In the first section, for the first time the layered doubled hydroxide (LDH) was the modified with an optically active and bioactive dicarboxylic acid N -tetrabromophthaloyl-glutamic to prepare modified-LDH (M-LDH). The modification was essential for improving of LDH compatibility with organic and biological environments such as polymer matrix. The process was accomplished under ultrasonic method as a fast, low cost and green way. In this work, the chiral poly(amide-imide) (PAI) was synthesized by reaction of N -trimellitylimido-L-leucine with 4,4?-diaminodiphenyl ether in the presence of triphenyl phosphite and the molten tetra-n-butylammonium bromide. In the second section to improve the thermal properties of poly(vinyl alcohol), LDH that was modified with dicarboxylic acids N -tetrabromophthaloyl-glutamic was used. Different amounts of M-LDH were used for the synthesis of PVA/M-LDH NCs via an ultrasonic irradiation technique. The properties and structures of the samples were studied by Fourier transfer infrared (FT-IR), X-ray diffraction (XRD), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA) and field emission scanning electron microscopy (FE-SEM) techniques. Due to the presence of inorganic nanolayers and strong hydrogen bonding between O–H groups of polymer and the layers of M-LDH sheets thermal properties reletively was improved.