Post-process thermal treatment of electrospun fibers obtained from poly(ethylene oxide) (PEO) water and methanol solutions was examined. PEO fibers from methanol solution showed larger diameters as observed by scanning electron microscopy. Fibers both from water and methanol solutions exhibited a significant dimensional stability and surface cracking during the specific exposure time after thermal treatments at 40, 50, and 60 °C. Changes in crystallinity after the thermal treatment were studied by wide-angle X-ray diffraction. The kinetics of secondary crystallization were positively influenced by the as-processed level of the amorphous phase and temperature of thermal treatment. Samples treated at 60 °C were degraded by thermooxidation within the time.
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