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A series of polyimide (PI) films with a high-temperature-induced shape memory effect and tunable properties were prepared via the facile random copolymerization of 4,4′-oxydianiline (ODA) with 4,4′-(hexafluoroisopropyl)diphthalic anhydride (6FDA) and 4,4′-oxydiphthalic anhydride (ODPA). The trigger temperature can be controlled from 294 to 326 °C by adjusting the ratio of monomers. The effects of monomer rigidity on the chain mobility, physical properties, and shape memory performance of as-prepared copolyimide were systematically investigated. The introduction of ODPA could enhance the mobility of PI macromolecular chains, which made chain entanglement more likely to occur and increased the physical crosslinking density, thereby improving the PI’s shape recovery up to 97%. Meanwhile, the existence of 6FDA enabled PI films to set quickly at low temperatures with a shape fixation of 98%. The shape memory cycling characteristics of the polyimide films are also studied, and the relationship between the PI chemical structure and the film properties are further discussed.

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