The structural evolution with temperature of an anionically synthesized ABA poly(styrene‐b‐isoprene) (SIS) lamellar block copolymer (total molecular weight 45,000; isoprene content 38% by weight) was studied by melt‐rheological measurements, electron microscopy, and x‐ray and light diffraction. Above 225°C, the dynamic viscosity was found to be independent of frequency up to a critical frequency. The variation of the elastic modulus confirmed the occurence of a transition between 215 and 225°C. For the temperature range considered, all results superimposed well on a two‐branch master curve. It was concluded that above 225°C, our SIS behaves like a Newtonian material, whereas for lower temperatures and/or higher frequencies classical non‐Newtonian behavior is found. The melt‐rheological properties were explained by microscopy and diffraction investigations, which allowed us to follow morphological changes as the temperature was raised. It was found that the two‐phase lamellar structure is progressively destroyed, and the transition temperature of 225°C corresponds to the temperature above which complete mixing occurs.
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