Carbazole was electrochemically synthesized on carbon fiber microelectrodes (CFMEs) in different electrolyte and solvent media. The characterization of polycarbazole thin films formed on micron sized carbon fiber electrodes was performed by electrochemical methods (i.e., cyclic voltammetric measurements, solid state conductivity measurements (four point probe), spectrophotometric methods (ultraviolet/visible spectroscopy (UV-vis), ex situ spectroelectrochemistry, fourier transform infrared reflectance spectroscopy (FTIR-ATR)) and scanning electron microscopy (SEM). The best electrolyte and solvent in regards to yield, conductivity and charge for the electrografting was sodium perchlorate in acetonitrile, whose conductivity was 3.60 mS cm )1 , had a yield of 89% and had a charge of 5.50C. The effects of scan rate, feed ratio, supporting electrolyte and solvent type on the electropolymerization are discussed.