Poly(N,N,N-trimethyl-(2-pyrrol-1-yl)ethyl ammonium iodide)/V 2O 5(PTPAI/V 2O 5) nanocomposites were synthesized by sol-gel method. This method involved formation of vanadium pentoxide xerogel in the presence of polypyrrole derivatives solution. X-ray diffraction(XRD) indicated that the polypyrrole derivative particles encapsulated in the fibrous V 2O 5 network and the layered distance significantly increased from 1.077 39 to 1.354 56 nm. The interaction between polypyrrole and V 2O 5 in the ‘nanocomposites’ was characterized by IR spectroscopy. The Scanning Electron Microscope(SEM) micrographs reveal the structural contrasts between the hybrid materials and the pristine vanadium oxide xerogel. Poly (N, N, N-trimethyl- (2-pyrrol-1-yl) ethyl ammonium iodide / V 2 O 5 (PTPAI / V 2O 5) nanocomposites were synthesized by sol- gel method. This method involved formation of vanadium pentoxide Xerogel in the presence of polypyrrole derivative solution. X-ray diffraction (XRD) indicated that the polypyrrole derivative particles encapsulated in the fibrous V 2O 5 network and the layered distance increased increased from 1.077 39 to 1.354 56 nm. The interaction between polypyrrole and V 2O 5 in the ’nanocomposites’ was characterized by IR spectroscopy. The Scanning Electron Microscope (SEM) micrographs reveal the structural contrasts between the hybrid materials and the pristine vanadium oxide xerogel.