Polyimides are attractive polymers because of valued intrinsic properties such as high thermal stability and good solvent resistance. At the same time, much effort is put into modifying polyimides to introduce different properties. This thesis describes a study where polyimides were modified with soluble metal compounds in an effort to create microcomposite films in which the location of the composite structure was controlled; namely at the film interfaces. Two different modification techniques were used in this study, in-situ chemical generation and infusion deposition. Results indicate that infusion deposition was successful in producing a gradient microcomposite structure in polyimide films when silver(I)nitrate was the metal dopant. Analysis revealed that formation of the microcomposite structure depends upon the glass transition temperature and precure temperature of the polyimide film being modified. / Master of Science