The crystallization and subsequent melting behaviors of water inside different annealed PVA films were performed on a calorimeter (PE DSC8000) under nitrogen atmosphere at a cooling/heating rate of 20.0°C/min. The heat flow and temperature were calibrated by pure indium before the experiments. To avoid the influence of free water on the PVA film surface, the shells of the PVA films were peeled off, leaving the core for testing. The relative amount of bulk-like water (fb) can be calculated as Wm,bWm,a+Wm,b=ΔHm,bΔHm,a+ΔHm,b, where W is the amount of water and ΔH is the enthalpy of ice melting.

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