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Plasmachemical reactors for special syntheses and decomposition
Brožek, Vlastimil ; Janča, J. ; Mastný, L.
In the contribution the design of laboratory plasmachemical reactors for performing chemical reactions with high activation energy is described. It concerns RF-reactors with the capacity or induction excitation of the plasma, plasmachemical reactor with the unipolar microwave discharge, low-frequency gliding plasma reactor (Glid-Arc), and particularly the high-performance generator with water stabilized plasma of Czech provenience WSP®. Operation, effectiveness and output of these reactors are demonstrated on the syntheses of boron carbide and boron nitride of both solid and gaseous precursors, on the syntheses of inorganic pigments on the basis of zirconia, fluorite or condensed polyphosphates and also on tungsten carbide. All of them can be prepared in nanometric particle size with high specific surface area (tens of m2/g).
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Plasma coatings of phosphated steels II
Pokorný, P. ; Mastný, L. ; Brožek, Vlastimil
This article follows the introductory part, presented at the conference APROCHEM 2012 and evaluates the possibility of using different kind of phosphate coatings for the pretreatment of mild steel intended for plasma sprayed ceramic coatings. The phosphate conversion coating has to improve the corrosion resistance of coated steel and also to improve and extend the adhesion of ceramic coating to mild steel surface. Selection the most appropriate phosphate coating (zinc, zinc-calcium, manganese and „three-cations“ phosphate) was established to study the dehydration curves by means of DTA and TGA analysis with subsequent analysis of morphology, integrity and composition of the coating after each dehydration section.Samples were exposed at 200 °C for 10 hours.The measurement results showed that the most stable is manganese phosphate. Plasma deposition of corundum was carried out low-temperature plasma generator WSP ®. The corrosion resistance of coated samples with different phosphate
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Interaction of chalcogenide glasses Ge-As-Se with hexagonal boron nitride
Mastný, L. ; Matušek, M. ; Randáková, S. ; Brožek, Vlastimil
Chalcogenide glasses on the base Ge-As-Se for the applications in infrared optics may content only trace amount of oxygen, because the chemical bonds of the type Ge-O and As-O induce in chalcogenide glasses the generation of absorption bands at the wavelength about 12.8 μm with the consequence of the lowering of optical transmittance of chalcogenide glasses. That is why the chalcogenide glasses must be synthesized in the tubes from special conditioned quartz for to avoid the quartz will be the source of oxygen impurities. The tubes from this quartz are very expensive. The aim of this works is to point out that the chalcogenide glasses may be synthesized also in the tubes from turbostratic hexagonal boron nitride which is refined in the mixture of trichloromethane and ammonia.
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Preparation of gold, silver and platinum colloid solutions by precursors decomposition in low temperature plasma
Brožek, Vlastimil ; Kutílek, Zdeněk ; Mastný, L. ; Sýkora, V. ; Benešová, L. ; Sofer, Z.
Liquid precursor decomposition in the low temperature plasma generated by WSP® was used for synthesis of precious metals nanoparticles. The gold in the form of H[AuCl4], silver in the form of AgNO3 and platinum in the form of H2[PtCl6] were used to generate colloid solutions with concentration of 5 mg.l-1 – 70 mg.l-1 and particle size of 20 nm – 120 nm. The solution contained elevated concentration of nitrite and nitrate ions due to the reaction of plasma with nitrogen form air. In order to reduce the concentration of nitrite and nitrate ions the plasma generated nanoparticles was projected by plasma torch to the ammonium chloride solution. Other way used for reduction of NO3- and NO2- concentration was optimization of geometry of plasma system. The other way was also by application of shrouding effect by nitrogen and ammonia gas. The size of nanoparticles and their concentration can be influenced by geometry of plasma torch, composition of carrier gas and by geometry of
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Production of nanoparticles utilizing water stabilized plasma
Bertolissi, Gabriele ; Brožek, Vlastimil ; Chráska, Tomáš ; Mušálek, Radek ; Neufuss, Karel ; Mastný, L. ; Sofer, Z.
Water stabilized plasma torch (WSP®) generates plasma jet with max. plasma velocity in the nozzle exit 7000m/s and temperature of 25000-30000 K. Reactants injected into the plasma jet undergo complicated radical reactions. Interaction of plasma with injected reactants depends on energy settings of the WSP plasma torch and lasts from 5 to 10 ms. Droplets of inorganic compound solution are fed to the plasma jet by pressurized spray nozzle device. Compounds of AgI,AlIII,TiIV,PtIV,VV, and CrVI undergo decomposition in the extremely high plasma temperature and the decomposed products are collected in liquid separators. Size of the produced nanoparticles in unsettled fraction is from 10 to 200 nm and depends primarily on concentration of inputting aerosol particles. In the case of 15 seconds reaction time and use of saturated solutions at 20°C, one can obtain colloidal solutions with silver, platinum, alumina, titania, vanadia, and chromia nanoparticles in concentrations of 3 to 180mg
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Possible way to prepare nanoparticles from aerosols released at plasma deposition
Brožek, Vlastimil ; Mastný, L. ; Moravec, Pavel ; Ždímal, Vladimír
During plasma deposition of powdered metals or inorganic compounds using WSP® generator, they interact with the plasma having temperature between 25000 and 30000 K. As a result, they melt, evaporate, thermally decompose, get ionized and/or react chemically both with plasma-forming medium and with the surrounding atmosphere or carrier gas. An experimental apparatus was constructed enabling us to capture aerosol particles emitted from the surface of the free flying particles (FFP) heated in a stream of plasma. In this work we studied content, composition and size distribution of nanosized particles of Ag and oxides of Al, Ti, Cr and W, released during plasma deposition process. These particles were analyzed by dynamic light scattering - photon correlation spectroscopy using instrument MALVERN, and with aerosol spectrometers SMPS 3936 and APS 3321.Concentration of aerosols containing nanoparticles of silver or metal oxides with diameters below 100 nm was found to be in the range 85 to
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Improving Bond Strenght between Carbon Steel and Plasma Sprayed Ceramics by Phosphating Process
Pokorný, P. ; Brožek, Vlastimil ; Mastný, L.
Phosphating is currently the highest standard of surface treatment before painting in the vehicle industry. Excluded phosphate crystal layer is due to its high porosity absorbing not only paints but also oil and lubricants that can reliably maintain the surface. Improved bond strenght in the case of coatings exposed in the humid atmospheres in comparison with multiple non-coated surface. Focus of this work is an effort to improve the bond strenght between the diferent plasma-sprayed coatings materials and carbon steel using different phosphate coatings. Because most of the eliminated phosphate crystallizes with four crystal waters the samples was covered by zinc-calcium phosphate, which crystallizes with only two waters [scholzite: Zn2Ca(PO4)2 . 2H2O] and coated from bath of „three-cationts“ phosphate due to the large thickness of the coating and compaction [fosfofylit: Zn2Fe(PO4)2 . 4 H2O]. They decided test for measuring the quality of bond strebght between coating and steel
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Ceramic coatings prepared by liquid precursor plasma spraying
Brožek, Vlastimil ; Kutílek, Zdeněk ; Bertolissi, Gabriele ; Mastný, L.
LPPS method (Liquid precursor plasma spraying) was performed using aqueous solutions of ammonium vanadate and chromate in order to přepade nano-crystalline ceramic coatings on steel and ceramic substrates. Their structure was studied and verified by injecting at different conditions the liquid precursors into the stream of water stabilized plasma. The surface coverage of nano-coatings is inversely proportional to the concentration of precursor and largely depends on the geometric arrangement of the depositing device in which there is a complex process multistage precursor processing within milliseconds.
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Processes of Nanoparticle Formation in Low Temperature Plasma
Brožek, V. ; Mastný, L. ; Moravec, Pavel ; Neufuss, Karel ; Ondráček, Jakub ; Ždímal, Vladimír
This work describes the synthesis of nanoparticles during interaction of several different metals (Ag) or their respective oxides (TiO2, Cr2O3) with oxygen-hydrogen plasma having temperatures above 25000 K. Resulting nanoparticles and/or their aggregates in the size range of 25-300 nm were deposited on metallic targets and/or trapped in the water filters and separated using ultra-centrifugal apparatus. The aerosol spectrometer SMPS 3936 (scanning mobility particle sizer) was used to study the particle size distribution of generated nanoparticles in the size range 14 – 700 nm. In order to extend the measured particle size range towards larger sizes, the APS 3321 spectrometer (aerodynamic particle sizer) with the size range 500-20000 nm was used simultaneously. Both spectrometers were set-up to sample with three minute time resolution. Process conditions and production of inorganic nanoparticles of defined composition are discussed in this work.
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