Zdenka Kozáková

Application of low temperature plasmas for restoration/conservation of archaeological objects

The low-temperature low-pressure hydrogen based plasmas were used to study the influence of processes and discharge conditions on corrosion removal. The capacitive coupled RF discharge in the continuous or pulsed regime was used at operating pressure of 100-200 Pa. Plasma treatment was monitored by optical emission spectroscopy. To be able to study influence of various process parameters, the model corroded samples with and without sandy incrustation were prepared. The SEM-EDX analyzes were carried out to verify corrosion removal efficiency. Experimental conditions were optimized for the selected most frequent materials of original metallic archaeological objects (iron, bronze, copper, and brass). Chlorides removal is based on hydrogen ion reactions while oxides are removed mainly by neutral species interactions. A special focus was kept for the samples temperature because it was necessary to avoid any metallographic changes in the material structure. The application of higher power pulsed regime with low duty cycle seems be the best treatment regime. The low pressure hydrogen plasma is not applicable for objects with a very broken structure or for nonmetallic objects due to the non-uniform heat stress. Due to this fact, the new developed plasmas generated in liquids were applied on selected original archaeological glass materials.

Influence of electrode material on hydrogen peroxide generation by DC pinhole discharge

Abstract In this work, several materials were studied as electrodes in a pinhole configuration of a DC plasma discharge to estimate their effect on the efficiency of the discharge, indicated by hydrogen peroxide production. Detection was carried out using a specific titanium reagent. This was combined with ICP-OES analysis of the final solutions to determine the difference between the amount of electrode material released during the discharge operation and electrolysis experiment carried out under the same conditions. It was found that from seven studied electrode materials, graphite gives the best results, while lower cost aluminum and titanium-zinc still work well. The most unsuitable materials were copper and brass; in these cases, no hydrogen peroxide was detected in the cathode part of the reactor. Results obtained by ICP analysis indicate that even in the case of brass, the absence of hydrogen peroxide is due to the presence of copper in the material. It probably affects both directly the phase of discharge creation and propagation and the decomposition reactions. Graphical Abstract

Discharge ignition in the diaphragm configuration supplied by DC non-pulsing voltage

This work deals with the ignition of the discharge in the diaphragm configuration generated in water solutions containing supporting NaCl electrolyte. The reactor has volume of 110 ml and it is made of polycarbonate. HV electrodes made of stainless steel are placed in this reactor. Ceramic (Shapal-MTM) diaphragm is placed in the barrier separating the cathode and the anode space. An electric power source supplies the reactor by constant DC voltage up to 4 kV and electric current up to 300 mA. The discharge ignition is compared in the reactor with different sizes of diaphragms. Measurements are carried out in electrolyte solutions with the same conductivity. Images of plasma streamers and bubble formation are taken by an ICCD camera iStar 734. Electrical characteristics are measured by an oscilloscope LeCroy LT 374 L in order to determine breakdown moments at different experimental conditions.

Influence of diaphragm configuration on DC diaphragm discharge breakdown in electrolyte solution

This paper deals with generation of diaphragm discharge in water solutions of sodium chloride with fixed conductivity of 275 μS. The photos were recorded by high-speed iCCD camera at defined times synchronized by the current passing through the system. Three different phases in the current-voltage curve were recognized under all conditions. Only electrolysis proceeds during the first phase at the lowest applied voltage (300 - 1200 V depending on the orifice dimensions), while bubbles were created thanks to the intense Joule heating inside the orifice during the second phase. Finally, the discharge was ignited at applied voltages over 1600 V. These facts were confirmed by iCCD images taken during all three phases. We concluded, by comparing current-voltage characteristics of different orifice diameter sizes, that this parameter had an important influence on the bubbles generation phase. On the contrary, the diaphragm thickness played an important role at the discharge breakdown.

Generation of High Frequency Pin-hole Discharge in Water Solutions

Abstract This paper presents results on electric discharge generation by high frequency high voltage (15–100 kHz) in NaCl solutions with different initial conductivity (100–1300 mS cm-1), and compares them with DC discharge in the same electrode configuration. A batch plasma reactor in the pin-hole configuration contained a ceramic dielectric barrier separating two planar stainless steel electrodes; barrier thickness of 0.6 mm and pin-hole diameter of 0.6 mm was used. Lissajous charts were evaluated from electric measurements for different discharge phases (electrolysis, bubble formation and discharge regular operation). Breakdown moments for different solution conductivities were determined from discharge power evaluation as a function of applied frequency. Breakdown voltage amplitude was decreased by the increasing conductivity in both regimes while frequency and current decreased. Changes of physical parameters (temperature, solution conductivity and pH) as well as production of hydrogen peroxide at different solution conductivities were compared. Solution conductivity was increased in both discharge regimes and with the initial conductivity value. Solution temperature was increased by the discharge in both regimes and with the increasing initial conductivity, too. Solution pH dropped to acidic conditions when HF or DC positive regime was applied while it was enhanced by DC negative regime.

Pin Hole Discharge Creation in Na2SO4 Water Solutions

This work deals with the diaphragm discharge generated in water solutions containing Na2SO4 as a supporting electrolyte. The solution conductivity was varied in the range of 270 ÷ 750 µScm-1. The batch plasma reactor with volume of 100 ml was divided into two electrode spaces by the Shapal-MTM ceramics dielectric barrier with a pin-hole (diameter of 0.6 mm). Three variable barrier thicknesses (0.3; 0.7 and 1.5 mm) and non-pulsed DC voltage up to 2 kV were used for the discharge creation. Each of the current–voltage characteristic can be divided into three parts: electrolysis, bubble formation and discharge operation. The experimental results showed that the discharge ignition moment in the pin-hole was significantly dependent on the dielectric diaphragm thickness. Breakdown voltage increases with the increase of the dielectric barrier thickness.