The research work was focused on the exploration of basic principles behind the micelles transformation during the BCPs (block copolymers) self-assembly process, the fabrication of hybrid organic/inorganic nanostructures based on the BCP self-assembly, and the development of a general methodology for the preparation of metal nanoshell on the surface of hybrid nanostructures. These works were based on the study of self-assembly of amphiphilic BCP in mixed solvents. Specifically, self-assembling of BCPs in mixed solvent can form various morphologies in solution, including spheres, cylinders, discs, vesicles, et al. When inorganic nanoparticles were introduced into this system, hybrid organic/inorganic nanostructures with specific morphologies could be achieved. Besides, more complicated hybrid nanostructures containing metal core, polymer shell (the first layer) and metal nanoshell (the second layer) were synthesized using a general method.