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Preparation Techniques and Characterization of Electrodes with Nanostructured Surface
Hrdý, Radim ; Trnková, Libuše (referee) ; Janderka,, Pavel (referee) ; Hubálek, Jaromír (advisor)
Nowadays, nanostructures fixed on solid substrates and colloidal nanoparticles permeate through all areas of human life, in area of sensors and detection as well. This dissertation thesis deals with the fabrication of nanostructures on the surface of planar electrodes via self-ordered nanoporous template of aluminum trioxide. The nanofabrication, as one of many possible techniques, is used to increase the active surface area of electrodes by creating unique surface types with specific properties. These electrodes are very perspective in the applications, such as biomolecules electrochemical detection and measurement. The transformation of aluminum layer into non-conductive nanoporous template in the process of anodic oxidation is a fundamental technique employed to obtain the array of nanostructures in this thesis. The fabrication of high quality nanoporous membranes with narrow pore size distribution on various types of metallic multilayers is one of the key experimental parts in this work. Several problems associated with the production of the thin-film systems, including the dissolving the barrier oxide layer, are discussed and solved. Another part of this work deals with the use of nanoporous membrane as a template for the production of metallic nanostructures via electrochemical metal ions deposition directly into the pores. The obtained nanostructures as nanowires, nanorods or nanodots are characterized by the scanning electron microscopy and energy-dispersive or wavelength X-ray spectroscopy. The electrode surface, modified by gold nanostructures suitable for the detection of biomolecules, has been chosen for the electrochemical measurements, due to the gold biocompatibility. The nanostructured electrodes were characterized by electrochemical impedance spectroscopy and cyclic voltammetry. The effect of nanostructured surface geometrical parameters, including the size of the electrochemically active area, on the results of electrochemical measurements has been observed and compared to flat gold electrodes. Two model biomolecules, namely guanine and glutathione, have been chosen for the study of potential application of these nanostructures in biosensors.
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Liquid electrolytes for supercapacitors
Bill, Jan ; Dvořák, Petr (referee) ; Sedlaříková, Marie (advisor)
This work deals with the preparation of liquid electrolytes from different types of aprotic solvents with the aim of their application as electrolytes in electrochemical supercapacitors. Different sorts of aprotic solvents have been chosen, in which the following forms of salts were used: LiBF4, LiClO4,LiPF6. In the next part of the work, the properties of these solvents were measured and the best electrolyte, according to the biggest possible capacity of the system, was chosen. In the theoretical part of this work, the physical principle of supercapacitors and their propeties are described. It deals with electrolytes, their division and with the properties that are appropriate for supercapacitors. The experimental part of the work describes the process of preparation of the samples of electrodes, electrolytes and the techniques of measuring their capacities.
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Impedance measurement of lead-acid accumulator properties
Vaculík, Sebastian ; Neoral, Jiří (referee) ; Abraham, Pavel (advisor)
This work deals with the new and unique four-point method measurement of the impedance characteristics for experimental positive electrode. The theoretical part provides a short introduction to the electrochemical power sources, including the lead-acid batteries, which were used for measurement. Furthermore, there is description of the principle of electrochemical impedance spectroscopy and analysis of obtained data by using the equivalent circuit, consisting of passive components. The experimental section is devoted to the description of the device, which is used for realization of connection of electrodes with Potenciostat VSP, and program which is used for the simplification of processing of results. The main aim of this bachelor thesis is to get better understanding of lead-acid accumulators and impedance measurements. At practical part of the thesis I performed first measurements by two-step method based on electrochemical impedance spectroscopy.
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Carbon based electrodes for supercapacitors
Moncoľ, Maroš ; Kunovjánek, Miroslav (referee) ; Dvořák, Petr (advisor)
This master thesis deals with supercapacitors based on electrical double layer and proper carbon electrodes for this type of supercapacitors. In theoretical part of work is described theory of supercapacitors, energy storage principles and their properties. In the next part are described carbon materials, their properties and electrochemical methods of measurements that we used. In the experimental part is described preparation of electrodes, results and conclusion.
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Electrochemical characteristics of AZ31 and AZ61 magnesium alloys in Hanks‘ solutions
Minda, Jozef ; Wasserbauer, Jaromír (referee) ; Tkacz, Jakub (advisor)
This thesis deals with the characterization of electrochemical corrosion properties of magnesium alloys as promising materials for biomedical applications. The wrought alloys AZ31 and AZ61 were used and exposed to corrosive environments of Hanks solutions (SBF) to simulate environmental conditions in living organisms. For the evaluation of the surfaces was used scanning electron microscopy (SEM) with elemental analysis measured by energy-dispersive spectroscopy (EDS). Short-term (5 min) and long-term (72 h) corrosion tests were conducted in order to optimize the measurement methodology and obtain corrosion parameters - especially corrosion potential (Ekor), corrosion current density (ikor) and polarisation resistance (RP). To evaluation of the short-term tests were by potentiodynamic tests, namely the linear polarization (LP) test. Long-term tests were measured by electrochemical impedance spectroscopy (EIS). Effects of the composition of the alloys (AZ31 and AZ61), surface treatment (grinding and polishing) and the composition of the solution (SBF without Ca, Mg, and with Ca, Mg) were compared. Complex corrosion behaviour in time was characterized and corrosion mechanisms were discussed.
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Nanoporous Enzyme-Based Impedimetric Biosensor
Košelová, Z.
The ordered nanopores surfaces has been studied in the field of biosensors for the detection of affinity interactions such as antigen-antibody or nucleic acid hybridization. Nanopores are frequently fabricated by anodic oxidation of aluminium. This method is practically simple method of highly ordered pore formation, but is not suitable for massive production. The principle of detection is usually based on the degree of pore blockage by biomolecular interaction that allows a sensitive electrochemical response. Here we show the development and characterization of the nanopore-based enzymatic biosensor for the detection of analytes. We performed and tested the concept of the simple and versatile method of nanopores formation on the electrode using non-conductive polystyrene nanoparticles. The variability in pore size was modulated by nanoparticles diameter (40 and 80 nm). We measured response of our designed biosensor using electrochemical impedance spectroscopy in presence of redox mediator at low potential. The smaller diameter of nanopores increases charge transfer resistance. Biosensors with 80 nm nanoparticles had behaviour similar to reference without nanoparticles, therefore the pore was too wide for this design. The limit of detection from Rct showed to be at most 0.01 mM for every sample type. This proposed biosensor contributes to the basic knowledge about nanopores sensors, and it could have a potential, for example, in the development of ―point of care‖ devices.
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Electrochemical Characterization of Self-Assembled Monolayers Containing Redox Switching Element
Nováková Lachmanová, Štěpánka ; Kocábová, Jana ; Vavrek, František ; Sebechlebská, Táňa ; Šebera, Jakub ; Kolivoška, Viliam ; Lukášek, J. ; Balzer, N. ; Valášek, M. ; Hromadová, Magdaléna
Adsorption properties of molecules containing [Ru(terpy)2]2+ and [Os(terpy)2]2+ redox switching element connected to the electrode surface by tripodal thiolate anchoring groups have been studied together with their charge transfer properties in the adsorbed form. STM-based current-voltage measurements confirmed that the conductance of self-assembled monolayer containing [Os(terpy)2]2+ redox switching element is lower than that containing [Ru(terpy)2]2+ element. This observation agrees with previously observed differences in the electron transfer rate constants of these molecules in their adsorbed state.
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Analysis of liquid electrolyte electrical parameters using impedance spectroscopy
Brabenec, Josef ; Pikula, Stanislav (referee) ; Havránek, Zdeněk (advisor)
The bachelor thesis deals with impedance spectroscopy of electrochemical systems, especially liquid electrolytes. The method of impedance spectroscopy is widely used to describe electrochemical cells, batteries and electrolytes for diagnostic purposes over a wide range of frequencies. This thesis presents the main types of impedance imaging in the complex and frequency domain, as well as basic information on the measurement methods used and the methods for impedance analysis. The main part of the thesis was the development of software for automated impedance measurements and estimation of equivalent circuit parameters using basic and specialized circuit elements. A workplace with fabricated electrodes for liquid electrolyte measurements was prepared for the application. The functionality of the application was verified by real measurements of different concentrations of water and salt solutions. The validity of the estimated equivalent circuit parameters was verified on measured simple circuits connected from basic circuit elements and was also verified using the commercially used ZView software.
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The effect of temperature on the charging and discharging characteristics of lithium-ion batteries
Doleželová, Eva ; Máca, Josef (referee) ; Libich, Jiří (advisor)
This thesis deals with operation principles of lithium-ion batteries, its degradation principles, capacity fade, materials used, formats, main characteristics, development, uses and mid to high temperature behaviour. The thesis aims to study aging characteristics of commercially available lithium-ion batteries. In the practical part of the thesis, the key parameters of selected types of commercially available lithium-ion batteries were measured under normal temperature conditions. The measurement was repeated at an elevated temperature. Results were analysed and effects of different temperatures on the selected characteristics were concluded both verbally and graphically. A conclusion evaluates short-term and long-term impacts of ambient temperature on rate capability, ageing, capacity fade and longevity.
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Development of Novel Electrochemical Methods Using Various Membrane Materials for Monitoring of Selected Anticancer Drugs and Phytochelatins
Skalová, Štěpánka ; Barek, Jiří (advisor) ; Labuda, Ján (referee) ; Trnková, Libuše (referee)
Present Ph.D. Thesis is focused on the development of electrochemical methods for determination of anticancer drugs using various types of membranes for their preliminary separation. Furthermore, this Thesis reports the study of transport mechanisms of heavy metals in the presence of phytochelatins across biological membranes. Sodium anthraquinone-2-sulphonate (AQS) was used as a model compound for its similar structure with anthraquinone-based (AQ-based) anticancer drugs (doxo/daunorubicin) and also due to its better availability. All these compounds can be easily electrochemically oxidized and/or reduced. Redox behaviour of AQS was investigated by cyclic voltammetry (CV) and differential pulse voltammetry (DPV) in a cathodic region on mercury meniscus modified (m-AgSAE) and polished silver solid amalgam (p-AgSAE) electrodes, Obtained results were used for the development of a micro-volume voltammetric cell (MVVC). Its applicability for voltammetric determination of anticancer drugs was verified by using doxorubicin (DX) as a model substance. The second part of this Thesis deals with therapeutic monitoring of anticancer drugs in the blood circulation of the patients. For pilot experiments, a liquid-flow system with dialysis catheter and amperometric detection was used. The flow rate of carrier...
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