The electrolytic polishing solution was a mixture of perchloric acid and methanol at a ratio of 1:9 .The optimum process of the electrolytic polishing solution was determined by adjusting the voltage and polishing time. The microstructure of the sample surface after polishing with different combination parameters was observed under field emission electron microscope. The polished surface quality of electrolytic polishing samples used for EBSD（Electron Back-Scattering Diffraction）depends on the experimental parameters of electrolytic polishing. Under which the sample is used for EBSD test, and clear images of Kikuchi pattern and grain orientation are obtained.