In this study, Tb-doped CdSe nanoparticles with variable Tb3+ content were synthesized by a simple sonochemical technique. The synthesized nanoparticles were characterized by X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and powder X-ray diffraction (XRD). The sono-photocatalytic activities of the as-prepared specimens were assessed for the degradation of Reactive Black 5. The experimental results show that the sono-photocatalytic process (85.25%) produced a higher degradation percentage than the individual sono- (22%) and photocatalytic degradation (8%) processes for an initial dye concentration and Tb-doped CdSe dosage of 20 mg/L and 1 g/L, respectively. Response surface methodology (RSM) was utilized to assess model and optimize the impacts of the operational parameters, namely, the Tb3+ content, initial dye concentration, catalyst dosage, and time. The addition of benzoquinone results in remarkably inhibited degradation and the addition of ammonium oxalate reduced the removal percentage to 24%. Superoxide radicals and photogenerated holes were detected as the main oxidative species.
