The self-discharge of an electric double-layer capacitor with composite activated carbon electrodes and aqueous electrolyte (1 M MgSO₄) was studied in detail. Under a long-term potentiostatic charge (stabilization), a decrease in the discharge capacity was observed in the region of voltages exceeding 0.8 V. The self-discharge process consists of two phases. In the initial phase, the cell voltage drop is due to the charge redistribution inside electrodes. During the main phase, the charge transfer between the electrodes determines the voltage drop. The optimal stabilization time of the self-discharge was found to be 50 min at 1.4 V. Hydrophilization of the negative electrode occurred during long-term polarization due to the formation of epoxy functional groups.

The electrochemical properties of the highly porous reduced graphene oxide/titanium dioxide (rGO/TiO₂) nanocomposite were studied to estimate the possibility of using it as a supercapacitor electrode. Granular aerogel rGO/TiO₂ was used as an initial material for the first time of manufacturing the electrode. For the aerogel synthesis, industrial TiO₂ Hombikat UV100 with a high specific surface area and anatase structure was used, and the aerogel was carried out with hydrazine vapor. Porous structure and hydrophilic–hydrophobic properties of the nanocomposite were studied with a method of standard contact porosimetry. This is important for a supercapacitor containing an aqueous electrolyte. It was found that the hydrophilic specific surface area of the nanocomposite was approximately half of the total surface area. As a result of electrochemical hydrogenation in the region of zero potential according to the scale of a standard hydrogen electrode, a reversible Faraday reaction with high recharge rate (exchange currents) was observed. The characteristic charging time of the indicated Faraday reaction does not exceed several tens of seconds, which makes it possible to consider the use of this pseudocapacitance in the systems of fast energy storage such as hybrid supercapacitors. Sufficiently high limiting pseudo-capacitance (about 1200 C/g TiO₂) of the reaction was obtained.

Low-reversible charging processes are studied on highly dispersed carbon electrodes used in double-layer capacitors and having high specific surface area (higher than 1000 m²/g). Restrictions on power and cyclability of such capacitors are due to the occurrence of irreversible and low-reversible electrode recharging processes. Here, most characteristic processes are those of electrolyte decomposition and those related to electrolyte intercalation into the inner structure of carbon material. Summing up the obtained data about the deep cathodic charging of the electrodes based on activated carbon, one can conclude that practically all of them can be explained from the viewpoint of a solid-phase bulk charging of carbon.

The types of cells and methods of electrochemical reduction of graphene oxide films were described. The possibility of creating ultrathin membrane–electrode assemblies of supercapacitor cells was demonstrated. The peculiarities of the electrochemical behavior of films of different thicknesses that contact with carbon and metal current collectors were shown. The limiting charge (1500–2000 C/g) for complete electrochemical reduction of graphene oxide was determined. Possible mechanisms of proton conductivity along the basal faces of graphene oxide flakes were proposed. The nature of the current collector was shown to affect the electron–hole conductivity of graphene oxide films and the observed contact potential difference.

Impedance and potentiodynamic studies have been carried out to investigate reversible processes on the surface of electrodes based on activated carbon (AC). Relationships have been found between the reversible capacity and true resistance, on the one hand, and the potential, on the other. Stoichiometric characteristics of AC charging in sulfuric acid have been obtained. A mechanism of the reversible surface process is suggested. It is concluded that Faraday pseudocapacity makes a considerable contribution to charging of AC electrolytes. The amount of gas liberated in the course of AC wetting in electrolyte has been measured. It is assumed that the amount of liberated gas depends on the amount of active oxygen involved in the current-forming reaction. Based on the data obtained, a redox surface reaction is substantiated in general form.

In this review electrochemical and structural data for the electrodes made of certain of perspective materials for supercapacitors are considered. These electrodes were made on the basis of high-dispersed carbon materials. The following materials were used: singlelayer and multilayer carbon nanotubes; reduced oxide of graphene; the carbide type activated carbon; polyacrilonitrile fibers treated by carbonization and activation; the activated carbon fibrous material; the activated carbon cloth; a composite of polyporphirine on carbon black; polyporhine of magnesium, electrodeposited on carbon paper; and a polyaniline composite with the singlelayer nanotubes, electrodeposited on carbon paper. The short review of techniques of synthesis of these electrode materials is presented. Comparison of capactance characteristics of these electrodes for the purpose of the recommendation of their use in certain types of electrochemical supercapacitors is carried out.