Poly(vinyl alcohol)/organo-clay/TiO2 nanocamposites films were prepared with 10 wt % of organo-nanoclay and various amount of TiO2 nanoparticles. Cloisite Na+ has been modified via cation exchange reaction using ammonium salt of natural L-leucine amino acid as a cationic surfactant. After that poly(vinyl alcohol)/organo-nanoclay/TiO2 nanocomposites were synthesized by dispersion of TiO2 on the surfaces of organo-nanoclay in poly(vinyl alcohol) matrix by using ultrasonic energy. Three nanocomposites with different loading of TiO2 were prepared and characterized by X-ray diffraction, fourier transform infrared spectroscopy, field emission type scanning electron microscope, scanning electron microscopy, transmission electron microscopy, thermogravimetric analysis and ultraviolet-visible transmission spectra. The results showed that the organo-nanoclay and TiO2 were dispersed homogeneously in poly(vinyl alcohol) matrix and also showed improvement in their thermal properties compared with the pure poly(vinyl alcohol).