Made available in DSpace on 2014-12-17T14:13:53Z (GMT). No. of bitstreams: 1 MichelleMA_DISSERT.pdf: 2721160 bytes, checksum: a6cf87e66222fcde35f5dcad4d548b9d (MD5) Previous issue date: 2011-08-05 / This laboratory study involves the participation of a group with professionals from different areas that had contributed to the construction of a multidisciplinary knowledge, about biological response of titanium surfaces modified through thermochemical treatment by plasma. Thus, the crystalline phase was previously characterized in relation to the topography, roughness, molhability and nitrogen concentration in the samples surface. It s indispensable that materials implanted can influence in a good cellular response as well as promotes a bacteria action. Surfaces modified by plasma were exposed to different cultures such as: cellular (human osteoblastic) and bacteria (Staphylococcus epidermidis ATCC35984 and Pseudomonas aeruginosa ATCC 27853) in order to evaluate the biological response. It was evaluated the adhesion, proliferation, morphology and cellular preference of human ostheoblastic cells (HOST), as well as the formation of a biofilm and bacteria proliferation. It was still analyzed the bacteria selectivity ability in relation to the surfaces. The software Image Pro Plus was used to the counting of cells and bacteria adhered to the surface of disks. The results were submitted to the variance analysis (ANOVA), and then, by the Kruskal-Wallis test, using GraphPad Instat ? software, version 3.5 to Windows. The nitrided samples in spite of show a higher roughness and molhability showed a smaller bacteria growing and higher cellular proliferation, when compared to non treated samples, indicating that the treated material present a high efficiency to biomedical implants / Este estudo laboratorial envolveu a participa??o de um grupo de profissionais de ?reas distintas, as quais contribu?ram na constru??o de um conhecimento multidisciplinar, acerca da resposta biol?gica de superf?cies de tit?nio modificadas por tratamento termoqu?mico a plasma. Para tanto, uma avalia??o da an?lise de fase cristalina, topografia, rugosidade, molhabilidade e concentra??o de nitrog?nio nas superf?cies das amostras foram previamente determinadas. ? imprescind?vel que materiais implant?veis influenciem uma boa resposta celular como tamb?m proporcionem uma a??o bacteriost?tica. Com o intuito de avaliar a resposta biol?gica, superf?cies modificadas por plasma foram expostas as seguintes culturas: celular (osteoblasto humano) e bacteriano (Staphylococcus epidermidis ATCC35984 e Pseudomonas aeruginosa ATCC 27853). Avaliou-se a ades?o, prolifera??o, morfologia e prefer?ncia de c?lulas osteobl?sticas humanas (HOST) bem como a forma??o de biofilme e prolifera??o bacteriana. Analisou-se, ainda, a capacidade de seletividade de superf?cie pelas bact?rias. O software Image Pro Plus foi utilizado para contagem das c?lulas e bact?rias aderidas ? superf?cie dos discos. Os resultados foram submetidos ? an?lise de vari?ncia (ANOVA), seguido pelo teste de Kruskal-Wallis, utilizando o GraphPad Instat ?, vers?o 3.5 para Windows. As amostras nitretadas apesar de apresentarem uma maior rugosidade e molhabilidade, quando comparadas com as amostras n?o tratadas, tiveram um menor crescimento bacteriano e uma maior prolifera??o celular. Indicando que o material tratado possui uma alta efici?ncia para implantes biom?dicos

Surfaces of carbon fibre roving were modified by means of a low temperature plasma treatment to improve their bonding with mineral fines; the latter serving as an inorganic fibre coating for the improved mechanical performance of carbon reinforcement in concrete matrices. Variation of the plasma conditions, such as gas composition and treatment time, was accomplished to establish polar groups on the carbon fibres prior to contact with the suspension of mineral particles in water. Subsequently, the rovings were implemented in a fine concrete matrix and their pull-out performance was assessed. Every plasma treatment resulted in increased pull-out forces in comparison to the reference samples without plasma treatment, indicating a better bonding between the mineral coating material and the carbon fibres. Significant differences were found, depending on gas composition and treatment time. Microscopic investigations showed that the samples with the highest pull-out force exhibited carbon fibre surfaces with the largest areas of hydration products grown on them. Additionally, the coating material ingresses into the multifilament roving in these specimens, leading to better force transfer between individual carbon filaments and between the entire roving and surrounding matrix, thus explaining the superior mechanical performance of the specimens containing appropriately plasma-treated carbon roving.

Carbon nanotubes (CNTs) have become one of the most interesting allotropes of carbon due to their intriguing mechanical, electrical, thermal and optical properties. The synthesis and electron emission properties of CNT arrays have been investigated in this work. Vertically aligned CNTs of different densities were synthesized on copper substrate with catalyst dots patterned by nanosphere lithography. The CNTs synthesized with catalyst dots patterned by spheres of 500 nm diameter exhibited the best electron emission properties with the lowest turn-on/threshold electric fields and the highest field enhancement factor. Furthermore, CNTs were treated with NH3 plasma for various durations and the optimum enhancement was obtained for a plasma treatment of 1.0 min. CNT point emitters were also synthesized on a flat-tip or a sharp-tip to understand the effect of emitter geometry on the electron emission. The experimental results show that electron emission can be enhanced by decreasing the screening effect of the electric field by neighboring CNTs. In another part of the dissertation, vertically aligned CNTs were synthesized on stainless steel (SS) substrates with and without chemical etching or catalyst deposition. The density and length of CNTs were determined by synthesis time. For a prolonged growth time, the catalyst activity terminated and the plasma started etching CNTs destructively. CNTs with uniform diameter and length were synthesized on SS substrates subjected to chemical etching for a period of 40 minutes before the growth. The direct contact of CNTs with stainless steel allowed for the better field emission performance of CNTs synthesized on pristine SS as compared to the CNTs synthesized on Ni/Cr coated SS. Finally, fabrication of large arrays of free-standing vertically aligned CNT/SnO2 core-shell structures was explored by using a simple wet-chemical route. The structure of the SnO2 nanoparticles was studied by X-ray diffraction and electron microscopy. Transmission electron microscopy reveals that a uniform layer of SnO2 is conformally coated on every tapered CNT. The strong adhesion of CNTs with SS guaranteed the formation of the core-shell structures of CNTs with SnO2 or other metal oxides, which are expected to have applications in chemical sensors and lithium ion batteries.

This diploma thesis deals with a plasmochemical treatment of photoanodes with an active layer containing TiO2 deposited on two different substrates by material printing. The plasmochemical treatment was performed by a low-temperature ambient-air plasma using a diffuse coplanar surface barrier discharge (DCSBD). The experimental part is focused on the investigation of DCSBD influence on the fabricated photoanodes photoelectrochemical properties, and the influence of plasma treatment time. Process optimization was achieved by height adjustment of the electrode. The processed coatings were electrochemically investigated by linear sweep voltammetry and chronoamperometry.

The diploma thesis deals with the possibility of using the addition of nanoparticles to improve the properties of cement composites. The theoretical part summarizes the findings of research in this area with a focus on methods of dispersion of nanoparticles and their treatment for use in cement composites. The experimental part focuses on the comparison of methods of dispersion and plasma treatment of reduced graphene oxide (rGO) nanoparticle solutions from the point of view of the agglomeration process. During this work, a method of systematic optical/visual monitoring of sedimentation/agglomeration was developed to complement sophisticated methods such as spectrophotometry (UV/Vis) and electron microscopy (SEM). Furthermore, the effect of the addition of rGO on the properties of cement mortar, in the form of aqueous solutions prepared by the dispersion methods determined in the previous section, was investigated.

The plasmachemical removal process of corrosion layers is based on a reduction effect of RF hydrogen low-pressure plasma, and it is used for archaeological objects. Incrustation layers on artifact surface become brittle and porous due to plasma processing. The structure and composition of corrosion layers is changed. Therefore, it is much easier to recover the original surface of the plasma treated artifacts in contrary to those treated by conventional ways. Moreover, we can save time on invasive and thus dangerous mechanical removal of corrosion layers as for example sanding is. After plasma treatment, we can observe fine details of the original surface and memory of tools used during its manufacturing. These details are important information on the origin and manufacturing methods of the artifacts. The plasma reduction process leads to the removal of impurities from cavities as well, and a function of mechanical components of archaeological object can be restored. Moreover, chlorides can be easily removed from the corrosion layers and thus any significant post-corrosion is protected. Each archaeological object is original and it has its own “corrosion history”. First, the object had been exposed to the atmosphere for a long time. Then, it had been often placed in a tomb or grave or it otherwise got into the soil or sea. Thus, each archaeological object was exposed to different corrosion stress (humidity, composition of corrosive environment, etc.). Due to these facts, any universal way of a corroded object treatment is very difficult or even impossible to propose. In this work, the problem was solved using model samples of common metals which were treated at various plasma treatment conditions. Archaeological objects made of iron are the most common artifacts, and the typical corrosion products on iron are akaganeite, rokuhnite, and szomolnokite. These three corrosion products were created on the model samples in laboratory and then, the plasmachemical reduction was applied for their removal. The experiment was done in a Quartz cylindrical reactor with capacitive coupled RF plasma created using outer electrodes. We used discharge power from 100 W to 400 W in a continuous or pulsed regime (duty cycle of 75 %, 50 % and 25 %). Flowing plasma was created in pure hydrogen at pressure of 150200 Pa. Sample temperature was monitored by a thermocouple, and it did not exceed 200C during all these experiments. This temperature is regarded as a limit temperature for metallographic changes of archaeological iron. Higher temperature can cause destruction of archaeological iron objects. The optical emission spectroscopy of OH radical was used for the process monitoring. We focused on the monitoring of OH-radicals generated in the plasma, which are characteristic species formed by this process. Each corrosion product has a different time evaluation of generated OH-radicals, which is closely related to the degradation of a given corrosion product. Corrosion layers were analyzed before and after the plasmachemical reduction by SEM-EDX. We have found that the plasmachemical reduction is not very suitable for the szomolnokite corrosion product, which is degraded with difficulty and at high applied powers, only. However, very good removal efficiency was obtained for the rokuhnite and akaganeite corrosion.

This doctoral thesis concerns the preparation of porous cerium oxide/carbon bilayers on silicon substrates. In this regard, carbonaceous films in the form of amorphous carbon (a-C) and nitrogenated amorphous carbon (CNx) are considered. The influence of various process parameters of the cerium oxide deposition on the morphology of the final cerium oxide/carbon bilayer is investigated. A correlation could be found between the morphol- ogy of the bilayer and the stoichiometry of the cerium oxide film determined by means of XPS. Furthermore, a study regarding the chemical composition of the used carbonaceous films by means of various spectroscopic techniques is presented. It was found that the chemical composition of the carbonaceous films strongly depends on the deposition con- ditions of these films and influences the behaviour of these films during oxygen plasma treatment and cerium oxide deposition, respectively. 1

Title: Modification of polymeric substrates by means of non-equilibrium plasma Author: Anna Kuzminova Department: Department of Macromolecular Physics Supervisor of the doctoral thesis: doc. RNDr. Ondřej Kylián, Ph.D. Abstract: Processing of polymeric materials by means of non-equilibrium plasma is a topic that reaches increasing attention, which is due to the wide range of possible applications. As an example can be mentioned processing of polymeric foils used for food packaging, where plasma treatment enables to improve their functional properties (e.g. increase their printability or enhance their barrier properties). In the frame of this PhD. thesis two different strategies suitable for the modification of polymeric materials were followed. The first one was based on treatment of polymers by atmospheric plasma. The main attention was devoted to the investigation of influence of atmospheric pressure plasma on surface properties of 8 commonly used polymers, namely on their chemical composition, morphology and wettability. In addition, it was observed that plasma treatment causes also alteration of their mechanical properties, may lead to their substantial etching and in some cases improves their biocompatibility. The second studied strategy was based on coating of polymers with thin functional...

Poly(dimethylsiloxan) (PDMS) ist ein wichtiges Polymer, das zunehmend in der Mikroelektronik aufgrund seiner hervorragenden Elastizität und thermischen Stabilität Verwendung findet. Ein limitierender Faktor für den Einsatz von PDMS ist aufgrund des Fehlens von reaktiven Gruppen und der niedrigen freien Oberflächenenergie seine geringe Adhäsion zu anderen Materialien. Zur Erhöhung der Adhäsion ist deshalb die Einführung von polaren, funktionellen Gruppen notwendig. Hier lag die Motivation der vorliegenden Arbeit, die sich eine gezielte Funktionalisierung von PDMS-Oberflächen als Aufgabe gesetzt hatte. Im ersten Teil der Arbeit wurde eine Verbesserung der Adhäsion zu einem fotostrukturierbaren Epoxidharz mittels der Sauerstoff- und Ammoniakplasmabehandlung angestrebt. In beiden Fällen führte die Plasmabehandlung zu der Einführung von unterschiedlichsten funktionellen Gruppen auf die Oberfläche und zu einer Verbesserung des Benetzungsverhaltens gegenüber Wasser. Zudem wurden Haftfestigkeiten erzielt, die um ein Vielfaches höher waren als jene zwischen Epoxidharz und einer unbehandelten PDMS-Oberfläche. Jedoch waren die hydrophilen Eigenschaften nach der Plasmabehandlung während der Lagerung an Luft zeitlich begrenzt, die PDMS-Oberfläche kehrt innerhalb kurzer Zeit in den einst hydrophoben Ausgangszustand zurück. Der Alterungsvorgang wird als „Hydrophobic Recovery“ bezeichnet und ist bei PDMS-Oberflächen, die höheren Plasmaleistungen und Behandlungszeiten ausgesetzt wurden, besonders auffällig. Die Vermeidung dieser Problematik war der Ausgangspunkt für den zweiten Teil der Arbeit. Auf der Grundlage der über die Plasmabehandlungen erzeugten funktionellen Gruppen wurden neue Konzepte für eine kovalente Anbindung von verschiedenen funktionellen Homo- und Copolymeren über die „Grafting to“-Technik entwickelt. Neben der Erhöhung der Adhäsion zu dem Epoxidharz war es möglich, das Benetzungsverhalten gegenüber Wasser durch die Unterbindung der „Hydrophobic Recovery“ zu stabilisieren. Des Weiteren gelang es, durch die Wahl der funktionellen Polymere, die PDMS-Oberfläche gezielt mit gewünschten Eigenschaften auszustatten. Somit ist der Einsatz der polymermodifizierten Oberflächen, außer in der Mikroelektronik, auch auf andere Anwendungen, wie der Biomedizin, der Mikrofluidik oder der Softlithografie übertragbar, in denen eine beständige, definierte Oberflächenfunktionalisierung ein wichtiges Kriterium darstellt.

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