Graduation date: 2008Metal/polymer nanocomposites are of increasing importance with their tunable properties being used in catalysis and sensors. Previous studies have focused on the effects of metal content, molecular weight of polymer and reaction conditions on the structure- property relationship of the metal/polymer nanocomposites. This thesis focuses on the effect of two synthetic routes, ex situ and in situ, on the structure and properties of palladium/polycarbonate (Pd/PC) nanocomposites. Discrete and agglomerated nanoclusters were obtained from ex situ and in situ methods, respectively. The effects of the varied morphology on the optical, thermal and electrical properties of the nanocomposites were studied. Dependence of the thermal stability of the nanocomposites on the heating rates, Pd content and synthetic methods was also investigated. The ex situ nanocomposites exhibited better optical transmission and thermal stability, while the in situ nanocomposites showed higher electrical conductivity. These observations lay the foundation for developing new synthetic strategies for designing new materials by varying the size, shape, concentration and distribution of metal nanoclusters in various polymer matrices. Such materials will be investigated for sensor and catalyst applications.