Summary: Nonlinear optical (NLO) polymers with high glass transition temperatures were prepared by the functionalization of poly(ether sulfone)s with hydroxyalkyl chromophores via the Mitsunobu reaction. Glass transition temperatures obtained were in the range of 158–212 °C. Thin spin‐coated films of the polymers were corona‐poled and analyzed by second‐harmonic generation measurements; second‐order susceptibility values (d33) up to 181 pm · V−1 were obtained. Poled‐order stability measurements over a period of 1 600 h showed that the percentage of the remaining NLO‐response at 125 °C was 84–96% under nitrogen and 54–76% in air.
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