The design and construct pn heterojunction to reduce the recombination rate of photogenerated electron-hole pairs can effectively improve photocatalytic activity. In this study, ZnO/NiO heterojunctions were fabricated by annealing a Zn/Ni metal organic framework precursor synthesized via coprecipitation. The effects of the precursor annealing temperature on the microstructure, morphology, and optical properties of the ZnO/NiO nanocomposites were investigated using X-ray diffraction, scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, and UV-vis absorption spectroscopy. The results showed that the nanocomposite was composed of hexagonal wurtzite ZnO and cubic NiO, with the former being the dominant phase. Large ZnO nanoparticles were attached to small NiO nanoparticles, and a pn heterojunction interface was formed. The photodegradation performance of the nanomaterials was evaluated by monitoring the degradation of RhB under irradiation by ultraviolet light. The ZnO/NiO nanocomposites exhibited excellent photocatalytic activity when the annealing temperature was 550 °C. The photodegradation mechanism was also analyzed in detail, revealing that the heterojunction between the n-type ZnO and the p-type NiO played an important role in impeding the recombination of photogenerated electron-hole pairs and improving the photocatalytic efficiency.

The degradation of pollutants in wastewater using abundant resources and renewable energy sources, such as light, is attractive from an environmental perspective. ZnO is a well-known photocatalytic material. Therefore, in this study, a hierarchical ZnO microsphere precursor was prepared using a hydrothermal method. The precursor was subsequently annealed at different temperatures, which enabled the production of a ZnO catalyst having a controllable morphology. Specifically, as the annealing temperature increased, the precursor crystallized into hexagonal wurtzite and the crystallinity also increased. The catalysts were tested for their photocatalytic activity for the degradation of dye molecules (methylene blue and rhodamine B), and the catalyst sample annealed at 400 °C showed the best photocatalytic activity. The origin of this activity was studied using electron paramagnetic resonance spectroscopy and transient photocurrent measurements, and the structure of the optimal catalyst was invested using electron microscopy measurements, which revealed that it was formed of two-dimensional nanosheets having smooth surfaces, forming a 2D cellular network. Thus, we have presented a promising photocatalyst for the mineralization of organic contaminants in wastewater.