SYNTHESIS OF CARBYNE ANALOGS BY CATHODIC ELECTROLYSIS OF HEXACHLOROBUTADIENE

Hexachloro-1,3-butadiene was potentiostatically electrolyzed (-2.0 V v s. SCE) or galvanostatically electrolyzed (1 mA cm(-2)) with a Pt cath ode at 0 degrees C in DMF containing tetrabutylammonium perchlorate as an electrolyte, giving insoluble black fragile films deposited on the electrode. The surface morphology was globular observed by SEM. Elect rical conductivity of the pristine film obtained by the potentiostatic method was about 5 x 10(-8) S cm(-1) which increased to 5 x 10(-5) S cm(-1) by iodine doping. The as-grown film obtained by the galvanostat ic method showed an electrical conductivity of 1 x 10(-4) S cm(-1). St ructural analyses of these products by IR, Raman, XRD, ESR, NMR, and e lemental analysis data suggested that these products were carbyne anal ogues n-doped and stabilized by the electrolyte.