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Carbon electrodes are widely used in electrochemistry both in the laboratory and on the industrial scale. The latter includes production of aluminium, fluorine, and chlorine, organic electrosynthesis, electrochemical power sources, etc. Besides the use of graphite (carbons) as a virtually inert electode material, the electrochemical intercalation deserves special attention. This topic will be treated in the next paragraph. In spite of the high effort focused on the carbon electrochemistry, very little is known about the electrochemical preparation of carbon itself. This challenging idea appeared in the early 1970s in connection with the cathodic reduction of poly(tetrafluoroethylene) (PTFE) and some other perfluorinated polymers. The standard potential of the hypothetical reduction of PTFE to elemental carbon: (CF2)n + 2e" + 2H + -> Cn + 2HF (5.5.28) estimated from the Gibbs free energies of formation (cf. Sections 3.1.4 and 3.1.5) equals 1.00 V at 25 C. The reductive carbonization of PTFE is, therefore, thermodynamically highly favoured, and it indeed occurs at the carbon/PTFE interface in aprotic liquid or solid electrolytes. The produced elemental carbon is termed electrochemical carbon. It is reversibly dopable (reducible) under insertion of supporting electrolyte cations into the carbon skeleton.

The surface mass patterning unique to azobenzenes is a fundamentally optical process, whereby the incident light pattern is encoded in the material. In an SRG experiment, two beams are intersected at an angle 2y at the sample surface, giving rise to an SRG with period: L l 2 sin y 4:1

316 It should be emphasized that the electrochemical carbonization proceeds, in contrast to all other common carbonization reactions (pyrolysis), already at the room temperature. This fact elucidates various surprising physicochemical properties of electrochemical carbon, such as extreme chemical reactivity and adsorption capacity, time-dependent electronic conductivity and optical spectra, as well as its very peculiar structure which actually matches the structure of the starting fluorocarbon chain. The electrochemical carbon is, therefore, obtained primarily in the form of linear polymeric carbon chains (polycumulene, polyyne), generally termed carbyne. This can be schematically depicted by the reaction: F F F F F" F" F~ F"

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where l is the wavelength of the inscription light. The amplitude (height) of the SRG depends on the inscription angle, displaying a maximum at yB151 (Barrett et al., 1996; Kim et al., 1995a). Grating height increases nonlinearly with irradiation time and power, up to a saturation point (Fukuda et al., 2000a; Bian et al., 1999). At moderate uence, the grating ef ciency depends only on the net exposure, not on the temporal distribution of irradiation. Gratings can be formed with intensities as low as 1 mW/cm2, as long as the inscription wavelength

_ l _ l ( _ l( _ l _ ^ ~~^f"~ f~~ f~~(f~" * =O=C-C~C_

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(5.5.29)

WP D (b)

F F F F F" F" F" F~ The product of the reaction (5.5.29) is, however, unstable against subsequent interchain crosslinking and insertion of supporting electrolyte cations. The electrochemical carbonization of fluoropolymers was recently reviewed by L. Kavan. Insertion (intercalation) compounds. Insertion compounds are defined as products of a reversible reaction of suitable crystalline host materials with guest molecules (ions). Guests are introduced into the host lattice, whose structure is virtually intact except for a possible increase of some lattice constants. This reaction is called topotactic. A special case of topotactic insertion is reaction with host crystals possessing stacked layered structure. In this case, we speak about 'intercalation' (from the Latin verb intercalare, used originally for inserting an extra month, mensis intercalarius, into the calendar). The intercalated guest molecules have a tendency to fill up completely the particular interlayer space in the host crystal, rather than to occupy randomly distributed interstitial sites between the layers. A peculiarity of intercalation is that the sequence of filled and empty interlayer spaces is very often regular, i.e. the structure of intercalation compounds consists of stacked guest layers interspaced between a defined number of the host layers. The number of host layers corresponds to the so-called stages of intercalation compounds. Stage 1 denotes successively stacked host and guest layers, stage 2 denotes a system with two host layers between one guest layer, etc. This is schematically depicted in Fig. 5.29. Graphite crystal is the best known host material for intercalation reactions. The host layers are clearly defined by planes of carbon hexagons, also called graphene layers. (The term 'graphene' has been derived by analogy with condensed aromatic hydrocarbons: naphthalene, anthracene, tetracene, perylene, etc.). In contrast to other host materials (e.g. inorganic sulphides), graphite also forms compounds with high stage numbers

Figure 4.2. Experimental setup for the inscription of a surface relief grating: S refers to the sample, M are mirrors, D is a detector for the diffraction of the probe beam, WP is a waveplate (or generally a combination of polarizing elements), and BS is a 50% beam splitter. The probe beam is usually a HeNe (633 nm), and the inscription beam is chosen on the basis of the chromophore absorption band (often Ar+ 488 nm). (a) A simple one-beam inscription involves re ecting half of the incident beam off of a mirror adjacent to the sample. (b) A two-beam interference setup enables independent manipulation of the polarization state of the two incident beams.

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