Polyaniline-vanadium oxide nanocomposite nanosheets with thickness between 10 and 20 rim, and lateral dimensions in the range of hundreds of nanometers to several microns have been synthesized by in situ intercalation polymerization of aniline with layered V2O5 under hydrothermal conditions. The product was characterized by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, and X-ray diffractometer (XRD). The effects of the concentration of aniline and reaction temperature on the morphologies of polyaniline-vanadium oxide nanocomposites have also been investigated.