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I,III(s) I(s), IJI(s) UI(s) I,H(s) I,III(s) I,III(s) I,HI(s) IJII(s) I,III(s) I,III(s)
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I indicates the Volmer mechanism (Eq. 5.7.1), II the Tafel mechanism (Eq. 5.7.2) and III the Heyrovsky mechanism (Eq. 5.7.3). The slowest step of the overall process is denoted (s).
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where m is the mass of the proton or its isotope, h is Planck's constant, (ox is the vibrational frequency of the bond between the proton and the rest of the molecule of the proton donor, cof is the vibrational frequency of the bond between the hydrogen atom and the metal and r is the proton tunnelling distance. When the hydrogen atom is weakly adsorbed, the vibrational frequency of the hydrogen-metal bond w{ is small and the proton tunnelling
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distance r is large and thus K is very small. Consequently, in the evolution of hydrogen at metals that adsorb hydrogen atoms very weakly, such as Hg, Pb, Tl, Cd, Zn, Ga and Ag, reaction (5.7.1) is the rate-controlling step. At high overpotentials, Eq. (5.3.17) is valid for the dependence of the rate constant on the potential. At lower overpotentials (at very small current densities) barrierless charge transfer occurs (see page 274), as indicated in Fig. 5.39. Distinct adsorption of hydrogen can be observed with electrodes with a lower hydrogen overpotential, such as the platinum electrode. This phenomenon can be studied by cyclic voltammetry, as shown in Fig. 5.40 for a poly crystalline electrode. The potential pulse begins at E = 0.0 V, where the electrode is covered with a layer of adsorbed hydrogen. When the potential is shifted to a more positive value, the adsorbed hydrogen is oxidized in two anodic peaks in the potential range from 0.1 to 0.4 V. At even more positive potentials, no electrode process occurs and only the current for electrode charging flows through the system. This is especially noticeable at high polarization rates. The potential range from 0.4 to 0.8 V is termed the double-layer region. At potentials of E > 0.8 V, 'adsorbed oxygen' begins to form, i.e. a surface oxide or a layer of adsorbed OH radicals. This process is characterized by a drawn-out wave. Evolution of molecular oxygen starts at a potential of 1.8 V. When the direction of polarization is reversed, the oxide layer is first gradually reduced. This process has a certain activation energy and occurs at more negative potentials than the anodic process. The reduction of oxonium ions, accompanied by adsorption, occurs at the same potentials as the opposite anodic process. If this experiment is carried out on the individual crystal faces of a single-crystal electrode (see Fig. 5.41),
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Fig. 5.39 Tafel plot of hydrogen evolution at a mercury cathode in 0.15 M HC1, 3.2 M KI electrolyte at 25 C. (According to L. I. Krishtalik)
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Fig. 5.40 Cyclic voltammogram of a bright platinum electrode in 0.5 M H2SO4. Geometrical area of the electrode 1.25 x 10~3cm2, periodical triangular potential sweep (dE/dt = 30 V s"1), temperature 20 C, the solution was bubbled with argon. (By courtesy of J. Weber)
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then the picture changes quite markedly. The shape of the voltammetric curve is also affected strongly by the procedure of annealing the electrode prior to the experiment. There are also very marked differences between the first voltammetric curve and the curve obtained after repeated pulsing. All these features are typical for electrocatalytic phenomena. It was demonstrated by R. Parsons and H. Gerischer that the adsorption energy of the hydrogen atom determines not only the rate of the Volmer reaction (5.7.1) but also the relative rates of all three reactions (5.7.1) to (5.7.3). The relative rates of these three reactions decide over the mechanism of the overall process of evolution or ionization of hydrogen and decide between possible rate-determining steps at electrodes from different materials. The effect of adsorption on the electroreduction of hydrogen ions, i.e. the Volmer reaction, is strongly affected by the potential difference in the diffuse electrical layer (Eq. 5.3.20). In the presence of iodide ions, the overpotential at a mercury electrode decreases, although the adsorption of iodide is minimal in the potential region corresponding to hydrogen evolution. The adsorption of iodide
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Fig. 5.41 A single-crystal sphere of platinum (magnification 100x). It is prepared from a Pt wire by annealing in an oxygen-hydrogen flame or by electric current and by subsequent etching. The sphere is then cut parallel to the face with a required Miller index to obtain a single-crystal electrode. (By courtesy of E. Budevski)
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retards the electrode process at other electrodes with large hydrogen overpotentials, such as the lead electrode. Hydrogen is evolved from water molecules in alkaline media at mercury and some other electrodes. As the adsorption energy increases, the rate of the Volmer reaction can increase until equilibrium is attained and the rate of the process is determined by either the Tafel or the Heyrovsky reaction. However, it is more probable for kinetic reasons that the Tafel reaction will occur at electrodes that form a moderately strong bond with adsorbed hydrogen (e.g. at platinum electrodes, at least in some cases). Electrodes that adsorb hydrogen strongly such as tungsten electrodes, are in practice completely covered with adsorbed hydrogen over a wide range of electrode potentials.
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The Tafel reaction would require breaking the adsorption bonds to two hydrogen atoms strongly bound to the electrode, while the Heyrovsky reaction requires breaking only one such bond; this reaction then determines the rate of the electrode process. The isotope effect (i.e. the difference in the rates of evolution of hydrogen from H2O and D2O) on hydrogen evolution is very important for theoretical and practical reasons. The electrolysis of a mixture of H2O and D2O is characterized, like in other separation methods, by a separation factor
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where cH/cu is the ratio of the atomic concentrations of the two isotopes. The separation factor is a function of the overpotential and of the electrode material. The reacting species are H 3 O + and H 2 DO + in solutions with low deuterium concentrations. The S values for mercury electrodes lie between 2.5 and 4, for platinum electrodes with low overpotentials between 3 and 4 and, at large overpotentials, between 7 and 8. The overpotential of hydrogen at a mercury electrode decreases sharply in the presence of readily adsorbed, weak organic bases (especially nitrogen-containing heterocyclic compounds). A peak appears on the polarization curves of these catalytic currents. The hydrogen overpotential is decreased as oxonium ions are replaced in the electrode reaction by the adsorbed cations of these compounds, BH ads + . The product of the reduction is the BHads radical. Recombination of these radicals yields molecular hydrogen and the original base. The evolution of hydrogen through this mechanism occurs more readily than through oxonium ions. The decrease in the catalytic current at negative potentials is a result of the desorption of organic compounds from the electrode surface. The electrode processes of oxygen represent a further important group of electrocatalytic processes. The reduction of oxygen to water O2 + 4H + + 4e<= 2H2O (5.7.6)
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has a standard potential determined by calculation from thermodynamic data as +1.227 V. The extremely low exchange current density prevents direct determination of this value. The simultaneous transfer of four electrons in reaction (5.7.6) is highly improbable; thus the reaction must consist of several partial processes. The non-catalytic electroreduction of oxygen at a mercury electrode will now be compared to the catalytic reduction at a silver electrode. J. Heyrovsky demonstrated that the stable intermediate in the reduction at mercury is hydrogen peroxide. Figure 5.42 depicts the voltammogram (polarographic curve) for the reduction of oxygen at a dropping mercury electrode. The first wave corresponds to the reduction of oxygen to hydrogen peroxide and the second to the reduction