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In this study, the three-dimensional (3D) reduced graphene oxide/TiO₂ (RGOT) aerogel was synthesized by a facile one-step hydrothermal treatment, and its photocatalytic efficiency was evaluated in the photodegradation of recalcitrant carbamazepine (CBZ) in aqueous solution. RGOT exhibited high adsorption and an almost two-fold higher photodegradation ability than bare TiO₂ as more than 99% CBZ removal was observed within 90 min in 10 ppm aqueous solution of the latter. The mass ratio of TiO₂ in the RGOT aerogel substantially affected CBZ adsorption and photocatalytic degradation, with the optimal TiO₂/GO ratio in RGOT found to be 2:1. The chemical bonding between TiO₂ and GO and the effective reduction of the latter during RGOT synthesis were also considered to achieve high photocatalytic efficiency, because the physical mixture of GO and TiO₂ showed a lower photocatalytic CBZ degradation …