Abstract: | A new model of molecular scale microcapsule named “super microcapsule” (SMC) obtained from a star copolymer consisting of hydrophilic and hydrophobic blocks was presented. As a first stage, 3 and 4-arm star polyethylene oxide-polylactide copolymers (s-PEO-PLA) were synthesized by the use of triethanolamine and pentaerythritol and initiating agent, respectively. The block length of PLA and PEO for the copolymers can be controlled by feed and reaction conditions. The molecular weight distributions found to be in the range of 1.3–1.7. The DTA data indicated that the phase separation behavior of s-PEO? PLA copolymers is different from that of linear PEO? PLA copolymers with comparable block length. As a evidence of SMC, the shell-core structure of s-PEO? PLA copolymers in solid state was observed by TEM. The SMC dimensions were estimated to be about 400–1000 Å |