The invention belongs to the technical field of non-
ferrous metal analysis and particularly relates to an 
electropolishing preparation method of a sample for EBSD (
Electron Back-Scattered 
Diffraction) analysis of a 
titanium-aluminum 
alloy. The 
electropolishing preparation method comprises the following steps: firstly, carrying out earlier stage treatment on the sample: determining the size of the sample to be smaller than 7mm*6mm*4mm, and carrying out standard metallographic treatment and mechanical 
polishing on the testing surface; secondly, setting up a portable device: connecting the sample with a positive pole of a power supply, connecting a stainless steel plate with a negative pole of the power supply and matching the bottom end of 
electrolyte with a 
magnetic stirrer; thirdly, preparing the 
electrolyte: selecting 4 to 12 percent of 
perchloric acid, 55 to 65 percent of methyl 
alcohol and the balance of n-butyl 
alcohol according to the volume ratio, wherein the total amount of the 
electrolyte is 700ml; putting the electrolyte into a 
beaker with the volume of 1L; fourthly, carrying out 
electrolysis treatment, washing and 
drying: controlling the temperature to be 30 DEG C below zero to 20 DEG C below zero, controlling the 
voltage to be 25 to 35V and controlling the 
polishing time to be 40 to 55 seconds. The 
electropolishing preparation method disclosed by the invention has the advantages of large surface area for treating the sample and suitability for preparing 
titanium-aluminum 
alloy samples with various components and various test purposes, which are prepared by different 
processing method. In addition, the electropolishing preparation method has the advantages of easiness and flexibility in operation, no restriction from site facilities and the like, good 
polishing effect and 
high rate of finished products; the device has the characteristics of high mobility, low cost, easiness in promotion and wide application prospect.