Ultrasound-assisted synthesis of ZnO photocatalysts for gas phase pollutant remediation: Role of the synthetic parameters and of promotion with WO3

The synthesis of ZnO photocatalysts by ultrasound-assisted technique was here investigated. Several experimental parameters including the zinc precursor (acetate, chloride, nitrate), sonication conditions (amplitude, pulse) and post-synthetic thermal treatment (up to 500 °C) were studied. Crystalline ZnO samples were obtained without thermal treatments due to the adopted reactant ratios and synthesis temperature. Sonication plays a major role on the morphological oxide features in terms of particle size and surface area, the latter showing a 20-fold increase with respect to conventional synthesis. Interestingly, 1 and 3 s sonication pulses led to morphological properties similar to continuous sonication. A thermal treatment at moderate temperatures (400–450 °C) promoted the loss of surface hydroxylation and the formation of lattice defects, while higher temperatures were detrimental for the sample morphology. The prepared ZnO was decorated with WO₃ particles comparing an ultrasound-assisted technique using 1 s pulses with a conventional approach, giving rise to composites with promoted visible light absorption. Samples were tested towards the photocatalytic degradation of nitrogen oxides (500–1000 ppb) in humidified air under both UV and visible light. By carefully controlling the synthetic procedure, better performance were observed with respect to the commercial benchmark. Samples from ultrasound-assisted syntheses, also in the case of pulsed sonication, showed consistently better results than conventional references, in particular for ZnO-WO₃ composites. The composite by ultrasound-assisted synthesis showed > 95% degradation in 180 min and doubled NO_x degradation under visible light with respect to the conventional composite.