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Study of plasmachemical reduction of corrosive layers on copper
Šimšová, Tereza ; Selucká, Alena (referee) ; Krčma, František (advisor)
The present diploma thesis concerns the research of plasmachemical reduction of copper corrosion layers. The process was based on using low pressure hydrogen RF plasma in which copper samples are treated for several hours. Four series of copper corrosion layers were prepared in four different corrosion atmospheres. The first two were prepared using saturated vapors of HCl and ammonium acetate that affected copper samples for one week. The second two sets were prepared by samples dipping in HNO3 and H2SO4. EDX analysis confirms visual composition of corrosion layers – chlorides, nitrides and sulphate, respectively. The ammonium acetate produced no corrosion layers and thus this set of samples was omitted. The optical emission spectroscopy was used to find out reactions in a hydrogen RF discharge. At the first, a character of plasma without samples was taken by measuring in continuous and pulsed regime. The integral spectrum intensity (300-700 nm) and intensities of hydrogen atomic lines were observed in the dependences on hydrogen flow, power and duty cycle. After that copper samples were treaded under various conditions in continual and pulse regime, typically at pressure of 170 Pa, 200 W power and hydrogen flow rate of 10.2 ml/min. The integral OH radical spectral intensity in the range of 305 – 330 nm was used as a monitor of plasma treatment process. The experimental results showed that intensities of OH radical depended strongly on the corrosion layer kind as well as on the RF discharge mode. Reduction of corrosion layers treated in the pulsed regime was not so satisfactory then in the continuous regime probably due to lower temperature of sample during the treatment. The total supplied energy into the system was also lower in this case. The sample sputtering was observed during the reduction in continuous regime. It means the corrosion was successfully removed but the process was not stopped at that moment, so it is necessary to propose another additional monitoring process besides observing OH radicals. Our experimental results are the first step in the spread research of plasmachemical treatment of copper made archaeological artifacts.
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Study of volatile hydrocarbon decomposition in non-thermal plasma of surface discharge at atmoapheric pressure
Věrná, Jana ; Rašková, Zuzana (referee) ; Kozáková, Zdenka (advisor)
The main goal of this thesis was to study plasma generated by surface discharge and its application in volatile organic compound destruction. Introduction of this thesis deals with the issue of volatile organic compound. The term of volatile organic compound was defined and explained. Summary of the most important sources of volatile organic compound emissions and possible technics for their elimination was presented. This thesis drew attention on negative aspects of volatile organic compounds on human organism and on the whole environment. The problems of surface discharge and its possible application in various branches are known only few years therefore construction of plasma reactor itself was the first independent step of this work. The plasma reactor was consisted of electrode, which was created from the series of metal stripes each other separated by dielectric barrier. On the surface of the electrode, discharge was regulated and distributed. For the reason of technical limits experiment time was limited up to one minute. The experimental part describes reactor for surface discharge and other parts of apparatus in which degradation volatile organic compound was carried out. Nitrogen was used as carrier gas and it was mixed with air before entering into the reactor. Samples of compounds after degradation process were taken from reactor for the subsequent analysis. Analysis of the products proceeded in a gas chromatogram linked to mass spectrometer. The decomposition products were adsorbed in the SPME filaments or in sorption tubes. The decomposition products were analysed also through the mean of Testo 350 M/XL. This apparatus provided the information on the concentration of small molecules such as CO, H2, NO, NO2 and CxHy Hexane, cyclohexane and xylene were used as VOC examples. Analysis of GC-MS showed decomposition products of hexane, cyclohexane and xylene. The decomposition products were especially various alcohols, ketones, aldehydes and benzene compounds. The apparatus Testo 350 M/XL was unable to detect any CxHy, only large quantity of NO2. This thesis was further focused on possible factors which could have an influence on degradation of compounds, for example input power or different flow of oxygen. It was found that increasing power declined the removal efficiency. The maximum removal efficiency was 87 % for degradation of hexane at the lowest input power. Next part of this thesis was focused on diagnostics of plasma generated in the surface discharge form. The optical emission spectroscopy has been chosen as the best method for plasma characterisation. By this method, various important discharge parameters can be determined, e.g. vibration and rotation temperature. The obtained numeric value of rotation temperature was 840±80 K and vibration temperature was 1880±140 K. The obtained results may be used as a fundament for further study of VOC decomposition in surface discharge.
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Study of chemical processes in Titan atmosphere
Klohnová, Karolína ; Grossmannová, Hana (referee) ; Krčma, František (advisor)
The bachelor’s thesis deals with study of chemical processes in Titan atmosphere simulated under laboratory conditions. The abnormal glow discharge as a for-step for gliding arc discharge was used for the plasma generation in nitrogen-methane gas mixture corresponding to the Titan atmosphere composition. The optical emission spectroscopy was chosen as the basic plasma diagnostic method. The theoretic part of thesis describes briefly history of Titan atmosphere studies including the last space craft obtained results. Later, the fundamental properties of plasmas including their diagnostics are given. The general components determined in Titan atmosphere include N2, CH4, H2 molecules as well as a suite of lower weight hydrocarbons including HCN, C2H2 and C2H4; some traces of higher hydrocarbons and amino acids were determined, too. The electrode configuration corresponding to gliding arc arrangement with interelectrode gap of 2 mm was used with high voltage power supply giving power up to 300 W. Plasma was generated in the nitrogen-methane mixtures (0.5 – 2.5 % of methane) at atmospheric pressure. Both gases had purity better than 99.999% and all system was evacuated before measurement to suppress oxygen traces. Optical emission spectra were taken in dependence of applied power and gas mixture composition. Nitrogen and CN radical spectra as well as atomic lines of hydrogen and carbon were identified in the spectra. The vibrational temperatures of 2300 - 8000 K were determined from the spectra of nitrogen second positive, CN violet and C2 spectral systems. Rotational temperature calculated from nitrogen second positive and CN violet 0-0 bands varied in the interval of 1200 - 4800 K depending on the experimental conditions. The obtained results were submitted as a part of paper into international journal. The obtained results maybe used as a fundament for the future study of Titan atmosphere using also other discharge.
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Characterization of plasma during organosilicone thin film deposition using haxamethyldisiloxane monomer
Blahová, Lucie ; Mazánková, Věra (referee) ; Krčma, František (advisor)
The aim of this thesis is plasma diagnostic during deposition of thin films based on organosilicones. Hexamethyldisiloxane was used as a precursor for plasma deposition in the presence of oxygen, and the diagnosis was performed by using optical emission spectroscopy. The theoretical part summarizes the basic characteristics of plasma and processes occurred at plasma polymerization and deposition. It also deals with thin films and their use in coating materials. A relatively large part is devoted to the specification of the physical-chemical nature of the used analytical method – optical emission spectroscopy. Finally, the principles of rotational, vibrational and electron temperature calculations are described. The contemporary deposition process was carried out in continuous and pulsed mode of radiofrequently excited capacitively coupled discharge. The effects of monomer flow rate, plasma power and duty cycle on the deposition process were studied. In the individual spectra, atomic hydrogen lines of Balmer’s series as well as an atomic oxygen line were identified. Molecular bands of CO have been identified as Angstrom’s system and 3. positive system. In the case of the identified fragments, the intensity dependencies on the monomer concentration in mixture, plasma power and duty cycle were detected. Electron temperature of plasma was also calculated using the relative intensities of atomic hydrogen lines of Balmer’s series. Vibrational and rotational temperature could not have been determined because no suitable fragments for their determination were found in the spectrum. Based on findings mentioned above, partial composition of plasma and some of its properties were estimated. The subject of the further research will be determination of the exact content and structure of the thin films and investigation of other plasma characteristics. Plasma deposition is influenced by many factors, and the study of their optimal combination for the most efficient deposition process is a goal for the future research.
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Corrosion layers removal in low-pressure plasma
Kujawa, Adam ; Grossmannová, Hana (referee) ; Krčma, František (advisor)
A plasmachemical reduction of corrosion layers on copper was studied. In this case two series of copper samples were prepared and putted in two corrosive environments for one week. The first corrosive environment contained a concentrated nitric acid and the second environment contained a concentrated sulfuric acid. Samples thus prepared were ready to be plasmachemicaly treated. The plasmachemical reductions took place in low-temperature, low-pressure, non-isothermal, high-frequency-inducted hydrogen plasma on the Faculty of Chemistry in University of Technology in Brno. The discharge was generated in continual or pulse mode with changeable pulse ratio. To monitor the reduction process an optical emission spectroscopy was used. The radiation from plasma discharge was measured by an optical spectrometer in the intervals of 1 to 10 minutes. An object of our concern in collected spectrum was the radiation of OH radicals with electromagnetical wavelenght in a range of 305 – 330 nm, and which were produced in a reaction between the hydrogen radicals and the oxygen atoms, contained in the corosion layers. A rotation temperature of plasma was calculated from the spectrums of OH radicals in a dependence of discharge conditions. Gathered findings will give us a better knowing of this conservation technique, that is used for treatment of the corroded surfaces of the archeological artifacts, and will also allow more provident appliance of this method on a copper historical objects.
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Plasma diagnostics during the organosilicone layers deposition
Jakobová, Martina ; Dvořák,, Pavel (referee) ; Krčma, František (advisor)
This Bachelor thesis deals with plasma diagnostics during deposition of thin organic-silicone layers. Hexamethyldisiloxane (HMDSO) was use as a precursor and emission spectroscopy of plasma was used as diagnostic method. Theoretical part describes plasma and its most important properties. Attention has been also paid to processes of plasma-chemical deposition of thin layers, their use and properties. Finally, principles of emission spectroscopy and calculation procedures of vibrational, rotational and electron temperatures in plasma are described. Deposition itself was realised both in pulse and continuous mode of RF discharge under decreased pressure of 60 Pa. Apart from deposition in pure HMDSO also depositions with HMDSO with addition of 10 and 25 % of oxygen were realised. Measurements were performed in wavelength interval from 320 to 780 nm. Individual lines of atomic hydrogen H-alpha and H-beta were identified in the obtained spectra, as well as molecular bands of CO transitions 0-0, 0-1, 0-2, 0-3 and the second positive nitrogen system transitions 0-0, 0-1. The spectral line of atomic O was identified if oxygen was added into the reaction gas mixture. The dependences of selected bands and lines intensities on the power supplied to plasma were observed. Electron temperature was determined from hydrogen atomic lines, and it was varied within the interval from 2700 to 5500 K in dependence on deposition conditions. It was impossible to determine vibrational and rotational temperatures, since the necessary molecular constants for the detected particles were not found. Based on the obtained results, it was possible to determine partly composition of plasma and to determine some of its properties. Results show that composition and supplied energy influence considerably plasma itself and that in future it will be necessary to investigate relation between these parameters and properties of created thin layers.
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Optical emission spectroscopy of the nitrogen post-discharge plasma with metal trace impurity
Bocková, Ivana ; Mazánková, Věra (referee) ; Krčma, František (advisor)
The bachelor´s thesis deals with the optical emission spectroscopy of the nitrogen post-discharge with metal trace impurity. The analysed sample introduced to the low-temperature plasma was zinc vapor and stannic chloride. As a diagnostic method was choosen optical emission spectroscopy as one of the simplest plasma diagnostic methods. The teoretical part is aimed to information about plasma and processes in the plasma. The special focus is deald for post-discharged plasma and the optical emission spectroscopy. Measurement itself is implemented in flowing regime of DC post-discharge under low pressure. The intensities of selected nitrogen bands and atomic lines are observed as a function of metal vapor presence. The simplified mechanism of the observed phenomen is presented. The possible excitation mechanisms are shown of metallic atoms during the post-discharge.
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Study of plasmachemical reduction of corrosive layers on brass
Řádková, Lucie ; Selucká, Alena (referee) ; Krčma, František (advisor)
The main topic of this bachelor thesis is plasmachemical treatment of archeological artifacts, especially plasma chemical treatment of brass corrosion layers. Low-pressure, low-temperature hydrogen plasma is used for this process. Nowadays, the technology is used mainly for iron or silver based materials but even for them the optimal conditions for the corrosion removal are not fully known yet. The knowledge about other metallic materials is fully missing. Two sets of brass samples were prepared in different corrosion atmospheres. The first atmosphere was prepared using saturated vapors of HCl. The samples were in this atmosphere during one month, and corrosion layers were orange-brown. The second set was prepared using ammonium solution, the samples were in this atmosphere for one day, corrosion layers were blue. The generation of capacitively coupled plasma in continuous mode by different supplied power was done. The experiments were carried out at 100 Pa with hydrogen gas flow of 50 sccm. Discharge power was varied in the interval 50 – 200 W and the treatment duration was 70 – 140 min. The optical emission spectroscopy of OH radical was used to find out all changes those have been resulting from plasmachemical reactions. The OH radical integral intensities were observed, they were used to monitoring plasma chemical reduction process. Spectral intensity of spectroscope was in the range 290 – 330 nm. After the plasmachemical treatment, it was very difficult to remove corrosion layers of HCl, but removing of NH3 corrosion layers was easy. It was caused by type of corrosion process (corrosion layers were influenced by time of corrosion process). This bachelor thesis is the start to find out conduct corrosion layers of brass in plasma treatment. In future, plasma treatment could be used to treatment of real archaeological artifacts.
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Study of processes during the organosilicone thin films deposition
Flamíková, Kristýna ; Rašková, Zuzana (referee) ; Krčma, František (advisor)
The aim of this work is plasma diagnostic during the deposition of thin films based on organosilicone compounds. Tetravinylsilane (TVS) was used in this study; the optical emission spectroscopy was applied for the diagnostics. The theoretical part of this work gives a basic fundaments of optical emission spectroscopy and brings the procedures for rotational, vibrational, and electron temperature calculations. The deposition process was carried out in pulsed regime with duty cycle 1:4 to 1:499. The pure TVS and TVS containing 10, 40 and 80 % with total gas mixture flow rate of 0.5 sccm were used during the deposition. The hydrogen atomic lines and many rotational lines of molecular hydrogen were identified in the spectra. Besides them, the molecular band of SiH, CH and C2 were observed. The atomic oxygen lines and continuum with a maximum at 550 nm were recorded in the case when oxygen was added. The rotational temperature calculated from 0-0 CH band was in the range 1700 - 2100 K depending on the discharge conditions. The electron temperature of about 1800 K was calculated from hydrogen atomic lines. The experimental results showed the partial plasma composition and some plasma basic characteristics were obtained.
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