AbstractMuch of the unique thermomechanical behavior of microphase‐separated block copolymers is well established for the diblock and triblock architectures, and most of the data base involves polymers with polystyrene and polydiene blocks. However, there have been few reports about phase‐separated multiblocks composed of polysiloxane blocks and polyimide blocks. Here, using various facets of electron microscopy, we have characterized the domain sizes and elemental composition of these copolymers.In situresponses to both thermal annealing and tensile strain have been examined as well. To suggest possible structure‐property relationships, differential scanning calorimetry and rheological tests have also been conducted. Measurements are reported for glass‐transition and decomposition temperatures, linear viscoelastic properties (storage and loss moduli), and nonlinear stress‐strain tensile p
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