Self-assembly of nanostructures obtained in a microwave-assisted oxidative polymerization of aniline

For the first time, microwave assisted aniline oxidative polymerization is performed in the presence of acetic acid (CH3COOH) and ammonium hydroxide (NH4OH) at different microwave power levels. The reaction system is kept at constant temperature of 24±1°C. The products are investigated by Fourier Transform Infrared Spectroscopy (FTIR), Raman, solid-state Nuclear Magnetic Resonance (NMR) and Electron Paramagnetic Resonance (EPR) spectroscopies. EPR signals in polyaniline (PANI) originate from the polarons formed upon protonation and doping by acid. The microwave radiation causes an increase in the spin concentration which is slightly more evident for 8 W than for 93 W. The morphol- ogy is investigated by using scanning electron microscopy (SEM). SEM micrographs revealed the formation of nanorods (in the presence of CH3COOH) and nanospheres (in the presence of NH4OH). FTIR, Raman and solid-state NMR spectro- scopies indicate the presence of PANI and aniline oligomers. X-ray Diffraction (XRD) measurements showed the presence of well-ordered structures.