The high-intensity ultrasound was applied to the preparation of nanocomposite of polyaniline (PANI) and gamma-zirconium phosphate (gamma-ZrP) by intercalation of aniline into gamma-ZrP. The intercalation rate was enhanced greatly and the interlayer distance of aniline-intercalated gamma-ZrP was determined to be 16.0 Angstrom. The intercalated aniline polymerized at low pH during the sonication by initiator (NH4)(2)S2O8 and nanocomposite of exfoliation of gamma-ZrP in PANI bulk was obtained. The intercalated or exfoliated compounds were characterized by XRD, FTIR, TEM, UV-Vis spectrum, and TG-DTA. (C) 2003 Elsevier Ltd. All rights reserved.