was measured by a newly developed high-current Faraday cup. On the basis of numerical modeling, the total magnetic field was set in a way that the permanent magnets of the magnetron and the coils of the ECR source are forming a minimum-B-structure, providing an effective electron trap by the magnetic mirror principle. Simultaneously, optimal electron heating is achieved by a closed ECR-surface at resonant magnetic flux density of 87.5 mT. Electron temperature increases towards the center of the source to a maximum of about 11 eV and was measured by a double Langmuir probe. Due to the heated electron population, efficient electron impact ionization of the Al atoms is accomplished. Al atoms are injected with a rate of more than 1E18 Al-atoms/s resulting in a maximum Al atom density of 2E10 1/cm³. The MECRIS produces mainly singly charged ions of the sputtered material (Al+) and the process gas (Ar+). The Al+ ion extraction current is elevated by one order of magnitude to a maximum of 135 μA by increasing the process parameters sputter magnetron power, microwave power, coil current, and acceleration voltage. Related to the extraction area of about 0.5 cm², the highest possible Al+ ion current density is 270 μA/cm². A corresponding process parameter dependency was found for the plasma density showing a peak value of about 6E11 1/cm³, which was deduced from probe measurements. The ratio of the extracted Al+ ion current to the Ar+ ion current can be enhanced from 0.3 to a maximum of 2 by optimization of the process parameters. This was confirmed by probe investigations of the appropriate ion density ratio. In conclusion, the ECR-surface needs to be located in the area of the highest Al atom density in the target plane in order to improve the extraction current and Al+/Ar+ ratio. The MECRIS plasma produces an Al+ ion current, which is up to 140 % higher compared to that of the sole sputter magnetron plasma (without microwave injection). As revealed by probe measurements, this effect is due to the higher plasma density and electron temperature of the MECRIS plasma, leading to a difference of one order of magnitude and 7 eV, respectively. Additionally, the MECRIS plasma has been characterized by optical emission spectroscopy and simulated by a global and a two-dimensional model. Retrieved process parameter dependencies of plasma density, electron temperature, Al+ ion density, and Ar+ ion density coincide with probe findings. Although a discrepancy of the absolute values of partly up to two orders of magnitude is evident. Potentially, the Al+ ion current can be enhanced to the mA-region by optimizing the ion extraction system for minimal idle electrode currents and by rising sputter magnetron power as well as acceleration voltage above the actual limits of 10 kW and 30 kV, respectively.

Μια από τις σημαντικότερες τεχνικές εγχάραξης σε μίκρο και νάνο-κλίμακα είναι αυτή της ξηρής εγχάραξης με πλάσμα. Η παρούσα εργασία είχε σαν σκοπό την κατασκευή διάταξης επεξεργασίας ψυχρού πλάσματος χαμηλής πίεσης που να λειτουργεί στο πεδίο των ραδιοσυχνοτήτων, με την προοπτική να χρησιμοποιηθεί για την επεξεργασία πολυμερών και άλλων υλικών που χρησιμοποιούνται στις μονώσεις υψηλών τάσεων ώστε να βελτιωθούν διάφορες ιδιότητές τους όπως η επιφανειακή υδροφοβία και η αντοχή στη ρύπανση. Ειδικότερα: Στο πρώτο κεφάλαιο γίνεται εισαγωγή του αναγνώστη στην επεξεργασία πλάσματος και συγκεκριμένα στην εγχάραξη και τους φυσικούς και χημικούς μηχανισμούς της. Αναλύεται η διάταξη RIE, η οποία εφαρμόζεται κατά την κατασκευή του συστήματος. Στο δεύτερο κεφάλαιο περιγράφεται ο σχεδιασμός και η κατασκευή της διάταξης επεξεργασίας, η οποία αποτελείτε από διακριτά μέρη όπως οι θάλαμοι, το πνευματικό σύστημα, το αντλητικό σύστημα και το σύστημα τροφοδοσίας της ισχύος. Δόθηκε ιδιαίτερη προσοχή στη λεπτομερή περιγραφή του κάθε εξαρτήματος που ενσωματώθηκε και ο εξειδικευμένος ρόλος του, ενώ τα αναλυτικά κατασκευαστικά σχέδια παρατίθενται στο παράρτημα. Στο τρίτο κεφάλαιο γίνεται βασικός χαρακτηρισμός του αντιδραστήρα. Δηλαδή, παρουσιάζονται οι ηλεκτρικές μετρήσεις οι οποίες ταυτίζονται με τη βιβλιογραφία, παρουσιάζονται οπτικές μετρήσεις από τις οποίες γίνεται ταυτοποίηση ενεργών σωματίων, τα οποία επίσης είναι σύμφωνα με τη βιβλιογραφία παρόμοιων συστημάτων και τέλος, γίνεται ενδεικτική επεξεργασία πολυμερούς και έλεγχος του αποτελέσματος, το οποίο είναι η πιστή απόδοση μοτίβου και ρυθμός εγχάραξης 30nm/min. Στο τέταρτο και τελευταίο κεφάλαιο προτείνονται μελλοντικές εργασίες και βελτιώσεις. / One of the most prominent etching techniques at micro and nano-scale is dry plasma etching. This work’s purpose was the fabrication of a cold plasma low pressure radio-frequency processing rig, with the prospect of being used for polymer and other materials processing, that are used in high voltage insulators, in order to improve their surface properties such as hydrophobicity and pollution resistance. In particular; In the first chapter the reader is being introduced in plasma processing and in particular in etching and physical and chemical mechanisms. RIE set-up, which is to be applied in our rig, is being analyzed. In the second chapter the design and fabrication of the processing rig are being described, which includes parts like the chambers, the pneumatic system, the pumping system and the power delivery system. Special care has been given for a detailed description of every added component and its specialized role, while their analytical mechanical designs are collocated in the appendix. In the third chapter a basic characterization of the reactor is being delivered. Namely, we present electrical measurements which correspond precisely to bibliography and we also present optical measurements from which identification of reactive species is derived, also in accordance to bibliography. Finally, a polymeric substrate is indicatively processed and the result is the faithful pattern transfer by an etching rate of 30nm/min. In the fourth and last chapter, suggestions for future work and improvements are made.

Le recours au plasma pour stériliser des dispositifs médicaux (DM) est un domaine de recherche ne datant véritablement que de la fin des années 1990. Les plasmas permettent, dans les conditions adéquates, de réaliser la stérilisation à basse température (≤ 65°C), tel qu’exigé par la présence de polymères dans les DM et ce contrairement aux procédés par chaleur, et aussi de façon non toxique, contrairement aux procédés chimiques comme, par exemple, l’oxyde d’éthylène (OEt). Les laboratoires du Groupe de physique des plasmas à l’Université de Montréal travaillent à l’élaboration d’un stérilisateur consistant plus particulièrement à employer les effluents d’une décharge N2-%O2 basse pression (2-8 Torrs) en flux, formant ce que l’on appelle une post-décharge en flux. Ce sont les atomes N et O de cette décharge qui viendront, dans les conditions appropriées, entrer en collisions dans la chambre de stérilisation pour y créer des molécules excitées NO*, engendrant ainsi l’émission d’une quantité appréciable de photons UV. Ceux-ci constituent, dans le cas présent, l’agent biocide qui va s’attaquer directement au bagage génétique du micro-organisme (bactéries, virus) que l’on souhaite inactiver. L’utilisation d’une lointaine post-décharge évite du même coup la présence des agents érosifs de la décharge, comme les ions et les métastables. L’un des problèmes de cette méthode de stérilisation est la réduction du nombre de molécules NO* créées par suite de la perte des atomes N et O, qui sont des radicaux connus pour interagir avec les surfaces, sur les parois des matériaux des DM que l’on souhaite stériliser. L’objectif principal de notre travail est de déterminer l’influence d’une telle perte en surface, dite aussi réassociation en surface, par l’introduction de matériaux comme le Téflon, l’acier inoxydable, l’aluminium et le cuivre sur le taux d’inactivation des spores bactériennes. Nous nous attendons à ce que la réassociation en surface de ces atomes occasionne ainsi une diminution de l’intensité UV et subséquemment, une réduction du taux d’inactivation. Par spectroscopie optique d’émission (SOE), nous avons déterminé les concentrations perdues de N et de O par la présence des matériaux dans le stérilisateur, ainsi que la diminution de l’émission UV en découlant. Nous avons observé que cette diminution des concentrations atomiques est d’autant plus importante que les surfaces sont catalytiques. Au cours de l’étude du phénomène de pertes sur les parois pour un mélange N2-%O2 nous avons constaté l’existence d’une compétition en surface entre les atomes N et O, dans laquelle les atomes d’oxygènes semblent dominer largement. Cela implique qu’au-delà d’un certain %O2 ajouté à la décharge N2, seuls les atomes O se réassocient en surface. Par ailleurs, l’analyse des courbes de survie bi-phasiques des micro-organismes a permis d’établir une étroite corrélation, par lien de cause à effet, entre la consommation des atomes N et O en surface et la diminution du taux d’inactivation des spores dans la première phase. En revanche, nous avons constaté que notre principal agent biocide (le rayonnement ultraviolet) est moins efficace dans la deuxième phase et, par conséquent, il n’a pas été possible d’établir un lien entre la diminution des concentrations et le taux d’inactivation de cette phase-là. / The use of plasmas to sterilize medical devices (MDs) is a research field, which really started only at the end of the 90’s. Plasmas under adequate conditions allow achieving low-temperature (≤ 65°C) sterilization, as required by MDs made from polymers, in contrast to heat-driven sterilization methods, and provide a non-toxic method, in contrast to chemical processes such as performed, for example, with ethylene oxide (EtO). The Groupe de physique des plasmas laboratories at Université de Montréal is working on the design and testing of a sterilizer, which has the peculiarity of utilizing the species outflowing from a N2-%O2 discharge at reduced pressure (2-8 Torrs), which is called a plasma flowing-afterglow. It is the N and O atoms of this discharge mixture that, under appropriate conditions, interact in the sterilization chamber to form NO* excited molecules, generating a significant level of UV photons. These are, in the present case, the actual biocidal agent which will create lethal lesions on the genetic material of the microorganisms (bacteria, viruses) that should be inactivated. Using a flowing late afterglow instead of the discharge itself enables us to avoid the presence of the erosive agents of the discharge (ions, metastable-state particles). A major problem of this sterilization method is the reduction in the concentration of NO* molecules resulting from the losses of the N and O atoms on the surfaces of the MD materials that we want to sterilize. These radicals are, in fact, well-known to interact with surfaces and recombine on them. The main aim of our work is to determine the loss level of such atoms following their surface recombination on materials such as Teflon, stainless steel, aluminum and copper and the corresponding influence of such losses on the inactivation rate of bacterial spores. We can expect that surface recombination of these atoms leads to a reduction in the UV emission intensity and, as a result, in a reduction in the inactivation rate. Using optical emission spectroscopy (OES), we have determined the loss of N and O concentrations resulting from the presence of various materials in the sterilizer chamber as well as the corresponding decrease in UV emission intensity. We have observed that this reduction in atomic concentrations increases with the catalytic properties (recombination coefficient) of these materials. While examining the surface recombination phenomenon on these various materials, we have noticed a competition between the surface recombination of N and O atoms where the latter appear to play the main role. This implies that above a certain percentage of O2 added to N2, only the O atoms do recombine on these surfaces. On the other hand, the analysis of the bi-phasic survivor curves has enable us to show a strong correlation between the consumption of N and O atoms on surfaces and the reduction in the inactivation rate coefficient in the first phase of the survivor curve. We have also observed that our main biocidal agent is less efficient in the second phase of the survivor curve and, as a result, it was not possible to make a connection between the reduction in N and O atom concentration and the inactivation rate of the second phase.

Après des décennies de développement, l'ablation laser est devenue une technique importante pour un grand nombre d'applications telles que le dépôt de couches minces, la synthèse de nanoparticules, le micro-usinage, l’analyse chimique, etc. Des études expérimentales ainsi que théoriques ont été menées pour comprendre les mécanismes physiques fondamentaux mis en jeu pendant l'ablation et pour déterminer l’effet de la longueur d'onde, de la durée d'impulsion, de la nature de gaz ambiant et du matériau de la cible. La présente thèse décrit et examine l'importance relative des mécanismes physiques qui influencent les caractéristiques des plasmas d’aluminium induits par laser. Le cadre général de cette recherche forme une étude approfondie de l'interaction entre la dynamique de la plume-plasma et l’atmosphère gazeuse dans laquelle elle se développe. Ceci a été réalisé par imagerie résolue temporellement et spatialement de la plume du plasma en termes d'intensité spectrale, de densité électronique et de température d'excitation dans différentes atmosphères de gaz inertes tel que l’Ar et l’He et réactifs tel que le N2 et ce à des pressions s’étendant de 10‾7 Torr (vide) jusqu’à 760 Torr (pression atmosphérique). Nos résultats montrent que l'intensité d'émission de plasma dépend généralement de la nature de gaz et qu’elle est fortement affectée par sa pression. En outre, pour un délai temporel donné par rapport à l'impulsion laser, la densité électronique ainsi que la température augmentent avec la pression de gaz, ce qui peut être attribué au confinement inertiel du plasma. De plus, on observe que la densité électronique est maximale à proximité de la surface de la cible où le laser est focalisé et qu’elle diminue en s’éloignant (axialement et radialement) de cette position. Malgré la variation axiale importante de la température le long du plasma, on trouve que sa variation radiale est négligeable. La densité électronique et la température ont été trouvées maximales lorsque le gaz est de l’argon et minimales pour l’hélium, tandis que les valeurs sont intermédiaires dans le cas de l’azote. Ceci tient surtout aux propriétés physiques et chimiques du gaz telles que la masse des espèces, leur énergie d'excitation et d'ionisation, la conductivité thermique et la réactivité chimique. L'expansion de la plume du plasma a été étudiée par imagerie résolue spatio-temporellement. Les résultats montrent que la nature de gaz n’affecte pas la dynamique de la plume pour des pressions inférieures à 20 Torr et pour un délai temporel inférieur à 200 ns. Cependant, pour des pressions supérieures à 20 Torr, l'effet de la nature du gaz devient important et la plume la plus courte est obtenue lorsque la masse des espèces du gaz est élevée et lorsque sa conductivité thermique est relativement faible. Ces résultats sont confirmés par la mesure de temps de vol de l’ion Al+ émettant à 281,6 nm. D’autre part, on trouve que la vitesse de propagation des ions d’aluminium est bien définie juste après l’ablation et près de la surface de la cible. Toutefois, pour un délai temporel important, les ions, en traversant la plume, se thermalisent grâce aux collisions avec les espèces du plasma et du gaz. / After decades of development, laser ablation has become an important technique for a large number of applications such as thin film deposition, nanoparticle synthesis, micromachining, chemical analysis, etc. Experimental and theoretical studies have been conducted to understand the physical mechanisms of the laser ablation processes and their dependence on the laser wavelength, pulse duration, ambient gas and target material. The present dissertation describes and investigates the relative importance of the physical mechanisms influencing the characteristics of aluminum laser-induced plasmas. The general scope of this research encompasses a thorough study of the interplay between the plasma plume dynamics and the ambient gas in which they expand. This is achieved by imaging and analyzing the temporal and spatial evolution the plume in terms of spectral intensity, electron density and excitation temperature within various environments extending from vacuum (10‾7 Torr) to atmospheric pressure (760 Torr), in an inert gas like Ar and He, as well as in a chemically active gas like N2. Our results show that the plasma emission intensity generally differs with the nature of the ambient gas and it is strongly affected by its pressure. In addition, for a given time delay after the laser pulse, both electron density and plasma temperature increase with the ambient gas pressure, which is attributed to plasma confinement. Moreover, the highest electron density is observed close to the target surface, where the laser is focused and it decreases by moving away (radially and axially) from this position. In contrast with the significant axial variation of plasma temperature, there is no large variation in the radial direction. Furthermore, argon was found to produce the highest plasma density and temperature, and helium the lowest, while nitrogen yields intermediate values. This is mainly due to their physical and chemical properties such as the mass, the excitation and ionization levels, the thermal conductivity and the chemical reactivity. The expansion of the plasma plume is studied by time- and space-resolved imaging. The results show that the ambient gas does not appreciably affect plume dynamics as long as the gas pressure remains below 20 Torr and the time delay below 200 ns. However, for pressures higher than 20 Torr, the effect of the ambient gas becomes important and the shorter plasma plume length corresponds to the highest gas mass species and the lowest thermal conductivity. These results are confirmed by Time-Of-Flight (TOF) measurements of Al+ line emitted at 281.6 nm. Moreover, the velocity of aluminum ions is well defined at the earliest time and close to the target surface. However, at later times, the ions travel through the plume and become thermalized through collisions with plasma species and with surrounding ambient gas.