We report here on the formation of hybrid compound block copolymer micelles encapsulating gold nanoparticles, utilizing a direct and general preparation method. The giant hybrid compound micelles are structured with micelles of PS‐b‐P2VP with gold nanoparticles in their P2VP core and PI‐b‐PS chains as the outer part of the compound micelles. The gold nanoparticles were produced using gold ion‐loaded PS‐b‐P2VP micelles as a nanoreactor, in a PS selective solvent (toluene), by the subsequent reduction of gold ions. The synthesis of the gold nanoparticles was monitored by UV‐vis spectroscopy. The gold containing micelles were then encapsulated in larger micelles of PI‐b‐PS copolymer, by successive utilization of toluene and heptane with the intermediate evaporation of toluene. The nanoassembly of the compound materials comprised a PI corona and a PS compound core, with P2VP/Au0 domains, and was characterized using UV‐vis spectroscopy, dynamic light scattering and transmission electron microscopy.
