In this paper, four new hyperbranched polytriazoles containing azo moieties, derived from different AB(2) -type monomers, were successfully prepared through the "click" chemistry reaction under copper(I) catalysis by modifying the synthetic route. The polymers were soluble in organic solvents and exhibited good second-order nonlinear optical (NLO) properties. Thanks to the self-assembly of perfluoroaromatic moieties in the periphery, HP2 showed the best NLO properties, with the d(33) value as high as 145.0 pm V(-1).
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