In the present investigation, the goal was the preparation, characterization, and surface morphology of poly(amide-imide)/TiO2/oganoclay nanocomposites. At first, an optically active poly(amide-imide) was synthesized from the polymerization reaction of N-trimellitylimido-l-isoleucine diacid with 4,4′-methylenebis(3-chloro-2,6-diethylaniline). The obtained polymer and TiO2 nanoparticles were used to prepare poly(amide-imide)/TiO2 nanocomposites through ultrasonic irradiation. Then, different amounts of organoclay were added to the poly(amide-imide)/TiO2 nanocomposite system to obtain poly(amide-imide)/TiO2/oganoclay nanocomposite. The resulting hybrids materials were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, and thermogravimetric analysis techniques.