Abstract: Scanning electron microscopy (SEM) is a common tool for the visual characterization of the microstructural morphology of the surface of samples. However, for zeolite samples, due to the low secondary electron yield, poor resistance to electron beams and bad conductivity, etc. caused by the silica and alumina components. The problems such as weak signal, charge effect, small loss of surface structure, and so on often emerge at the performance of SEM characterization of zeolite. The accelerating voltage, spot size, work distance etc. are the common adjustment parameters. By optimizing the above parameters, the SEM image quality of ZSM-5 zeolite was studies. The results showed that high quality scanning electron microscopic images can be obtained for sample testing at a low accelerating voltage, a spot size of 3.0 and a work distance of less than 5 mm. The contrast showed that the SEM images of ZSM-5 zeolite were the worst after coating platinum on the sample.