The effect of sonication on the size and structure of polymeric aggregates formed by amphiphilic block copolymers was studied by the combination of dynamic and static light scattering. Poly(ethylene oxide)‐block‐polyisoprene, poly(ethylene oxide)‐block‐polystyrene diblock copolymers, and poly(ethylene oxide)‐block‐polyisoprene‐block‐poly(ethylene oxide) triblock copolymer were used as typical polymeric amphiphiles. Sonication was found to be an effective method to break up inter‐micellar associations and split large polymeric aggregates, present initially in the aqueous solutions, into monodisperse micelles. The content and type of hydrophobic block, copolymer solution‐preparation protocol, and copolymer concentration were also investigated as co‐factors in conjunction to the effect of sonication time.magnified image