A series of novel amphiphilic triblock poly(ethylene glycol) -b-poly(2-aminoethyl methacrylate hydrochloride)-b-poly(heptadeca-fluorodecyl acrylate) (PEG-b-PAEMA-b-PHFDA) comprised of two hydrophilic PEG and PAEMA segments and one hydrophobic PHFDA segment was designed and synthesized. The structure of the triblock copolymer was characterized by H-1-NMR and GPC analysis. The amphiphilic triblock copolymer was capable of self-assembling into liquid-filled micelles that consisted of PHFDA and liquid perfluorocarbons (PFCs) as the core and PEG as outer shell. PAEMA can be used as cross-linking sites to increase the stability of the liquid-filled micelles. The shape, size, and Acoustic properties of the obtained liquid-filled micelles were investigated. (C) 2009 Wiley Periodicals, Inc. J Appl Polym Sci 114: 3472-3478, 2009