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Fig. 5.26 Beer-De Nora dimensionally stable electrode with a RuO2-TiO2 layer
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313 were rapidly 'burnt' by evolved O2 and Cl2, and thus the cathode-anode spacing gradually increased, which caused an unwanted increase of voltage during prolonged electrolysis. Carbon. The electronically conductive carbons are derived from the hexagonal crystalline modification graphite. (Note: Electronic conductivity, and even superconductivity at ca. 10 K, was observed with a new carbon polymorph, buckminsterfullerene, synthesized in 1990. Electrochemical and photoelectrochemical properties of a semiconducting diamond electrode were studied by Pleskov.) Graphite is a thermodynamically stable form of elemental carbon below approximately 2600 K at 102MPa; its crystallographic description is D ^ P63/mmc, unit cell constants: a{) = 245.6 pm, co = 670.8 pm. It shows a marked anisotropy of electronic conductivity: in the c-direction around 1 S/cm (increasing with temperature as with semiconductors), but in the a-direction around 105S/cm (decreasing with temperature as with metals). The latter value can further be increased to a 106 S/cm level by intercalation with AsF5 or SbF5 (see the discussion of intercalation compounds below). At least one of the graphite intercalation compounds (C8K) is a superconductor at low temperature. Large single crystals of graphite are rare; therefore, graphite is employed in polycrystalline form (solid blocks, paste electrodes, suspensions, etc.). Nevertheless, some carbons prepared by chemical vapour deposition (pyrolytic carbons) match the properties of a graphite single crystal. The supported layer of pyroiytic graphite is actually polycrystalline, but the individual crystallites show a high degree of preferred orientation with carbon hexagons parallel to the surface of the substrate. This is especially true with the so-called highly oriented pyrolytic graphite (HOPG), prepared from ordinary pyrolytic graphite by heat treatment under simultaneous compressive stress (stress annealing) around 3500 C. A HOPG contains well-ordered crystallites, whose angular scatter is typically less than 1 . The faces parallel to the plane of carbon hexagons (100), also called basal planes, show chemical and electrochemical properties significantly different from those of the perpendicular (edge) planes (110). The latter contain unsaturated carbon atoms (dangling bonds), which are highly active, for example, against oxidation with oxygen, both chemical and electrochemical. The structure of thus formed surface oxides on carbons is very complex, but it can be derived from the common oxygen functional groups known from organic chemistry: carboxyl, hydroxyl, and carbonyl. These occur on the oxidized carbon surface either individually or in various combinations: surface anhydride, ether, lactone, etc. (see Fig. 5.27). Surface carbonyls (quinones) are reversibly reducible; further anodic oxidation of graphite and carbons occurs through intermediates such as mellithic acid to finally give CO2. The basal plane of graphite (or HOPG) is essentially free from surface oxygen functionalities. This is manifested by almost flat, featureless
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Fig. 5.27 Oxygen functional groups on the edge plane of graphite
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voltammetric curves in aqueous electrolytes, and relatively low charging currents. Unlike platinum, the basal plane HOPG virtually does not adsorb anions and most organic substances. Some molecules, such as phtalocyanines or porphyrines, form, however, n-n complexes with graphite, and are thus strongly adsorbed, being oriented parallel to the basal plane. The most popular carbon material for electrochemistry is probably the glass-like carbon. (This term is preferable to the common names 'glassy carbon' and 'vitreous carbon', which are actually trade marks and should not be used as terms.) Glass-like carbon is prepared by pyrolysis of suitable polymers, e.g. polyfurfurylalcohol or phenolic resins. If the heating programme is properly controlled, the gaseous by-products of pyrolysis evolve sufficiently slowly and the final product is a monolithic, hard carbon, showing very low porosity and permeability to liquids and gases. Glass-like carbon is, in contrast to graphite, isotropic in electrical conductivity and other physico-chemical properties. This explains its structure, characterized by randomly oriented strips (lamellae) of pseudographitic layers of carbon hexagons. The lamellae occasionally approach the graphitic interlayer spacing (335 pm), forming extremely small graphitic regions with crystalline dimensions L a , Lc of the order of 1-10 nm. These regions are interconnected by a non-graphitic carbon material as shown in Fig. 5.28. A similar three-dimensional network of graphitic microcrystallites can also be found in other forms of 'amorphous' carbon, and, according to the forces needed for breaking the network crosslinks (orientation of crystallites), we can classify almost all the solid carbons as hard (nongraphitizable) and soft (graphitizable) ones. Most polycrystalline carbons, including glass-like carbon, show an increase of electrical conductivity with increasing temperature; they can be regarded as intrinsic semiconductors with a band-gap energy of several tens to hundreds meV.
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