Copolymer microtubes composed of aniline and o-toluidine were prepared through the synthesis of the desired polymer within the pores of a microporous anodic aluminum oxide (AAO) template. Scanning electron microscopy and transmission electron microscopy revealed that the obtained copolymer microtubes had uniform and well-aligned arrays, and the aspect ratios of the AAO membranes could be controlled through their diameter and length. Infrared spectrometry and X-ray photoelectron spectroscopy supported the surface analysis for the microtubes and also proved the formation of copolymers. Ultraviolet-visible/ near-infrared spectra proved that the doping effect decreased with an increase of o-toluidine in the copolymers, but the solubility greatly improved (up to 3.83 g/L in N,N-dimethylformamide), and the conductivity was as high as approximately 17.4 S cm(-1). (c) 2005 Wiley Periodicals, Inc.