RESUMO
Tungsten oxide (WO3) and zinc oxide (ZnO) are n-type semiconductors with numerous applications in photocatalysis. The objective of this study was to synthesize and characterize different types of nanostructures (WO3, WO3-Mo, TiO2, and TiO2-ZnO) for a comparison of hybrid and pure nanostructures to use them as a photoanodes for photoelectrocatalytic degradation of emerging contaminants. With the aim of comparing the properties of both samples, field emission scanning electron microscopy (FE-SEM) and confocal laser-Raman spectroscopy were used to study the morphology, composition, and crystallinity, respectively. Electrochemical impedances, Mott-Schottky, and water splitting measurements were performed to compare the photoelectrochemical properties of photoanodes. Finally, the photoelectrocatalytic degradation of the pesticide Imazalil was carried out with the best optimized nanostructure (TiO2-ZnO).
RESUMO
In the present work, TiO2/ZnO hybrid nanosponges have been synthesized for the first time. First, TiO2 nanosponges were obtained by anodization under hydrodynamic conditions in a glycerol/water/NH4F electrolyte. Next, in order to achieve the anatase phase of TiO2 and improve its photocatalytic behaviour, the samples were annealed at 450 °C for 1 h. Once the TiO2 nanosponges were synthesized, TiO2/ZnO hybrid nanosponges were obtained by electrodeposition of ZnO on TiO2 nanosponges using different temperatures, times, and concentrations of zinc nitrate (Zn(NO3)2). TiO2/ZnO hybrid nanosponges were used as photoanodes in photoelectrochemical water splitting tests. The results indicate that the photoelectrochemical response improves, in the studied range, by increasing the temperature and the Zn(NO3)2 concentration during the electrodeposition process, obtaining an increase in the photoelectrochemical response of 141% for the TiO2/ZnO hybrid nanosponges electrodeposited at 75 °C with 10 mM Zn(NO3)2 for 15 min. Furthermore, morphological, chemical, and structural characterization was performed by Field Emission Scanning Electron Microscopy (FE-SEM) with Energy Dispersive X-Ray spectroscopy (EDX), Raman Confocal Laser Spectroscopy, X-Ray Photoelectron Spectroscopy (XPS), and Grazing Incidence X-Ray Diffraction (GIXRD).
RESUMO
Advanced oxidation processes driven by renewable energy sources are gaining attention in degrading organic pollutants in waste waters in an efficient and sustainable way. The present work is focused on a study of TiO2 nanotubes as photocatalysts for photoelectrocatalytic (PEC) degradation of acetaminophen (AMP) at different pH (3, 7, and 9). In particular, different TiO2 photocatalysts were synthetized by stirring the electrode at different Reynolds numbers (Res) during electrochemical anodization. The morphology of the photocatalysts and their crystalline structure were evaluated by field emission scanning electron microscopy (FESEM) and Raman confocal laser microscopy (RCLM). These analyses revealed that anatase TiO2 nanotubes were obtained after anodization. In addition, photocurrent densities versus potential curves were performed in order to characterize the electrochemical properties of the photocatalysts. These results showed that increasing the Re during anodization led to an enhancement in the obtained photocurrents, since under hydrodynamic conditions part of the initiation layer formed over the tubes was removed. PEC degradation of acetaminophen was followed by ultraviolet-visible absorbance measurements and chemical oxygen demand tests. As drug mineralization was the most important issue, total organic carbon measurements were also carried out. The statistical significance analysis established that acetaminophen PEC degradation improved as hydrodynamic conditions linearly increased in the studied range (Re from 0 to 600). Additionally, acetaminophen conversion had a quadratic behavior with respect to the reaction pH, where the maximum conversion value was reached at pH 3. However, in this case, the diversity of the byproducts increased due to a different PEC degradation mechanism.