Abstract: The morphology and structure of metal-organic frameworks (MOFs) have a significant impact on their performance and application. However, MOFs generally have poor electrical conductivity and are sensitive to electron beams, which can be easily damaged and appear charge phenomena during the scanning electron microscopic (SEM) testing. Therefore, it is of great significance to explore the proper test parameters to obtain high-quality SEM images of MOFs. Taking MIL-101 (Cr), Fe-MOF, Mn-MOF and ZIF-67(Co) as examples, the effects of acceleration voltage, beam current, working distance, probe and gold spray on SEM images were investigated. The results showed that the increase of the acceleration voltage can effectively improve the image resolution, but at the same time the penetration depth of electron beam also increased, which may lead to the charge breakdown effect and damage to the surface structure. A moderate increase of the beam current can improve the signal-to-noise ratio of the image, but too large a beam current will cause an indistinct edge of nanoparticles, so a medium beam current of 0.1~0.4 nA was preferred. As to the selection of the probe, it should be noted that on the Everhart-Thornley detector (ETD) and in-lens secondary electrons detector (T2) a good stereoscopic perception can be obtained on the in-lens backscattered electrons detector (T1) a poor three-dimensional sense can be obtained, but the contrast is better. The best resolution can be obtained on the in-column secondary electrons detector (T3) , but is more easily charged and appears to have flat particles. The gold spraying treatment can effectively improve the conductivity of the samples. These above results are helpful to explore the morphology of MOFs by SEM.