A simple method for controlling the spatial distribution of nanoparticles in a diblock copolymer is shown. By varying the ligand functionality of the nanoparticles, as well as the processing conditions, the distribution of gold nanoparticles in the microdomains of the diblock copolymer was controlled and altered. In addition, the nanoparticles are found to affect the diblock copolymer morphologies. Thermal treatment caused a redistribution of the nanoparticles inside one microdomain.