Polyacetylene films were synthesized using homogeneous catalytic systems based on Ti(O-C4H9)4, Al(C22H5)3, poly(iso-butylalumoxanes) (MM = 470, 900) and poly(ethylalumoxane) (MM = 560). The physicochemical characteristics of these films were studied with IR spectroscopy, 2-mm ESR, cyclic voltammetry, and conductometry. Polyacetylene synthesized using Ti(O-C4H9)4- poly(isobutylalumoxane) (MM = 900) catalyst has a higher density, a lower rate of oxidation and ageing, and more stable electric properties after six months of storage in argon at 0 oC