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Andrews, A. T., Electrophoresis, Theory, Techniques and Biochemical and Clinical
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Applications, Oxford University Press, Oxford, 1982. Boguslavsky, L. I., Insulator/electrolyte interface, CTE, 1, 329 (1980). Butler, J. A. V., see page 202. Gaal, O., G. Medgyesi, and L. Vereczkey, Electrophoresis in the Separation of Biological Macromolecules, John Wiley & Sons, New York, 1980. Gerischer, H., Semiconductor electrode reactions, AE, 1, 31 (1961). Gerischer, H., Electrochemical photo and solar cells. Principles and some experiments, /. Electroanal. Chem., 58, 263 (1975). Green, M., Electrochemistry of the semiconductor-electrolyte interface, MAE, 2, 343 (1959). Hunter, R. J., The double layer in colloidal systems, CTE, 1, 397 (1980). Lyklema, J., The electrical double layer on oxides, Croatica Chem. Acta, 43, 249 (1971). Maredek, V., Z. Samec, and J. Koryta, Electrochemical phenomena at the interface of two immiscible electrolyte solutions, Advances in Interfacial and Colloid Science, 29, 1 (1988).
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244 Morrison, S. R., Electrochemistry of the Semiconductor and Oxidized Metal
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Electrodes, Plenum Press, New York, 1980. Myamlin, V. A., and Yu. V. Pleskov, Electrochemistry of Semiconductors, Plenum Press, New York, 1967. Pleskov, Yu. V., Electric double layer on semiconductor electrode, CTE, 1, 291 (1980). Samec, Z., The electrical double layer at the interface of two immiscible electrolyte solutions, Chem. Revs, 88, 617 (1988). Spaarnay, M. J., see page 203. Vanysek, P., see page 191. Verwey, E. J. W., and J. Th. G. Overbeek, Theory of the Stability of Lyophobic Colloids, Elsevier, Amsterdam, 1948.
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5 Processes in Heterogeneous Electrochemical Systems
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In the case of electrodes with low overpotential the process of molecular hydrogen evolution is particularly more complicated than with electrodes showing high overpotential where a single assumption of slow discharge step could successfully elucidate all experimental results. It can be taken for sure, however, that in the case of electrodes with low overpotential it is necessary to consider, as a slow step, the process of removal of molecular hydrogen from the electrode together with the discharge process. A. N. Frumkin, V. S. Bagotzky, and Z. A. Iofa, 1952 5.1 Basic Concepts and Definitions
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This chapter will be concerned with the kinetics of charge transfer across an electrically charged interface and the transport and chemical processes accompanying this phenomenon. Processes at membranes that often have analogous features will be considered in 6. The interface that is most often studied is that between an electronically conductive phase (mostly a metal electrode) and an electrolyte, and thus these systems will be dealt with first. A system consisting of two electrodes in an electrolyte medium is called an electrolytic cell. It should be realized here that there is no basic difference between the concepts of a 'galvanic cell' and an 'electrolytic cell'. In common usage, the term 'galvanic cell' is understood to refer to a system in the absence of current flow (it can be at equilibrium, as mentioned in the previous chapter, or only in a steady state, as will be demonstrated in Section 5.8.4 on mixed potentials) or to a system that yields electric work to its surroundings; an 'electrolytic cell' is then a system receiving energy from its surroundings to carry out the required chemical conversions. In fact, however, a given system sometimes can have both functions depending on the electrical potential difference between the electrodes. If an electrode reaction at a given electrode results in the transfer of a positive electric charge from the electrolyte to the electrode material or a negative charge from the electrode material to the electrolyte, then the corresponding current is defined as cathodic (/c) and the process is termed a
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246 cathodic reaction or reduction. In the opposite case, the current is termed anodic (/a) and the process is an anodic reaction or oxidation. The terms cathode and anode have already been defined in Section 1.1.1. For example, in a Daniel cell (see Section 3.1.4), the cathode is the copper electrode when the cell carries out work; if the applied voltage is greater than the equilibrium value, current flows in the opposite direction and the cathode becomes the zinc electrode at which zinc ions are reduced. According to the IUPAC convention, anodic current is considered to be positive and cathodic current to be negative. Generally, an electrode that is macroscopically characterized by a smooth surface actually contains many steps and other microscopic irregularities. The real (physical) electrode surface Ar is thus mostly larger than the geometric (macroscopic) surface Ag. The current density is usually defined as the current divided by the geometric surface area. The ratio of the real and geometric surface areas is termed the roughness factor, / R = AT/Ag. The physical and geometric surface areas are identical at mercury and other liquid electrodes. The flow of electric current through the electrolytic cell is connected with chemical, electrochemical and physical processes which, as a whole, are termed the electrode process. The main electrochemical step in the electrode process is the actual exchange of charged species between the electrode and the electrolyte, which will be termed the electrode reaction (charge transfer reaction). Substances participating directly in the charge transfer reaction are termed electroactive. These substances can be either soluble or insoluble in the electrolyte or electrode material. Common basic types of electrode reactions are as follows: 1. Reduction processes where the electrode is the cathode: (a) Reduction of ions or complexes to a lower oxidation state, the reduction of inorganic or organic molecules; the reduced form remains in solution. (b) Deposition of ions or complexes on the electrode with formation of a metallic or gaseous phase or of an amalgam. (c) Reduction of insoluble compounds or surface films with formation of a metal phase or an amalgam or an insoluble phase with different composition. 2. Oxidation processes in which the electrode is an anode: (a) Oxidation of ions, complexes or molecules to a soluble higher oxidation state. (b) Oxidation of the electrode material with formation of soluble ions or complexes. (c) Oxidation of the electrode material with formation of insoluble anodic films or oxidation of insoluble films or other insoluble substance to form insoluble substances with a higher oxidation state. Of these electrode reactions, two one oxidation and one reduction
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form a pair in a reversible charge transfer reaction (e.g. the deposition of metal ions with subsequent amalgam formation and ionization of the amalgam with formation of metal ions in solution). A more fundamental classification considers the character of the charge transfer between the electrode and the electroactive substance: 1. The transfer of electrons or holes between the electrode and the electroactive substance present in solution. 2. Transfer of metal ions from the electrolyte into the electrode and vice versa. 3. Emission of electrons from the electrode into the solution with formation of solvated electrons and the subsequent reaction between the solvated electrons and the electron 'scavenger' in solution. These processes have various characteristic properties when they occur at metallic or semiconductor electrodes and if they occur between partners (electroactive substances or electrons or holes in the electrode) that are in the ground or the excited state. The basic condition for electron transfer in cathodic processes (reduction) to an electroactive substance is that this substance (Ox) be an electron acceptor. It must thus have an unoccupied energy level that can accept an electron from the electrode. The corresponding donor energy level in the electrode must have approximately the same energy as the unoccupied level in the substance Ox. On the other hand, in oxidation processes, the electroactive substance Red must have the character of an electron donor. It must contain an occupied level with energy corresponding to that of some unoccupied level in the electrode. Oxidation occurs through transfer of electrons from the electroactive substance to the electrode or through the transfer of holes from the electrode to the electroactive substance. Thus, an electrode redox reaction occurs according to the scheme Red + unoccupied level * Ox + occupied level (5.1.1) This situation is depicted in Fig. 5.1. The occupied level in the substance Red2 has an energy corresponding to the unoccupied level in the electrode. Thus, oxidation can occur (either through the transfer of an electron e~ to the electrode or of a hole h + from the electrode). On the other hand, the unoccupied level in the substance Oxx has too high an energy, so that it does not correspond to any of the occupied levels in the electrode as all these levels lie below the Fermi level F, while the energy of the unoccupied level of the substance Oxt is far above this level. Reduction can thus not occur. The situation is the opposite for the substances Red2 and Ox2. As was demonstrated in Section 3.1.2, the energy of the Fermi level is identical with the electrochemical potential of an electron in the metal. A change in the inner potential of the electrode phase by A(p (attained by changing the potential difference of an external voltage source by AE =
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