Abstract: Single crystal ZnO microrods were deposited on the surface of Zn plate through corrosion of Zn plate by H₂O₂. The sample components and crystal structure analysis are conducted by X-ray diffraction (XRD). Transmission electron microscope (TEM) and scanning electron microscope (SEM) are adopted to analyze the morphology of as-synthesized ZnO microrods. Methyl orange (MO) is used as the pollutant and the ZnO/Zn are applied as photocatalysts under the irradiation of UV lamp, in order to record the degradation process through UV- spectrophotometer. The obtained wurtize-type ZnO microrods present an effective degradation of methyl orange under ultraviolet, and it keeps a good efficiency during the ten times repeated photocatalytic tests. This experiment is suitable for the undergraduate innovative experimental teaching with green and simple preparation process, and cheap experiment material. From the preparation and structure characterization of experimental materials to the application of photocatalytic properties, it is helpful for students to deepen their understanding of the concepts of preparation, characterization and properties of materials in practical operation.