Three metallosurfactants C (n) -Cu-C (n) (n = 8, 12, 16) were synthesized via two-step in this paper. All of these surfactants were characterized by ultimate analysis, H-1 NMR, FT-IR, LC-MS, elemental analysis. In addition, the three surfactants can form vesicles under sonication at a relatively high concentration, and their aggregation behavior and the stability of C (n) -Cu-C (n) vesicles were investigated by surface tension, electrical conductivity, FT-IR, negative staining-TEM. Results showed that C-12-Cu-C-12 vesicles with average size of similar to 60 nm had good stability over inorganic salt, temperature, and aging time. Doxorubicin hydrochloride was incorporated into C-12-Cu-C-12 vesicles with a remarkably high efficiency of above 70 %, and the delivery system has obvious sustained release effect.