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A series of poly (dimethylsiloxane) -b- poly- {2,5-bis[(4-methoxyphenyl)-oxycarbonyl]styrene}(PDMS-b-PMPCS) were synthesized1 to detect the glass transition temperature of coil-like polymer (PDMS) confined in rod-coil diblock copolymer (PDMS-b-PMPCS).The PDMS-b-PMPCS form different microphase separation structure like lamellar structure (LAM),double gyriod structure (GYR) based on different composition and annealing temperature,according to the SAXS experiment at the synchrotron radiation facility.