A novel ternary nano composite of poly (3-4 ethylenedioxidethiophene)/nickel oxide/Flyashcenosphere (PEDOT/NiO/FAC) was synthesized. The prepared ternary nano composites were characterized using Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Powder X-Ray Diffraction (XRD), X-Ray Photoelectron Spectroscopy (XPS) and photo-catalytic degradation. XRD, TEM and SEM results suggested interaction between all the components and formation of the composite. XRD result showed the characteristic peak of PEDOT and FAC at 2 circle minus similar to 26.03 and 26.24 respectively. TEM indicated that synthesized NiO nanogranules and PEDOT have a size of 56.43 nm and 156.9 nm respectively. The XPS curve indicated that Ni was present in Ni2+ and slightly in Ni3+ form at binding energy 852.2 and 869.6 ev respectively and O in NiO was present in O2- at binding energy of 531.2 ev. The composites were used to study the photo-degradation of methyl orange involving azo group (N=N). Photo-catalytic degradation showed that 2% PEDOT/NiO/FAC composites have the highest degradation of dye under visible light with first order rate constant (k) value of 0.0042min(-1). (C) 2016 Elsevier B.V. All rights reserved.