Abstract: The preparation of nano zinc oxide is a classic inorganic chemistry experiment with distinctive characteristics. In this paper, an innovative improvement is made to solve the existing problems in the experimental process of basic chemistry experiment “preparation of nano zinc oxide powder”. The preparation and photocatalytic activity of zinc oxide nanoparticles based on the microemulsion method were designed. This experiment features a mild reaction, simple operation, obvious phenomenon, and environmental friendliness. It can not only cultivate students’ basic operation skills but also stimulate students’ interest in experiments, and exercise students’ comprehensive ability. Compared to the traditional experiment for the preparation of nano zinc oxide, this approach has higher time efficiency and a scientifically reasonable experimental arrangement. The phenomena are more apparent, and it is more interesting. It is comprehensive and exploratory, as it not only consolidates students’ basic experimental skills but also nurtures their scientific research thinking and expands their research skills.