Abstract The formation of ABC triblock terpolymers through solution casting is still challenging. In this study, core?shell double gyroid network structures are fabricated via solution casting using poly(2,2,2-trifluoroethyl methacrylate) (PTFEMA) (F)-b-[poly(4-vinylpyridine) (P4VP) (P)]-b-[polystyrene (PS) (S)] (FPS) triblock terpolymers in N,N-dimethylformamide (DMF). Upon heat treatment, the polymer tends to form a sphere-in-lamellar structure at the F/S interface. Given the solubility properties of each component in DMF, it is anticipated that the effective volume fraction of F relative to P would increase in concentrated solutions and the effective volume fraction of S would decrease. The microphase-separated structure derived from the DMF solution consistently results in the formation of a network structure composed of a core?shell double gyroid, with F as the matrix, P as the shell, and S as the core, and their periodic lengths gradually increase to 110.8, 131.8, and 162.7ﾂ�nm as increase molecular weights of PS blocks to 13.8, 20.7, and 28.8ﾂ�kg mol?1. Based on the solubility properties of the polymer components highlighted in this study, the solvent selection strategy is broadly applicable to ABC triblock terpolymers featuring various polymer components, offering a more efficient avenue for fabricating core?shell double gyroid structures.
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