Differential scanning calorimetry, optical microscopy, and infrared spectroscopy were performed to characterize poly(ε-caprolactone) (PCL)/poly(benzyl methacrylate) (PBzMA) blend of full compositions. The binary polymer mixture of all compositions forms a true miscible blend with a homogeneous phase structure attributed to matched polarity. The thermal transition behavior suggests that the intermolecular interactions between the pairs are likely non-specific and only comparable with those among the homopolymer molecules. The FT-IR results infers that inter-molecular mixing in segmental scales does exist, although the segmental scales are not particularly fine and some minor homomolecular aggregation might be present. It is concluded that the blend phase behavior is miscibility with non-specific, mostly being of a matched polarity, intermolecular interactions. Upon heating, phase separation occurs via a binodal nucleation & growth (NG) mechanism at above 240 °C. The phase separation phenomenon is attributed to a cause of thermodynamic lower critical solution temperature (LCST) behavior. Upon cooling at regularly reasonable rates, phase separation could be reversed back to original homogeneity of miscibility.
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