The crystallization behaviors and morphology of asymmetric crystallinecrystalline diblock copolymers poly(ethylene oxide-lactide) (PEO-b-PLLA) were investigated using differential scanning calorimetry (DSC), wide angle X-ray diffraction (WAXD), and microscopic techniques (polarized optical microscopy (POM) and atomic force microscopy (AFM)). Both blocks of PEO 5 -b-PLLA 16 can be crystallized, which was confirmed by WAXD, while PEO block in PEO 5 -b-PLLA 30 is difficult to crystallize because of the confinement induced by the high glass transition temperature and crystallization of PLLA block with the microphase separation of the block copolymer. Comparing with the crystallization and morphology of PLLA homopolymer and differences between the two copolymers, we studied the influence of PEO block and microphase separation on the crystallization and morphology of PLLA block. The boundary temperature (T b ) was observed, which distinguishes the crystallization into high-and low-temperature ranges, the growth rate and morphology were quite different between the ranges. Crystalline morphologies including banded spherulite, dendritic crystal, and dense branching in PEO 5 -b-PLLA 16 copolymer were formed. The typical morphology of dendritic crystals including two different sectors were observed in PEO 5 -b-PLLA 30 copolymer, which can be explained by secondary nucleation, chain growth direction, and phase separation between the two blocks during the crystallization process. Lozenge-shaped crystals of PLLA with screw dislocation were also observed employing AFM, but the crystalline morphology of PEO block was not observed using microscopy techniques because of its small size.

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