Polyaniline (PANI) micro/nanostructures are synthesized by electrochemical polymerization, and characterized by field-emission scanning electron microscopy, Fourier transform infrared spectroscopy and UV-visible spectroscopy. It is revealed that the PANI microwires are produced with high yield with diameters of about 2 mm and lengths of several hundreds of micrometers, while nanostructures in the presence of PAA have diameters of about 500 nm. The micro/nanostructured PANI films are very stable and show high electrocatalytic reduction toward H 2 O 2 , which makes it an ideal substrate for H 2 O 2 detection and offers great promise for biosensing applications. Fig. 12 Amperometric response (A) of 0.5 (a), 1.0 (b), 2.0 (c), 5.0 (d) and 10 (e) mM H 2 O 2 at PANI-PAA nanowires film modified GC electrode in PBS (pH 7.0) at 0.7 V vs. SCE. Inset is the enlargement of i-t curve of PANI-PAA nanowires film modified GC electrode for 0.5 (a) and 1.0 (b) mM H 2 O 2 . (B) presents plots of current vs. H 2 O 2 concentrations. Inset is the morphology of PANI on GEC. 69072 | RSC Adv., 2015, 5, 69067-69074 This journal is