Novel macrocyclic amine-linked oligocarbazole hollow microspheres are synthesized via a one-step oxidative method in aqueous solution. Upon altering the oxidants and acidic media, the average diameters of the obtained hollow microspheres are tunable from 0.23 to 2.0 mu m. With attractive amine and carbazole functionalities, exposed surface area, thermostability, and photoluminescent properties, the amine-linked oligocarbazole hollow microspheres are directly assembled to yield heavy metal sorbents with excellent selectivity and recyclability, shown to efficiently remove lead from contaminated water.