New multiblock copolymers based on dimethylsiloxanes and phenylene diacrylate derivatives have been prepared by hydrosilation polymerization. Copolymerization was performed using either low molecular weight monomers or high molecular weight macromers. The organic macromer was prepared by acyclic diene metathesis (ADMET) polymerization of para‐phenylenediacrylic acid dipent‐4‐enyl ester. Hexamethyltrisiloxane and α,ω‐bishydride‐terminated polydimethylsiloxane (PDMS) were used as inorganic macromers. The copolymers show microphase separation of the soft siloxane block and the hard semicrystalline organic block, as observed by differential scanning calorimetry (DSC), X‐ray scattering experiments (SAXS and WAXS) and transmission electron microscopy (TEM). The crosslinking rate upon UV‐irradiation is slightly higher for the microphase‐separated copolymer than for the corresponding homopolymer. When films of the polyester‐PDMS multiblock copolymers were irradiated with linearly polarized light, optically anisotropic films were obtained with a polarizing efficiency of 67%, whereas the crosslinked films of the homopolymer had a polarizing efficiency of at most 43%.
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