Apresentamos neste trabalho uma técnica alternativa para a obtenção de filmes finos de silício amorfo hidrogenado (&#945-Si:H). Nós depositamos &#945-Si:H em um sistema de deposição que utiliza descarga luminescente a baixas freqüências (60Hz). Para tanto, nós projetamos todo o reator para que este objetivo pudesse ser atingido. Os filmes obtidos por nós mostram propriedades ópticas e eletrônicas bastante próximas aquelas dos filmes produzidos pela técnica convencional de descarga luminescente a radiofreqüência (13,56 MHz). A temperatura do substrato ótima para a técnica de descarga luminescente a baixas freqüências está na faixa 150-170&#176C, em torno de 100&#176C menor do que aquela usada para radiofreqüência. Neste trabalho nós apresentamos medidas das propriedades dos filmes, incluindo condutividade no escuro, fotocondutividade, comprimento de difusão ambipolar, absorção no infra-vermelho, gap óptico, e densidade de defeitos de níveis profundos. Para realizar parte destas medidas, nós construímos sistemas experimentais de caracterização exclusivos para o &#945-Si:H. / In this work we present an alternative technique for producing hydrogenated amourphous silicon thin films (&#945-Si:H). We deposited &#945-Si:H in a low-frequency (60 Hz) glow-discharge deposition system. For this purpose, we designed completely the reactor. The films we produced show electronic and optical properties nearly equivalent to those of films prepared by the conventional radio-frequency (13,56 MHz) glow-discharge technique. The optimal substrate temperature for the low-frequency glow-discharge technique is 150-170&#176C, about 100&#176C lower than that radio-frequency. In this work, we report measurements of film properties, including dark conductivity, photoconductivity, ambipolar diffusion lenght, infrared absorption, optical band gap, and deep defect density. To do these measurements, we assembled experimental systems used to characterize &#945-Si:H.

Fluidos em uma descarga brilhante à pressão atmosférica usando uma barreira de dielétrico DBD atraiu o interesse das comunidades de termo-dinâmica, fluido-dinâmica, e comunidades de controle. Este trabalho investiga os efeitos de um atuador de plasma operando numa voltagem e frequência de 8 kV e 4.4 kHz sobre a curva do Cp de um cilindro de PVC em baixa velocidade de escoamento. O experimento foi repetido com o atuador em vários ângulos no cilindro. Os resultados mostram uma aceleração do escoamento junto com um atraso da separação. Esses efeitos são maiores quando o atuador é posicionado num ângulo mais próximo da região da separação. / Fluids in a dielectric barrier DBD glow discharge at atmospheric pressure attracted the interest of the communities of thermo and fluid dynamics as well as control. This dissertation investigates the effects of a plasma actuator operating at 8 kV and 4.4 kHz, on the Cp curve of a PVC cylinder in a low velocity airflow. The experiment was repeated with the actuator at various angles. The results show an acceleration of the flow accompanied with a delay of the flow separation. These effects were shown to be larger when the actuator was positioned at an angle closer to the region of separation.

Made available in DSpace on 2017-07-21T19:26:06Z (GMT). No. of bitstreams: 1 Bruna Corina Kurelo.pdf: 9097435 bytes, checksum: 9e2ea56fd2dfc2427ab47a5b071d8244 (MD5) Previous issue date: 2013-04-30 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / Nitriding by glow discharge (DL) and a new technique called luminous glow discharge with cathodic cage (DLGC) were techniques widely employed today for surface treatment. In the present work were investigated nanoscale tribo-mechanical properties of three grades:austenitic stainless steel (AISI 316), Martensitic (AISI 420) and supermartensitic (HP13Cr) subjected to treatments by DL and DLGC techniques. Martensitic steels have been previously heat-treated in 1025 C (AISI 420) and 1100C (HP13Cr) with subsequent rapid cooling in oil. The three classes of steels have been nitrided using the following parameters of temperature – time : 350 C/6 h, 400 C/6 h e 450 C/6 h (to DL and DLGC). The nitriding treatments were held in atmospheres of N2/H2 in the proportions of 20 %-80 % (in volume) to DL and 80 %-20 % (in volume) to DLGC. For the characterization of the samples were employed the techniques of x-ray diffraction (DRX), scanning electron microscopy (SEM), optical microscopy (OM), atomic force microscopy (AFM) and Energy Dispersive X-ray Spectrometry (EDS). The mechanical properties were evaluated by instrumented indentation (II), and, with the same equipment, the nano scratch tests. In the samples treated by DL the temperature influence the formation of different stages (γN or αN, γ'-Fe4N, ε-Fe2 + xN, CrN). In the treatments carried out at low temperature (350 C) the predominant phase formed is γN to austenitic steel AISI 316 and phases γ' and ε for martensitic steels HP13Cr and AISI 420, due to difference in solubility and diffusivity of nitrogen in the austenite and martensite phases.Nitriding treatments by DL cause the effect of chromium depletion to all steels in the temperature of 450°C. To DLGC treatments occurs the formation of ε phase regardless of temperature. By this way higher temperatures favor the formation of the phases γN and αN. In treatments by DLGC, hardness of the deposited layer measured by II remained, regardless of steel, next to that of the reference sample. The hardness of the modified layers existing below the films produced by DLGC is next the hardness of the layers produced by DL but no border effect and low roughness. In treatments by DL, the hardness increased from 2,5 GPa up to 15,5 GPa for steel AISI 316. The estimated thicknesses of modified surfaces treated by DL are superior to those of the layers deposited and modified by DLGC at same parameters. The scratch resistance of modified surfaces by DL increases to any conditions of treatment. The greatest value of critical load of scratch resistance obtained (126.7 ± 32.1 mN) for the layers deposited by DLGC is too low for typical applications expected of these steels. However, further analyzes are necessary in the modified layer to check the applicability of this technique for these steels.The conditions of excellence found for DL technique can provide an increase in the useful life of the parts treated in the media, where they are employed that require good mechanical and tribological properties. / Dentre as várias técnicas empregadas na atualidade para tratamento de superfícies, destaca-se a nitretação por Descarga Luminosa (DL) e uma nova técnica denominada nitretação iônica por DL com Gaiola Catódica (DLGC). No presente trabalho investiga-se as propriedades tribo-mecânicas em nanoescala de três classes de aços inoxidáveis: austenítico (AISI 316), martensítico (AISI 420) e supermartensítico (HP13Cr) submetidos a tratamentos pelas técnicas de DL e DLGC. Os aços martensíticos foram previamente tratados termicamente em 1025 °C (AISI 420) e 1100 °C (HP13Cr) com posterior resfriamento rápido em óleo. Os três aços foram nitretados nas seguintes condições de temperatura/tempo: 350 °C/6 h, 400 °C/6 h e 450 °C/6 h (DL e DLGC). As nitretações foram realizadas em atmosferas de N2/H2 nas proporções de 20 %-80 % para DL e 80 %-20 % para DLGC. As superfícies foram caracterizadas pelas técnicas de difração de raios X (DRX), microscopia eletrônica de varredura (MEV), microscopia de força atômica (MFA) e espectroscopia de raios X por energia dispersiva (EDS). As propriedades mecânicas foram avaliadas por indentação instrumentada (II), e, com o mesmo equipamento, realizaram-se os ensaios de nanorisco. Na técnica de DL ocorre influência da temperatura de tratamento na formação das diferentes fases (γN ou αN, γ’-Fe4N, ε- Fe2+xN, CrN); nos tratamentos realizados a baixa temperatura (350 °C) predomina a formação da fase γN para o aço austenítico AISI 316 e das fases γ’ e ε para os aços HP13Cr e AISI 420, de estrutura martensítica, devido a diferença de solubilidade e difusividade de nitrogênio nas diferentes fases austenita e martensita. Os tratamentos de nitretação por DL causam o efeito da depleção do cromo em quaisquer dos aços na temperatura de 450 C. Nos tratamentos por DLGC ocorre a formação da fase independentemente da temperatura. Entretanto temperaturas mais altas propiciam a formação das fases γN e αN. Nos tratamentos por DLGC, a dureza da camada depositada medida por II permaneceu, independentemente do aço, próxima à da amostra de eeferência. A dureza das camadas modificadas existentes abaixo dos filmes produzidos por DLGC é próxima a dureza das camadas produzidas por DL mas sem efeito de borda e com baixa rugosidade. Nos tratamentos por DL, a dureza elevou-se de 2,5 GPa a até 15,5 GPa para o aço AISI 316. As espessuras estimadas para as camadas modificadas de amostras tratadas por DL são superiores às das camadas depositadas e modificadas de amostras tratadas por DLGC nos mesmos parâmetros. A resistência ao risco das superfícies modificadas por DL aumenta para quaisquer condições de tratamento. O maior valor de carga crítica de resistência ao risco (126,7 ± 32,1 mN) obtido para as camadas depositadas por DLGC é um valor muito baixo para as aplicações típicas esperadas desses aços. No entanto, são necessárias análises complementares na camada modificada para verificar a aplicabilidade dessa técnica para estes aços. As condições de excelência encontradas para a técnica de DL podem proporcionar um aumento da vida útil das peças tratadas nos meios onde são empregadas que exigem boas propriedades mecânicas e tribológicas.

The properties of materials, especially of solids, can be attributed mainly to the phenomena occurring at the surface. Surface engineering deals with altering the surface properties of materials to realize useful functionalities like wear and corrosion resistance, biocompatibility, hardening etc. Among the various methods adopted, plasma surface modification stands out, because of the inherent dry processing nature and little amount of left over chemicals. In conventional plasma systems, the process is carried out in a low pressure environment. This restricts its use in treating vacuum incompatible materials including tissues and bio-medical samples. Moreover, the batch processing nature and use of expensive vacuum pumps put a bottle-neck in the throughput of any production line. The subject matter of this thesis is about developing and optimizing an atmospheric pressure (760 torr) plasma system and to use it for surface modification of polymers. The experimental system developed, consists of two parallel electrodes facing each other, each of which is covered with a dielectric plate. A gap of 4mm exists between the dielectric surfaces, through which an axial flow of the working gas is maintained. When a high voltage is applied across the electrodes, the gas breaks down, creating plasma. The surface of the sample kept in this plasma, undergoes various phenomena, depending on the power applied, type of gas used and gas flow rate. To drive the plasma a high voltage power supply, which is able to generate 10 kV at 5.8 kHz, was developed in the laboratory. By varying the process parameters, the inherent filamentary nature of discharge can be converted to a diffuse uniform glow. The purity of plasma was studied and established by analyzing the optical emission from the plasma. After optimizing the system, it was used to modify the surface properties of polyester sheets. The wetting nature was altered using fluorocarbon and oxygen plasmas, realizing hydrophobic and hydrophilic surfaces. The contact angle of a water droplet made with the surface changed from 72° to 84° degree for hydrophobic and to 22° for hydrophilic surfaces respectively. Through this investigation, an insight to the procedure for developing an Atmospheric glow discharge system was developed. The details about system frame work, the power supply, electrical and optical characterization of the plasma, are well studied and recorded. The work establishes the various parameters to be varied to convert the filamentary discharge to a uniform glow. Purity of the plasma has been studied extensively and the system design and process values essential for maintaining the purity have been dealt with. Finally the plasma was put in use for surface modification of polymers, and the surface wetting nature alteration was studied and quantified.

Die vorliegende Arbeit hat zum Ziel, ausgehend vom aktuellen Stand der Technik, die Möglichkeiten der optische Glimmentladungsspektroskopie (GD-OES) für Tiefenprofilanalysen dünner und dünnster Schichten (Schichtdicken = 1 bis 100 nm) zu bestimmen und geeignete instrumentelle und methodischen Modifikationen vorzuschlagen, um die Einsatzmöglichkeiten weiter auszubauen. Dies gilt gleichermaßen unter Berücksichtigung der Anforderungen des Einsatzes im Routinebetrieb (geringe Bruttoanalysezeit und Reproduzierbarkeit) sowie in der Erforschung und der Entwicklung dünner Schichten (geringe Nachweisgrenzen, hohe Flexibilität zum Beispiel bei den analysierbaren Elementen oder der Leitfähigkeit der Proben, geringe Matrixeffekte, etc.). Während jeder GD-OES Analyse finden drei räumlich und zeitlich getrennte Teilprozesse statt: (A) durch das Zerstäuben der Oberfläche wird die Probe in der lateralen Ausdehnung des Anodendurchmessers in die Tiefe abgetragen und in die atomaren Bestandteile zerlegt (Sputterprozess); (B) in das Plasmagebiet diffundierte Partikel reagieren mit dem Analysegas (i. d. R. Argon), dadurch werden die Atome (und Ionen) der Probe in angeregte Zustände versetzt, im nachfolgenden Relaxationsschritt emittieren diese unter anderem Photonen einer charakteristischen Wellenlänge, die (C) alle in einem Detektionssystem (Mono- bzw. Polychromator oder CCD-Spektrometer) in ihrer Intensität als Funktion der spektralen Wellenlänge und der Zeit erfasst werden. Ein Vorteil der Methode, die niedrige Analysendauer bedingt durch den vergleichsweise hohen Sputterabtrag bewirkt, dass die Analyse dünner Schichten innerhalb weniger – im Extremfall sogar nur innerhalb von Bruchteilen von – Sekunden stattfindet. Dies lässt die Herausforderungen für die Analyse dünner Schichten verstehen. Der unter anderem von den elektrischen Entladungsbedingungen abhängige Sputterprozess und die komplexen Reaktionen im Plasma müssen möglichst unmittelbar (< 50 ms) nach dem Zündvorgang in einen stabilen Zustand übergehen. Einerseits ist dies instrumentell durch eine Anpassung der Steuer- und Regelungstechnik (z. B. Wahl geeigneter Druckregelventile, -sensoren, etc.) gelungen. Andererseits beeinflussen die unvermeidlichen Kontaminationen [Wasser(filme) und Kohlenwasserstoffe], die in das Plasmagebiet diffundieren, negativ die Stabilität die Entladung. Die Hauptstrategie zur Unterdrückung dieser ‚Dreckeffekte’ sind erfolgreich verschiedene Wege der ex-situ (maximalmögliche Reduzierung der Leckrate, Einsatz von Hochvakuumbauteilen, Einführung von Richtlinien zur Vakuumhygiene) und in-situ Dekontamination (aktive Desorptionsminderung durch ein Vorsputtern mit Si) gewählt worden. Erst in der Summe aller apparativen Verbesserungen ist die Voraussetzung für die Verwendung der Glimmentladungsspektroskopie als zuverlässige Methode der Dünnschichtanalytik gegeben. Für die laborpraktischen Arbeiten wurde während der sukzessiven Optimierung des Vakuumsystems als Nebenergebnis ein anwenderfreundlicher Schnelltest zur Charakterisierung des Geräts für Kurz- und Langzeitvergleiche entwickelt. Dieser wertet die Abpumpkurven bzw. Druckanstiegskurven aus. In Abhängigkeit der Bedürfnisse und dem Aufwand des Anwenders lassen sich interessante Parameter, wie das effektive Saugvermögen, eine Zeitkonstante für die Gasabgabe oder die Leckrate IL bestimmen. Die Bandbreite der untersuchten Proben ist dabei ähnlich unterschiedlich, wie die Fragestellungen: leitfähige und nichtleitfähige Proben; Nachweis und Bestimmung von Matrixelementen, Legierungsbestandteilen oder Spuren; Einfach-, Mehrlagen- und Wechselschichten, Oberflächen- und Zwischenschichten; Adsorbate an Ober- und Grenzflächen, Schichtdickenhomogenität als Teil der Qualitätskontrolle, etc. Ein Teil dieser Schichtsysteme sind in dieser Arbeit ausführlicher diskutiert worden. Das Hartstoffschichtsystem TiN gehört mit den Schichtdicken von 0,5 bis 3 µm zwar eher zu den dicken Schichten, wobei besonders der oberflächennahe Bereich (< 100 nm) zuverlässig untersucht wurde (vgl. Kap. 4.1). Mit dem Nachweis und der Quantifizierung von in der Grenzfläche (100 bzw. 1000 nm unter der Oberfläche) zwischen den elektrochemisch (ECD-Cu) und physikalisch (PVD-Cu) abgeschiedenen Cu-Schichten versteckten Adsorbaten bietet GD-OES dem Schichthersteller oder dem Werkstoffwissenschaftler wichtige Informationen, um zum Beispiel gezielt Gefügeänderungen für die Erhöhung der Elektromigrationsresistenz einzustellen. Es wurde einerseits die prinzipielle Machbarkeit und andererseits auch die Grenzen der Methode im Vergleich mit TOF-SIMS gezeigt. Ein weiteres Schichtsystem aus der Mikroelektronik ist im anschließenden Kap. 4.3 Gegenstand der GD-OES Untersuchungen. Dabei wurde nicht nur die Schichtdicken von 10 bis 50 nm dünnen TaN-Barriereschichten, sondern auch die Homogenität der Schichtdicken über einen kompletten 6’’ Wafer bestimmt. Die nachzuweisenden Unterschiede liegen im Bereich von einigen Angström bis zu wenigen Nanometern. Die GD-OES Untersuchungen von TaN zeigen zu Beginn und in der Nähe der Grenzfläche zum Substrat ungewöhnliche Intensitätsverläufe von Ta und N. Erst in Kombination mit anderen oberflächenanalytischen Verfahren (XPS und AES) gelang die Interpretation der Messergebnisse. Aus der Summe aller Argumente wird die Hypothese formuliert, dass sich im Fall des Zerstäubungsprozesses von TaN wegen der großen Unterschiede in den Atommassen ein Vorzugssputtern (engl. preferential sputtering) herausbildet. Bei anderen sputternden Verfahren, z. B. SIMS, ist dieses Phänomen längst bekannt und wurde auch für die Glimmentladungsspektroskopie vermutet. Dies konnte bislang allerdings noch nie beobachtet werden. Rechnungen mit einem Simulationsprogramm für Kollisionsvorgänge aufgrund ballistischer Effekte (TRIDYN) stützen diese Hypothese. Begünstigt wurde die Beobachtung des Vorzugssputterns durch die sauberen Messbedingungen, durch die man in Lage versetzt war, Anfangspeaks klar von Kontaminationspeak zu unterscheiden. Das vorletzte Kapitel 4.4 beschäftigt sich mit Schichten im untersten Nanometerbereich (< 5 nm). Es zeigt sich, dass die wenige Nanometer dicken, natürlichen Oxidschichten deutlich besser analysierbar sind, wenn man die in der Arbeit vorgestellte in-situ Dekontamination durch ein Vorsputtern anwendet. Die GD-OES Untersuchungen an organischen Monolagenschichten in Kap. 4.5 sind Teil einer aktuellen wissenschaftlichen Diskussion innerhalb der weltweiten GD-OES Fachwelt. Die von KENICHI SHIMIZU vorgestellten Ergebnisse konnten am Beispiel von Thioharnstoff mit RF bestätigt und erstmals auch mit einer DC-Entladung gezeigt werden. Das Verfahren der GD-OES kann qualitativ die Existenz von monomolekularen Schichten im Subnanometerbereich nachweisen. Allerdings stellen die Ergebnisse von Substraten mit anderen Molekülen die Interpretation der Intensitäts-Zeitprofile in Frage. Ein anderer Interpretationsansatz wird als Hypothese formuliert, konnte jedoch noch nicht verifiziert werden. Mit den vorgestellten Optimierungen der Messtechnik lassen sich die Möglichkeiten der Anwendung der optischen Glimmentladungsspektroskopie für die Untersuchungen dünner und dünnster Schichten deutlich erweitern.

The aim of this study was to define and examin the capabilities of the low voltage transmission electron microscope LVEM 5 in the detection and identification of viruses, taking into consideration various contrasting agents, and a comparison to data from HV TEM.

Apresentamos neste trabalho uma técnica alternativa para a obtenção de filmes finos de silício amorfo hidrogenado (&#945-Si:H). Nós depositamos &#945-Si:H em um sistema de deposição que utiliza descarga luminescente a baixas freqüências (60Hz). Para tanto, nós projetamos todo o reator para que este objetivo pudesse ser atingido. Os filmes obtidos por nós mostram propriedades ópticas e eletrônicas bastante próximas aquelas dos filmes produzidos pela técnica convencional de descarga luminescente a radiofreqüência (13,56 MHz). A temperatura do substrato ótima para a técnica de descarga luminescente a baixas freqüências está na faixa 150-170&#176C, em torno de 100&#176C menor do que aquela usada para radiofreqüência. Neste trabalho nós apresentamos medidas das propriedades dos filmes, incluindo condutividade no escuro, fotocondutividade, comprimento de difusão ambipolar, absorção no infra-vermelho, gap óptico, e densidade de defeitos de níveis profundos. Para realizar parte destas medidas, nós construímos sistemas experimentais de caracterização exclusivos para o &#945-Si:H. / In this work we present an alternative technique for producing hydrogenated amourphous silicon thin films (&#945-Si:H). We deposited &#945-Si:H in a low-frequency (60 Hz) glow-discharge deposition system. For this purpose, we designed completely the reactor. The films we produced show electronic and optical properties nearly equivalent to those of films prepared by the conventional radio-frequency (13,56 MHz) glow-discharge technique. The optimal substrate temperature for the low-frequency glow-discharge technique is 150-170&#176C, about 100&#176C lower than that radio-frequency. In this work, we report measurements of film properties, including dark conductivity, photoconductivity, ambipolar diffusion lenght, infrared absorption, optical band gap, and deep defect density. To do these measurements, we assembled experimental systems used to characterize &#945-Si:H.

Fluidos em uma descarga brilhante à pressão atmosférica usando uma barreira de dielétrico DBD atraiu o interesse das comunidades de termo-dinâmica, fluido-dinâmica, e comunidades de controle. Este trabalho investiga os efeitos de um atuador de plasma operando numa voltagem e frequência de 8 kV e 4.4 kHz sobre a curva do Cp de um cilindro de PVC em baixa velocidade de escoamento. O experimento foi repetido com o atuador em vários ângulos no cilindro. Os resultados mostram uma aceleração do escoamento junto com um atraso da separação. Esses efeitos são maiores quando o atuador é posicionado num ângulo mais próximo da região da separação. / Fluids in a dielectric barrier DBD glow discharge at atmospheric pressure attracted the interest of the communities of thermo and fluid dynamics as well as control. This dissertation investigates the effects of a plasma actuator operating at 8 kV and 4.4 kHz, on the Cp curve of a PVC cylinder in a low velocity airflow. The experiment was repeated with the actuator at various angles. The results show an acceleration of the flow accompanied with a delay of the flow separation. These effects were shown to be larger when the actuator was positioned at an angle closer to the region of separation.

. / .

The aim of the diploma thesis was the diagnostics of plasma generated in the atmosphere simulating conditions on Mars. This diploma thesis is focused on the simulation of Mars’ atmosphere at atmospheric pressure and normal laboratory temperature. Due to the similar conditions of Mars' atmosphere with Earth, this planet has been explored in the past as well as up to now. Mars' atmosphere is composed mostly of carbon dioxide, which makes up more than 90 % of Mars' atmosphere. A glow discharge generated in a special reactor at atmospheric pressure at a flow of pure CO2 was used to simulate the atmosphere of Mars. Part of the measurement was performed only in pure CO2 with changing current of 20, 25, 30, 35 and 40 mA. Part of the measurements was focused on the study of the effect of the addition of various gases, such as nitrogen, hydrogen and methane, at changes in their flow rates of 1, 2, 3, 4 and 5 sccm. The products formed in the special reactor were analysed using a mass spectrometer with proton ionization and with a flight time analyser. Optical emission spectrometry was used for plasma diagnostics and composition. Mainly simple aliphatic hydrocarbons, alcohols, aldehydes, and ketones were detected. With increasing flow rates of the individual gases, more complex aromatic compounds with higher molecular weights were formed. Corresponding mass and optical emission spectra were measured simultaneously.