Sol−gel-based hydrothermal method for the synthesis of 3D flower-like ZnO microstructures composed of nanosheets for photocatalytic applications

Self-assembled 3D flower-like ZnO microstructures composed of nanosheets have been prepared on a large scale through a sol−gel-assisted hydrothermal method using Zn(NO₃)₂·6H₂O, citric acid, and NaOH as raw materials. The product has been characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The optical properties of the product have been examined by room temperature photoluminescence (PL) measurements. A possible growth mechanism of the 3D flower-like ZnO is proposed based on the results of experiments carried out for different hydrothermal treatment times. Experiments at different hydrothermal treatment temperatures have also been carried out to investigate their effect on the final morphology of the ZnO. The photocatalytic activities of the as-prepared ZnO have been evaluated by photodegradation of Reactive Blue 14 (KGL) under ultraviolet (UV) irradiation. The experimental results demonstrated that self-assembled 3D flower-like ZnO composed of nanosheets could be obtained over a relatively broad temperature range (90−150 °C) after 17 h of hydrothermal treatment. All of the products showed good photocatalytic performance, with the degree of degradation of KGL exceeding 82% after 120 min. In particular, the sample prepared at 120 °C for 17 h exhibited superior photocatalytic activity to other ZnO samples and commercial ZnO, and it almost completely degraded a KGL solution within 40 min. The relationship between photocatalytic activity and the structure, surface defects, and surface areas of the samples is also discussed.