A series of nanocomposites between aniline and vinyl acetate were synthesized chemically by an oxidative polymerization and inverse emulsion polymerization by using different solutions and oxidants such as ammonium persulfate/potassium iodate and potassium permanganate/benzoyl peroxide in the presence of various surfactants such as sodium dodecylbenzenesulfonate, poly(vinyl alcohol) and hydroxypropylcellulose, respectively. The products were characterized in terms of conductivity, morphology, particle size, conversion of monomers to polymer and molecular structure. The results show that the morphology, particle size and electrical conductivity of products are dependent on the type of surfactant and solution and the arrangement of monomer injection. The molecular structure of the product was studied by Fourier transform infrared spectroscopy.