Block copolymer self-assembly provides a template for the synthesis of nanostructured inorganic materials with applications in areas such as energy materials such as solar cells and supercapacitors, catalysis, separation media, and metamaterials with unique optical and electronic properties. The incorporation of two different types of inorganic materials could enable new applications such as multifunctional catalysts and metamaterials with unforeseen properties. One limitation in the development of block copolymer-templated hybrid materials, is the relatively small library of available templates. Current research efforts are devoted to the synthesis of new block copolymers with new block chemistry and functionality. Change of mechanism polymerization provides a potential mechanism for incorporating new combinations of polymer blocks into the same template. In this dissertation, we report the synthesis of ABC triblock terpolymers with polycarbonate and polyester blocks using a combination of anionic polymerization and rapid chain-shuttling polymerization. To fabricate nanostructured inorganic materials with two different inorganic components, we synthesized and developed an ABC triblock terpolymer with orthogonal degradability. We describe the incorporation of   two different metals into a single block copolymer template using sequential polymer degradation and backfilling with inorganic materials.