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A simple bottom-up method for the preparation of novel and very efficient photocatalytic nanocomposite system based on carbonized form of polyaniline (PANI) and colloidal TiO2 nanocrystals has been developed. The carbonized PANI/TiO2 nanocomposites were synthesized in a two-step procedure. Firstly, non-carbonized PANI/TiO2 nanocomposites were synthesized by the chemical oxidative polymerization of aniline (ANI) with ammonium peroxydisulfate, in the presence of colloidal TiO2 nanoparticles (TiO2 NPs) (d ∼ 4.5 nm). Initial [TiO2]/[ANI] mole ratios were 20, 50, and 80. In the second step, following the polymerization process, the carbonization of PANI/TiO2 nanocomposites was performed by thermal treatment in an inert atmosphere at 650 o C. The morphological and structural properties of the carbonized nanocomposites were studied using transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray powder diffraction (XRD) and Raman spectroscopy. The accomplishment of complete carbonization of PANI in PANI/TiO2 nanocomposites was confirmed by Raman spectroscopy. The appearance of anatase and rutile crystal forms in TiO2 NPs upon carbonization, with mass ratio depending on the initial molar ratio of ANI and TiO2 NPs was revealed by XRD measurements, TEM, SEM and Raman spectroscopy. The photocatalytic activities of carbonized PANI/TiO2 nanocomposites were evaluated following the photocatalytic degradation processes of Rhodamine B and Methylene blue. Carbonized PANI/TiO2 nanocomposites showed higher photocatalytic efficacy compared to bare TiO2 NPs and non-carbonized PANI/TiO2 nanocomposites. The porosity and surface structure of carbonized PANI/TiO2 nanocomposites, as well as crystalline structure of TiO2, affect photocatalytic activity of nanocomposites.

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