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ABSTRACT Glassy polymer nanofibers with spatially confined poly(ethylene oxide) (PEO) were fabricated by coaxial electrospinning of PEO with polyacrylonitrile (PAN) or polystyrene. The effect of melt-annealing on the crystallization behavior of the confined PEOs was studied using differential scanning calorimetry. It is found that the crystallization behavior of the confined PEOs varies with annealing temperature ( Ta), annealing time ( ta), and molecular weight of PEO. Notably, it is observed that the crystallization temperature ( Tc) and melting temperature ( Tm) of PEO increase with prolongation of ta, for PEO600K/PAN and PEO2K/PAN coaxial electrospun fibers. This phenomenon can be interpreted by the annealing-induced demixing at the core-sheath interface. After the coaxial electrospinning, the core and sheath of the PEO/PAN coaxial fibers are partially compatible due to the miscible solvents used for the core and sheath polymers. Upon annealing, demixing occurs at the core-sheath interface, leading to improved crystallizability of PEO. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018, 135, 45760. [ABSTRACT FROM AUTHOR]