Description:
<jats:p>The step‐wise solution self‐assembly of double crystalline organometallic poly(ferrocenyldimethylsilane)‐<jats:italic>block</jats:italic>‐poly(2‐<jats:italic>iso</jats:italic>‐propyl‐2‐oxazoline) (PFDMS‐<jats:italic>b</jats:italic>‐P<jats:italic>i</jats:italic>PrO<jats:italic>x</jats:italic>) diblock copolymers is demonstrated. Two block copolymers are obtained by copper‐catalyzed azide‐alkyne cycloaddition (CuAAC), featuring PFDMS/P<jats:italic>i</jats:italic>PrOx weight fractions of 46/54 (PFDMS<jats:sub>30</jats:sub>‐<jats:italic>b</jats:italic>‐P<jats:italic>i</jats:italic>PrOx<jats:sub>75</jats:sub>) and 30/70 (PFDMS<jats:sub>30</jats:sub>‐<jats:italic>b</jats:italic>‐P<jats:italic>i</jats:italic>PrOx<jats:sub>155</jats:sub>). Nonsolvent induced crystallization of PFDMS in acetone leads in both cases to cylindrical micelles with a PFDMS core. Afterward, the structures are transferred into water for sequential temperature‐induced crystallization of the P<jats:italic>i</jats:italic>PrOx corona, leading to hierarchical double crystalline superstructures, which are investigated using scanning electron microscopy, wide angle X‐ray scattering, and differential scanning calorimetry.
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