Polypyrrole/layered niobate (PPy-Nb(6)O(17)) nanocomposite has been synthesized by the intercalation of pyrrole monomer into the layer structure of organo-modified niobate followed by the subsequent in situ polymerization of pyrrole in the interlayer spaces. The microstructure and morphology characterizations for the resulting material have been investigated by means of XRD, FTIR, and SEM. On the basis of the experimental results, the mechanism for the formation of PPy chains within the confined galleries of the inorganic host material is presented. The cyclic voltammogram of the PPy-Nb(6)O(17) nanocomposite thin film exhibits a fine diffusion-controlled electrode process, which hints the possibility of being utilized as an electrode modifying material.