The synthesis of polyaniline (PANI) and its composites with transition metals like Cu and polyvinyl alcohol (PVA) was carried out by the chemical oxidative polymerization and inverse emulsion polymerization method of aniline. The samples were characterized by UV/Vis, FT-IR, XPS, NEXAFS, and SSNMR. Elemental analysis was carried out to calculate the composition of products. SEM images were taken to study the morphology of PANI and its composites. TGA and XRD data was collected to study the thermal properties and crystallinity of the resulting PANI and its composites. Cyclic voltammetry and conductivity measurement were carried out to check the electro activity and conductivity of PANI and its composites. The UV/Vis, FT-IR, XPS, NEXAFS and SSNMR and elemental analysis showed that polyaniline was formed in a partially oxidized form, partially protonated, and doped with [CuCl3] - as the counter ion. Low concentration of weak oxidant results in the formation of leucoemeraldine form of PANI. SEM results show the spherical morphology of PANI particles doped with [CuCl3] -. In case of co-composites of PANI with PVA and copper a smooth morphology was observed from the SEM images as compared to the irregular morphology of PANI-PVA and PANI-Cu obtained by inverse emulsion polymerization. The X RD and TGA confirm the amorphous nature and an improved thermal stability of composites. CV analysis shows that PANI and its composites are electro active. The composites of PANI have better conductivity in comparison to PANI as shown by conductivity measurement.