Nanostructured materials have potential technological applications due to their characteristic dimensions. The material performance will depend on the atomic structure, and composition of these materials. This thesis focuses on proposing a reliable method for fabricating nanoporous alumina and palladium nanoparticles inside the templates.Palladium nanoparticles were synthesized in commercial porous alumina templates using electrodeposition. Pores within these nanoporous membranes act as templates for the synthesis of nanostructures of the desired material. Electrodeposition is achieved using a three-terminal set-up and a potentiostat. Different types of deposition techniques were investigated to improve the distribution of the deposit. The nanoparticles were characterized by SEM/EDX for composition. The commercial templates have high aspect ratio, but are not hexagonally ordered. Hence porous alumina was fabricated in the laboratory by anodization of aluminum.