This study covers the synthesis of conducting poly-indole (PIN) homopolymer, poly(vinyl chloride)/polyindole (PVC/PIN) composites, and preparation of their freestanding films. PIN and composites were synthesized chemically by radicalic mechanism using FeCl3 as an initiator. Films of PVC and PVC/PIN composites were prepared by casting on glass Petri dishes. Mechanical properties of films were examined by stress-strain experiments. From FTIR spectra of polymers, it was revealed that polymerization reaction occurred by 2-3 mechanism. The conductivities of polymers at different temperatures were also measured by four-probe technique and found in the range 10(-4) to 10(-5) S cm(-1). Magnetic properties of the polymers were analyzed by Gouy scale measurements and were found that their conducting mechanisms are of polaron and bipolaron natures. Thermal properties of polymers were investigated by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) and found that they had shown adequate thermal stability. X-ray diffraction (XRD) spectra showed the amorphous nature of the polymers. Scanning electron microscopy (SEM) was used for microstructural analysis. (C) 2010 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 48: 1290-1298, 2010