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(10,11,. . ,). Intercalation of some guest species, such as alkali metals, can simply be performed via a chemical reaction of a gaseous reactant with graphite. Some other guest species (e.g. H2SO4, HC1O4 and other inorganic acids), however, do not react spontaneously with graphite, but the intercalation can be induced by an auxiliary oxidizing or reducing agent. The redox reaction promo ting intercalation can also be performed electrochemically; the advantage of electrochemical intercalation is not only the absence of any foreign chemical agent and the corresponding reaction by-products, but also a precise control of potential, charge and kinetics of the process. The electrochemical intercalation into graphite leads in the most simple case to binary compounds (graphite salts) according to the schematic equations: Cn + M + + e"-> M + C~ Cn + A - - e ^ C A (5.5.30) (5.5.31)
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In the first case, the graphite lattice is negatively charged and the electrolyte cations, M + (alkali metals, N R | , etc.) compensate this charge by being inserted between the graphene layers. In the second case, anions, A" (CIOJ, AsF^, BF4", etc.) are analogously inserted to compensate the positive charge of the graphite host. Reactions (5.5.30) and (5.5.31) proceed prevailingly during intercalation from solid or polymer electrolytes (cf. Section 2.6) or melts. When using common liquid electrolyte solutions, a co-insertion of solvent molecules (and/or intercalation of solvated ions) very often occurs. The usual products of electrochemical intercalation are therefore ternary compounds of a general composition: M+(Solv)>;Cor C(Solv) y A~
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The electrochemical intercalation of HSO4 anions together with H2SO4 was described by Thiele in 1934. The composition of the product of prolonged anodic oxidation of graphite in concentrated sulphuric acid is
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318 and it is the stage 1 intercalation compound. By a very rapid heating of this compound, the intercalate vaporizes and forces the graphene layers apart, like in an accordion. The product is called exfoliated graphite', it exhibits various peculiar properties, for example, up to hundred times smaller density than graphite. It is used, for example, in the preparation of graphite foils. The electrochemical intercalation/insertion has not only a preparative significance, but appears equally useful for charge storage devices, such as electrochemical power sources and capacitors. For this purpose, the co-insertion of solvent molecules is undesired, since it limits the accessible specific faradaic capacity. The electrochemical intercalation/insertion is not a special property of graphite. It is apparent also with many other host/guest pairs, provided that the host lattice is a thermodynamically or kinetically stable system of interconnected vacant lattice sites for transport and location of guest species. Particularly useful are host lattices of inorganic oxides and sulphides with layer or chain-type structures. Figure 5.30 presents an example of the cathodic insertion of Li+ into the TiS2 host lattice, which is practically important in lithium batteries. The concept of electrochemical intercalation/insertion of guest ions into the host material is further used in connection with redox processes in electronically conductive polymers (polyacetylene, polypyrrole, etc., see below). The product of the electrochemical insertion reaction should also be an electrical conductor. The latter condition is sometimes by-passed, in systems where the non-conducting host material (e.g. fluorographite) is finely mixed with a conductive binder. All the mentioned host materials (graphite, oxides, sulphides, polymers, fluorographite) are studied as prospective cathodic materials for Li batteries. From this point of view, fluorographite, (CF^)^ with J C ^ I , deserves
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Fig. 5.30 Insertion of Li+ between TiS2 host layers. (According to C. A. Vincent et aL)
319 special attention. It is a covalent non-conductive compound whose structure is characterized by parallel planes of sp3 carbon atoms in trans-linked perfluorinated cyclohexane chairs. The electrochemical reduction of fluorographite in a lithium cell was originally considered as a simple defluorination with the formation of LiF and elemental carbon. Further studies revealed, however, that the primary process, controlling the discharge rate and the cell voltage, is an electrochemical Li+ intercalation between the layers in the fluorographite lattice. A typical product of this reaction is a ternary intercalation compound containing the co-inserted solvent molecules, Solv: The electrochemical properties of fluorographite are also interesting in connection with the electrolysis of melted KF-2HF, which is used for industrial production of fluorine. Fluorine is here evolved at the carbon anode, which is spontaneously covered with a passivating layer of fluorographite; hence it causes an undesired energy loss during the electrolysis. Chemically modified electrodes. Chemical and/or electrochemical surface pretreatments are always needed in order to get reproducible data on solid electrodes (see page 307); they are mostly focused on the removal of surface impurities (oxides). The 'activation' of solid electrodes by (electro)chemical pretreatment is, however, a complex and not well understood process. For instance, recent studies by scanning tunnelling microscopy demonstrated that the common pretreatment of a platinum electrode by a series of cyclic voltammetric pulses in the potential range of H 2 /O 2 evolution (see page 307) cannot simply be regarded as chemical 'purification' from adsorbed species, since it is accompanied with marked changes in surface topography. A qualitatively new approach to the surface pretreatment of solid electrodes is their chemical modification, which means a controlled attachment of suitable redox-active molecules to the electrode surface. The anchored surface molecules act as charge mediators between the elctrode and a substance in the electrolyte. A great effort in this respect was triggered in 1975 when Miller et al. attached the optically active methylester of phenylalanine by covalent bonding to a carbon electrode via the surface oxygen functionalities (cf. Fig. 5.27). Thus prepared, so-called 'chiral electrode' showed stereospecific reduction of 4-acetylpyridine and ethylphenylglyoxylate (but the product actually contained only a slight excess of one enantiomer). A large selection of chemical modifications employing the surface oxygen groups on carbon and other electrode materials (metals, semiconductors, oxides) has been presented. For instance, surfaces with a high concentration of OH groups (typically SnO2 and other oxides) are modified by organosilanes: [S] OH + Cl SiR3- [S] O SiR3 (5.5.32)
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320 where [S] stands for electrode surface, and the radical R might bear various electroactive species, such as ferrocene, viologenes, porphyrins, etc. Surfaces with OH groups can also be modified via l,3,5-trichloro-2,4,6-triazine as a coupling agent. This further reacts with alcohols, amines, Grignard reagents, etc. Another method employes the surface carboxylic groups on carbon electrodes, usually activated by conversion to acylchloride with SOC12, followed by esterification or amidization in order to anchor the desired electroactive species. In an ideal case the electroactive mediator is attached in a monolayer coverage to a flat surface. The immobilized redox couple shows a significantly different electrochemical behaviour in comparison with that transported to the electrode by diffusion from the electrolyte. For instance, the reversible charge transfer reaction of an immobilized mediator is characterized by a symmetrical cyclic voltammogram ( p c - E pa = 0; ypa = ~7pc= l/pl) depicted in Fig. 5.31. The peak current density, / p , is directly proportional to the potential sweep rate, v\ jp = n2F2Tv/ART (5.5.33)
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where T is the surface coverage of electroactive species, which might simply be determined from the voltammetric charge per unit electrode area (area of the peak, see Fig. 5.31): T=Q/nF (5.5.34)
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or, alternatively, by non-electrochemical techniques of surface analysis (Section 5.5.6). Besides the charge transfer reactions of the immobilized mediator, the
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