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Study of Nanocomposites for Electrical Insulation
Klampár, Marián ; Mentlík, Václav (referee) ; Váry,, Michal (referee) ; Liedermann, Karel (advisor)
The dissertation thesis submitted deals with the study of dielectric properties of epoxy nanocomposites containing nanoparticles of inorganic oxides. These nanocomposites may have a promising technologic application for electric insulations in view of their higher resistance against partial discharges; yet information about their behavior in the course of ageing is not available. If at least a partial mass replacement of the currently used epoxy insulation with nanocomposite-based insulations is due to occur, the knowledge of the changes of their dielectric properties in the course of their operation will become indispensable. Within the framework of this dissertation, ensembles of samples of epoxy resins without fillers and with Al2O3, WO3, TiO2 and SiO2 fillers in the form of nanopowders, in concentrations up to 12 wt %, have been prepared. These ensembles have been measured prior to ageing and exposed to long-time (up to 5000 hours) ageing at increased temperatures 200, 250 and 300 °C and in a few cases also at 330 and 360 °C. Samples were measured in the course of ageing roughly in a logarithmic time series after 1, 2, 5, 10, 20, 50, 100, 200, 500, 1000, 2000 and 5000 hours. The measured quantities included complex permittivity , internal resistivity i and loss factor tan at temperatures ranging from -153 °C to +167 °C and in the frequency range 10-2 – 106 Hz. Changes in nanocomposites have been investigated using not just dielectric spectroscopy measurements, but other methods, too, namely Fourier-transformed infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). The experiments have proved that materials with different fillers respond to the same concentrations of various fillers in different ways. The addition of nanoparticles, without the addition of microparticles, at a relatively low concentration (max 12 wt %), was not sufficient for reaching fundamental changes in dielectric spectrum; only smaller changes of dielectric strength and shifts of relaxations and in relaxation maps have occurred. Out of more pronounced changes, increase of concentration of the SiO2 filler in the epoxy matrix brings about a decrease of electrical conductivity in the resulting nanocomposite. The TiO2 filler had a different impact. Different TiO2 concentrations make their marked appearance in the region between the relaxation and relaxation. The TiO2-filled nanocomposites do not exhibit the unambiguous dependence of electrical conductivity on nanofiller concentration. It can be concluded that the mere addition of nanoparticles, without the addition of established microparticles, does not change the dielectric spectrum substantially. Generally, a serious problem was the production of the nanocomposite with a uniform distribution of nanoparticles. The preparation of such a nanocomposite was not trivial and, in industrial applications, this issue will require a specific focus, so as to avoid the formation of undesirable aggregates. Within the framework of this research, a methodology for the production of an epoxy nanocomposite has been developed with as high as possible uniformity of nanoparticle distribution.
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Characterization of Nanostructures Deposited by High-Frequency Magnetron sputtering
Hégr, Ondřej ; Boušek, Jaroslav (advisor)
This thesis deals with the analysis of nano-structured layers deposited by high-frequency magnetron sputtering on the monocrystalline silicon surface. The content of the work focuses on the magnetron sputtering application as an alternative method for passivation and antireflection layers deposition of silicon solar cells. The procedure of pre-deposite silicon surface cleaning by plasma etching in the Ar/H2 gas mixture atmosphere is suggested. In the next step the silicon nitride and aluminum nitride layers with hydrogen content in Ar/N2/H2 gas mixture by magnetron sputtering are deposited. One part of the thesis describes an experimental pseudo-carbide films deposition from a silicon target in the atmosphere of acetylene (C2H2). An emphasis is placed on the research of sputtered layers properties and on the conditions on the silicon-layer interface with the help of the standard as well as special measurement methods. Sputtered layers structure is analyzed by modern X-ray spectroscopy (XPS) and by Fourier infrared spectroscopy (FTIR). Optical ellipsometry and spectrophotometry is used for the diagnostic of the layers optical properties depending upon the wavelength of incident light. A special method of determining the surface lay-out of the charge´s carrier life in the volume and on the surface of silicon is employed to investigate the passivating effects of the sputtered layers.
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Study of Optical Properties of Metallic Structures and Their Applications in Nano-Optics
Neuman, Tomáš ; Munzar,, Dominik (referee) ; Kalousek, Radek (advisor)
Interaction of metallic structures with electromagnetic radiation is a living topic of near-field optics including plasmonics and nanophotonics. The field-matter interaction treated on the subwavelength scale opens the path to a wide range of applications, among others to different variants of the surface enhanced spectroscopy. In this thesis we theoretically describe how the near-field properties of the metallic structures can be accessed by a probe of near-field scanning optical microscope. Formation of the signal in the near-field microscopy utilizing weakly interacting probes is discussed. Further, we elucidate the mechanism of the surface enhanced infrared spectroscopy. We utilize a model example of linear dipole antennas interacting with sample structures. A close connection is found between the spectroscopic signal and signal of the scattering type near-field optical microscopy.
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The use DC electrical method in diagnostics of insulating materials
Volf, Michal ; Rozsívalová, Zdenka (referee) ; Frk, Martin (advisor)
In this work describe to the Dielectric relaxation spectroscopy for the evaluation of the actual status of insulation systém. The used methods of quantifying the dielectric response in time domain are polarization-depolarization current and recovery voltage measurement and in frequency domain the loss factor and the complex capacitance measurement. Influence of thermal ageing and temperature dependences of charge and dischage currents are observed.
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Preparation of organic semiconducting thin films by vacuum evaporation
Schön, Martin ; David, Jan (referee) ; Salyk, Ota (advisor)
This thesis deals with preparation of organic molecular thin film compounds and its properties like morphology and purity. The vapour deposition was used for thin films preparation, because used materials are very few soluble. Thin films properties were characterized with the infrared spectroscopy (FTIR) and scanning electron microscope. There are described basics of infrared spectroscopy, spectra measurement and interpretation in the theoretical part. Process of thin film preparation is also described in this part. In the experimental part are described used vacuum technology and measuring instruments, process of sample measurement and there is the list of studied materials. 12 derivates of diketopyrrolopyrrols (DPP) were studied in this thesis. Diketopyrrolopyrroles (DPP) and its derivates have interesting chemical and physical properties, expecting wide range of applications, especially in electronics industry.
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Diagnostics of plasma chemical deposition processes using organometallic precursors
Sahánková, Hana ; Dvořák, Pavel (referee) ; Krčma, František (advisor)
The aim of this work is diagnostic of plasma chemical deposition thin films based on organometallic precursors. Thin layers have recently become one of the most used methods for surface treatment of materials. They are used as a protective, functional layer, they improve surface properties of materials or increase or reduce the adhesion to various compounds. Plasma polymers are a modern trend in surface treatment technology. Their structure is different from classical polymers. The titanium (IV)isopropoxide was chosen as a monomer example, which is frequently used as a monomer for photocatalytic TiO2 films plasma deposition. These thin films are very promising for the removal of various air and water pollutants and thus they can significantly help in the increase of the environmental quality. Measurements took place on a commercial device Plasmatreater AS 400. The theoretical part describes the background needed for the study and diagnostics of plasma processes and technologies. The optical emission spectroscopy was chosen as a diagnostic method, and thus its principles are outlined in the theoretical part. Infrared spectroscopy and X-ray photoelectron spectroscopy were applied for the diagnostics of prepared thin films and they are also described in the theoretical part. The experimental part contains two sections. The first section is dedicated to the plasma diagnostics by optical emission spectroscopy. Discharge was generated in nitrogen or in the air. Measurements were performed at seven different duty cycles and at two different flow rates for each of the working gases. The molecular bands of nitrogen first negative and second systems, CN violet bands, and atomic lines of oxygen and nozzle elements (Cu, Cr) were identified in the spectra. The titanium lines, and bands of TiO were determined if the precursor was added. Electron temperature was calculated using chromium lines, and electron temperature maps were obtained for continuous mode and pulse mode with duty cycle 70% for nitrogen plasma with 500 sccm precursor flow. Similar discharge maps were also processed using the selected line of titanium (520 nm) TiO band (625 nm) again for the same discharge conditions. Furthermore, the dependences of the same quantities were obtained along the discharge axis as a function of duty cycle in both gases with precursor flow of 1000 sccm. The second part of results brings material analyzes of the deposited samples. The peaks of anatase and rutile have been identified by infrared spectroscopy. Using X-ray photoelectron spectroscopy, we found that our layers contain a significant amount of non-dissociated precursor. Moreover, a large number of radicals, which can interact with atmospheric gases, was determined on the surface. These radicals are removable by annealing or by ion etching. All results obtained during this research can significantly help us to improve the quality of deposited layers and allow us also some prediction of the thin film properties at given plasma conditions. Of course, further experimental as well as theoretical studies should be completed to obtain complete knowledge needed for the wide applications of these layers.
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Occurance of urinary stones in the CR and simulation of conditions of their rise.
Zbořilová, Eliška ; Márová, Ivana (referee) ; Vránová, Dana (advisor)
The aim of this diploma thesis was identification of urinary concrements by the infrared spectroscopy and study of conditions of formation of the most frequent urinary stones (calcium oxalates) by the thermodynamic simulation. The theoretical part of this study includes basic information about problems with urolithiasis and technique of identification of urinary concrements. Important part has been devoted to the thermodynamic simulation of formation of calcium oxalate concrements and on this simulation were determinated the conditions for formation of urinary stones. The experimental part contains analysis of real urinary concrements by the infrared spectroscopy and statistical evaluation of the file of 50 149 samples, which were analysed in years 1994 - 2010.
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Physical-chemical property characterisation of thin reflective layers on silicon substrates
Rozsívalová, Zdeňka ; Studýnka, Jan (referee) ; Krčma, František (advisor)
This thesis deals with surface analysis and characterization of optical features of thin films created by hexamethyldisiloxane (HMDSO) plasma polymerization on silicon wafers. The RF plasma industrial deposition equipment was used for the thin layers formation. These thin films serve as protective coatings on the reflective layer in the car light or solar panels. Theoretic part gives basic information about plasma, its occurrence, features, diagnostics and applications. Thin layers, their production and characterization are discussed here, too. Theoretic description of monomer material (including the group of other organosilicones) is also presented here. The FTIR spectroscopy and elipsometry are mentioned as the main methods for thin films characterisation. Because material during its practical use degrades due to external conditions, the influence of them on the thin layer properties is studied using the accelerated aging of created films. Industrial deposition chamber AluMet 1800V made by Leybold Optics, Ltd. installed in Zlin Precision company was used for the thin films production. Thin films were created under different conditions that were selelected near to the real conditions used in technology. Various applied powers (2-5 kW) were used for the deposition under different monomer flows. Further, the influence of oxygen addition on the created film properties was investigated. The deposition process was monitored by optical emission spectroscopy. The spectrometer Jobin Yvon Triax 320 with CCD detector was used. The selected part from every samples set was exposed by UV radiation (48 hours at radiation density of 0.68 W/m2 at 340 nm) to simulate the probable conditions during the layers real use. The surface properties were investigated by measurement of reflected light spectral intensity in the visible range at different angles. The angle between incident and reflected beam was varied in the interval of 40 - 150° with 10° step. The influence of sample preparation conditions as well as their aging effect was studied at the selected angles. Spectral reflectance doesn´t depend significantly on applied discharge power and oxygen addition. The significant shift of reflectance into the red part of spectrum was observed at UV exposed samples more or less independently on the applied discharge power of monomer flow rate. Addition of oxygen during the deposition suppresses this effec significantly. Characterization of thin layer structure was done by FTIR spectroscopy. No significant changes were observed in the structure at different discharge powers of monomer flow rates except total absorption intensities that are proportional to the layr thickness. The oxygen addition, of course, changes the structure significantly. These results are only preliminary because the layers were very thin (deposition conditions were near to the common process standard) and thus the signal/noise ratio was relatively low.
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Analytical methods for hyaluronan
Černá, Lucie ; Mravec, Filip (referee) ; Pekař, Miloslav (advisor)
This thesis deals with of simple methods for determining the concentration of hyaluronan in aqueous solution and compares the performance of each selected methods such as UV -VIS spectroscopy, IR spectroscopy and the method of determination by alcian blue. These methods were chosen for their simplicity and low cost of the assay. As the most reliable of these three methods, seems to be the method of IR spectroscopy. Determination of the concentration of HA by this method is relatively accurate at concentrations above 0.4 % in deionized water. The method of UV-VIS spectroscopy is based on a linear calibration curve determination, but no characteristic peak was detected, which means that this determination could be influenced by other components of the aqueous solution. Weak ionic strength and molecular weight of HA does not affect the determination. In the method with alcian blue, the results were quite unsatisfactory and does not correspond with the literature. Therefore, this method is not applicable in this form for determining the concentration of HA. Another option for determining the concentration of the HA is ELISA method. These are commercially produced kits suitable for determining low concentrations in low volumes. Its price is higher than the above- mentioned methods.
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Stability of Soil Organic Matter
Heldesová, Michaela ; Doskočil, Leoš (referee) ; Kalina, Michal (advisor)
This bachelor thesis summarizes available information about current research of soil organic matter stability and it divides them into two logical units. The first part includes environmental, physical and chemical factors, including human activities, which affect the stability or decomposition of soil organic matter. The methods used for the study of organic matter in the soil are summarized in the second part of this thesis. There the attention is paid to the accumulation of organic matter in specific pools, the ways of extraction of organic compounds and the use of quantitative and qualitative analytical methods to describe various characteristic of organic matter.
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