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Brass Corrosion Layers Reduction by Low-Pressure Low-Temperature Plasma
Řádková, Lucie ; Slavíček,, Pavel (referee) ; Zahoran,, Miroslav (referee) ; Krčma, František (advisor)
This thesis presents results of the corrosion layers removal which could be found on the archaeological artefact surfaces. The low pressure low temperature plasma reduction was used for this purpose. Brass samples were chosen for this study. Two different ways have been used to form model corrosion layers. Several sets of corrosion layers were prepared in laboratory in two different corrosion atmospheres, namely ammonia atmosphere and atmosphere of hydrochloric acid. These samples were placed into desiccator. Small quantities of sand were added to some sets of samples so samples with sandy incrustation were prepared. The corrosion layers had been usually formed during four weeks. The second way, which was used to prepare model corrosion layer, was the natural corrosion in soil or compost. In this case, the corrosion layers had been formed approximately 2 years. The samples were treated in the low pressure (150 Pa) cylindrical Quartz reactor (90 cm long and 9.5 cm in diameter) with a pair of external copper electrodes connected via the matching network to a radiofrequency generator (13.56 MHz). The flows of working gases were set by independent mass flow controllers. Whole system was continuously pumped by the rotary oil pump which was separated from the discharge reactor by liquid nitrogen trap with aluminium chips eliminating dust and reactive species from the gas flow. Each sample was placed on a glass holder at the reactor center. Plasma was generated in pure hydrogen or in mixture of hydrogen and argon. Total flow of working gas was 50 sccm. Different ratios of gas mixture were tested, the ratio 30 sccm hydrogen and 20 sccm argon flows was the best. RF discharge was used in a continuous and pulsed regime. Pulsed mode was carried out with various duty cycle at the frequency of 1000 Hz. There were two ways of temperature monitoring. The sample temperature during the treatment was monitored by a K-type thermocouple installed inside the sample in the first case. Thermometer optical probe was connected to the sample surface by a small stainless plate and allowed continuous sample temperature monitoring in the second way. Safe object temperature for copper and copper alloys is 100–120 °C. To avoid exceeding this temperature, power control or the duty cycle in pulse mode were automatically controlled if thermometer optical probe was used. Plasma chemical treatment is based on generation of reactive atomic hydrogen in plasma discharge. The main reactions during reduction were reactions between oxygen and chloride contained in the corrosion layer and the hydrogen ions and neutral atoms generated in the plasma. These reactions create an unstable OH radical, which emits light in the region of 306–312 nm. This radiation was detected by the optical emission spectroscopy using Ocean Optics HR4000 spectrometer with 2400 gr/mm grating. Data obtained from this method were used to calculate rotational temperatures and integral intensity of OH radicals that were used for the process monitoring. Corrosion layer was not completely removed during the reduction, but due to the reactions which occur in the plasma corrosion layer became brittle and after plasma chemical treatment can be removed easily. The SEM-EDS material analyses were carried out before and after treatment of some samples. Some samples were analysed by XRD analysis. EDS analysis showed that amount of oxygen and chloride was decreased, mainly at 400 W pulse mode.
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Preparation and characterization of nanostructures for catalysis and gas detection
Haviar, Stanislav ; Matolínová, Iva (advisor) ; Zahoran, Miroslav (referee) ; Plšek, Jan (referee)
First part of this thesis is focused on magnetron sputtering deposited layers of cerium oxide using carbonaceous substrates. Micrographs from scanning and transmission electron microscopes reveal that cerium oxide layers exhibit remarkable roughness and nano-porosity. In this work there are presented optimized key preparation parameters for growth of highly nano-porous layers of cerium oxide on amorphous graphite as well as on graphite foil. The effect of residual atmosphere during the magnetron sputtering deposition is discussed. Results of deposition using oxygen/argon mixture as working gas are presented. A simple growth model is formulated and discussed. Second part deals with utilization of cerium and tungsten oxides as conductometric gas sensors. A testing station was constructed for gathering sensorial properties of such devices. The construction and abilities of the measuring system designed by the author are noted. Preliminary results of measurements of response to hydrogen are presented. Cerium oxide layers suprisingly exhibit measurable response to hydrogen gas. Tungsten oxide nanowires grown on mica substrate were formed into gas sensor via electron beam lithography and show high sensitivity. Powered by TCPDF (www.tcpdf.org)
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Preparation and characterization of nanostructures for catalysis and gas detection
Haviar, Stanislav ; Matolínová, Iva (advisor) ; Zahoran, Miroslav (referee) ; Plšek, Jan (referee)
First part of this thesis is focused on magnetron sputtering deposited layers of cerium oxide using carbonaceous substrates. Micrographs from scanning and transmission electron microscopes reveal that cerium oxide layers exhibit remarkable roughness and nano-porosity. In this work there are presented optimized key preparation parameters for growth of highly nano-porous layers of cerium oxide on amorphous graphite as well as on graphite foil. The effect of residual atmosphere during the magnetron sputtering deposition is discussed. Results of deposition using oxygen/argon mixture as working gas are presented. A simple growth model is formulated and discussed. Second part deals with utilization of cerium and tungsten oxides as conductometric gas sensors. A testing station was constructed for gathering sensorial properties of such devices. The construction and abilities of the measuring system designed by the author are noted. Preliminary results of measurements of response to hydrogen are presented. Cerium oxide layers suprisingly exhibit measurable response to hydrogen gas. Tungsten oxide nanowires grown on mica substrate were formed into gas sensor via electron beam lithography and show high sensitivity. Powered by TCPDF (www.tcpdf.org)
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Investigation of Pt-SnOx gas sensors
Kúš, Peter ; Matolín, Vladimír (advisor) ; Zahoran, Miroslav (referee)
1 is a suitable material for thin-film gas sensors. Higher sensitivity could be achieved by platinum dopping of the layer. This work focuses on the optimalization of and thin film preparation by radio-frequency magnetron sputtering method. Subsequent analysis by means of XPS, AFM, SEM and XRD was carried out to determine physicochemical attributes of resulting layers. It appears that after the deposition, platinum within the layer is present in the metalic , as well as in the mixed chemical state. After the annealing process mixed state dominates over metalic state and after additional annealing platinum is present solely in oxidized form. Sensory response of layers for presence of hydrogen were examined on two different chip platforms (glass with chromium contacts and sapphire with platinum contacts). Contrary to expectations, the platinum dopped layers performed worse in comparison to the pure tin dioxide layers. This could be explained by the fact, that after annealing platinum within the layer was present mainly in the non-metalic form. Both and layers were more sensitive on sapphire platform, which could be associated with the crystal structure formed on its surface or with presence of metalic contacts.
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Brass Corrosion Layers Reduction by Low-Pressure Low-Temperature Plasma
Řádková, Lucie ; Slavíček,, Pavel (referee) ; Zahoran,, Miroslav (referee) ; Krčma, František (advisor)
This thesis presents results of the corrosion layers removal which could be found on the archaeological artefact surfaces. The low pressure low temperature plasma reduction was used for this purpose. Brass samples were chosen for this study. Two different ways have been used to form model corrosion layers. Several sets of corrosion layers were prepared in laboratory in two different corrosion atmospheres, namely ammonia atmosphere and atmosphere of hydrochloric acid. These samples were placed into desiccator. Small quantities of sand were added to some sets of samples so samples with sandy incrustation were prepared. The corrosion layers had been usually formed during four weeks. The second way, which was used to prepare model corrosion layer, was the natural corrosion in soil or compost. In this case, the corrosion layers had been formed approximately 2 years. The samples were treated in the low pressure (150 Pa) cylindrical Quartz reactor (90 cm long and 9.5 cm in diameter) with a pair of external copper electrodes connected via the matching network to a radiofrequency generator (13.56 MHz). The flows of working gases were set by independent mass flow controllers. Whole system was continuously pumped by the rotary oil pump which was separated from the discharge reactor by liquid nitrogen trap with aluminium chips eliminating dust and reactive species from the gas flow. Each sample was placed on a glass holder at the reactor center. Plasma was generated in pure hydrogen or in mixture of hydrogen and argon. Total flow of working gas was 50 sccm. Different ratios of gas mixture were tested, the ratio 30 sccm hydrogen and 20 sccm argon flows was the best. RF discharge was used in a continuous and pulsed regime. Pulsed mode was carried out with various duty cycle at the frequency of 1000 Hz. There were two ways of temperature monitoring. The sample temperature during the treatment was monitored by a K-type thermocouple installed inside the sample in the first case. Thermometer optical probe was connected to the sample surface by a small stainless plate and allowed continuous sample temperature monitoring in the second way. Safe object temperature for copper and copper alloys is 100–120 °C. To avoid exceeding this temperature, power control or the duty cycle in pulse mode were automatically controlled if thermometer optical probe was used. Plasma chemical treatment is based on generation of reactive atomic hydrogen in plasma discharge. The main reactions during reduction were reactions between oxygen and chloride contained in the corrosion layer and the hydrogen ions and neutral atoms generated in the plasma. These reactions create an unstable OH radical, which emits light in the region of 306–312 nm. This radiation was detected by the optical emission spectroscopy using Ocean Optics HR4000 spectrometer with 2400 gr/mm grating. Data obtained from this method were used to calculate rotational temperatures and integral intensity of OH radicals that were used for the process monitoring. Corrosion layer was not completely removed during the reduction, but due to the reactions which occur in the plasma corrosion layer became brittle and after plasma chemical treatment can be removed easily. The SEM-EDS material analyses were carried out before and after treatment of some samples. Some samples were analysed by XRD analysis. EDS analysis showed that amount of oxygen and chloride was decreased, mainly at 400 W pulse mode.
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