Polymer based nanocomposites are classified as an important materials, which were developed in recent years. The main goals of this project are the preparation of high performance nanocomposites based on metal oxide nanoparticles (ZnO and TiO 2 ) and optically active polymers. Among the different polymers, polyamides (PA), polyimides (PI) and poly(amide-imide)s (PAI) show great interest due to the unexpected chemical and physical properties. These materials can be excellent candidates for using in nanocomposites as matrixes. The PAIs structures in this project were designed based on the diamines and diacid chlorides. The reaction of the mono amine containing compounds with 3,5-dinitrobenzoyl chloride caused to preparation of dinitro benzamide compounds. The catalytic reductions of nitro groups produced compounds 3,5-diamino- N -(4-hydroxyphenyl) benzamide(1) and 3,5-diamino- N -(3,4-dihydroxyphenethyl)benzamide(2) as diamines. The formations of diamines were confirmed by NMR in dimethy sulfoxide. The symmetric diacid chloride compounds were synthesized in two steps. In the first step, condensation reaction of dianhydride and two moles of different L -amino acids including alanine, phenylalanine, leucine, isoleucine and valine were achieved, and in the second step, reaction of prepared imide acids with thionyl chlorides caused to preparation of diacid chloride compounds. New aromatic-aliphatic PAIs with benzamide pendant substituted groups have been synthesized in one step from the condensation reaction of equimolar amounts of the diamines and diacid chlorides in DMAc as a solvent in the presence of propylene oxide as an acid scavenger at low temperature. All PAIs were obtained in high yields 78% and were characterized by common spectroscopic methods such as FT-IR, 1 H-NMR and elemental analysis. In other part of the project polymer/metal oxide nanocomposites have been prepared by introduction of nanoparticles (NP)s in polymer matrixes. For this propose, in order to increase the compatibility of nanomaterials with polymer matrixes the surfaces of were treated with silane coupling agents. The ZnO were modified with ?-methacryloxypropyltrimethoxy silane (KH570) and ?-aminopropyltriethoxysilane (KH550). Also TiO 2 were treated with KH550. Two polymeric structures based on phenyalanine (BP) and isoleucine (BI) amino acid containing linkages were selected as matrixes. Then PAI-BP/ZnO-KH550, PAI-BI/ZnO-KH550, PAI-BP/ZnO-KH570, PAI-BI/ZnO-KH570 for ZnO and PAI-BP/TiO 2 -KH550 nanocomposites (NCs) for TiO 2 were synthesized under ultrasonic process. The resulting NCs were characterized by various techniques including FT-IR, X-ray diffraction )XRD( and their morphology were iected by field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The FE-SEM and TEM results showed that, these particles have a mean diameter below than 85 nm and generally have fine edges. FE-SEM and TEM micrographs demonstrated uniform nanostructure inorganic moieties in polymeric matrix and confirmed that the metal oxide were presented in nanoscale in NCs structures. The discovery of the atomic force microscope (AFM) has offered new chances for obtaining three-dimensional high resolution images under ambient conditions to investigation of surfaces of materials like NCs structures. It appeared that with introducing the metal oxide in polymer matrix the hills of surface due to the residual of the in the surface were increased.