L. Kavan et al., ELECTROCHEMICAL CARBYNE FROM PERFLUORINATED HYDROCARBONS - SYNTHESIS AND STABILITY STUDIED BY RAMAN-SCATTERING, Carbon, 33(9), 1995, pp. 1321-1329
The synthesis of electrochemical carbyne from perfluorinated hydrocarb
ons was optimized. The relative yield of carbyne was monitored by Rama
n spectroscopy using the C=C stretching mode. The position and relativ
e intensity of this band depend on the type of fluorocarbon and reduci
ng agent used. Optimum conditions were attained for electrochemical re
duction of poly(tetrafluoroethylene) with K- or Na-amalgams. Poly(tetr
afluoroethylene) oriented by mechanical stretching gives partly orient
ed polyyne chains with a conjugation length of 16 carbon atoms. Electr
ochemical carbyne is stabilized against interchain crosslinking (graph
itization) by interspersed microcrystalline alkali metal fluoride (rea
ction byproduct). Carbyne decomposes spontaneously if the alkali metal
fluoride is extracted from the composite by leaching out with water.
The final salt-free product is a highly disordered carbon material res
embling diamond-like amorphous carbon; it graphitizes after thermal an
d pressure treatments.