The role of the temperature in the morphology and properties of zinc oxide structures obtained by electrosynthesis in aqueous solution

Abstract

Herein, ZnO micro and nanostructures were synthesized by an electrochemical method in aqueous solution employing NaCl as the electrolyte. Different parameters influencing the synthesis process, i.e. current intensity, reaction time and temperature, were investigated. From this, it was concluded that the productivity of the reaction increases with longer reaction time, whereas the use of higher current intensity augments the specific energy consumption. On the other hand, the increase in temperature seems to exert a negative effect. The characterization of the resulting materials by scanning electron microscopy, X-ray diffraction and thermogravimetric analysis demonstrated that a mixture of Zn(OH)2 and ZnO crystalline structures is formed directly from the synthesis procedure. The content of Zn(OH)2 phase in the sample decreases as the temperature of the synthesis increases, this fact indicates that the low productivity obtained at higher temperatures is related to the nature of the resulting material. Thermal annealing of the samples containing both phases prepared following synthesis allows the phase transformation from Zn(OH)2 to pure ZnO structures. The band gap energies of the ZnO materials were determined by diffuse reflectance measurements according to the Kubelka Munk theory, revealing low values in all the cases which were highly dependent on the size of crystals within the materials. The photocatalytic properties of the pure ZnO samples post calcination were investigated by the decomposition of an organic dye under UV light irradiation. The results show the beneficial photocatalytic properties of the samples that had undergone calcination, these were superior in comparison to those prepared at room temperature which mainly consisted of Zn(OH)2.