Palladium nanoparticles have been successfully incorporated into a porous diblock copolymer template using a novel technique. An ordered bicontinuous double gyroid phase was created from poly(isoprene)block-poly(2-vinylpyridine). The poly(isoprene) matrix of this structure was subsequently removed by ozonolysis, creating a high specific surface area material composed of a poly(2-vinylpyridine) double gyroid network texture. Palladium ions were then adsorbed and reduced within the material. Large loadings of the nanoparticles were possible. It was also possible to kinetically control the dimensions (similar to 5-10 nm) and number density of the nanoparticles. Because of the high porosity and specific surface area of the template, this technique is very promising for high-performance catalysts and other applications.