Electrolysis polishing method for preparing pure titanium and titanium alloy EBSD (electron back-scattered diffraction) sample

[0028] Example 1:

[0029] Use wire cutting technology to take a pure titanium flake with a thickness of 0.5mm from the pure titanium sample to be tested, and grind the two sides of the pure titanium flake with 280# and 400# silicon carbide dry sandpaper until its thickness is reduced to 0.28mm. , Grind the side of the obtained pure titanium flakes with 400# silicon carbide dry sandpaper and then use 600#, 800#, 1000# and 1200# silicon carbide dry sandpaper to grind and control its thickness to 0.12mm. Take 3 samples of length x width 5 x 5mm from the obtained pure titanium flakes, grind the burrs of the samples smoothly with 1200# silicon carbide dry sandpaper, and place the pure titanium samples taken out in the sample of the magnetodynamic double jet thinner In the clip, the smoother side of the pure titanium sample is placed on the conductive metal sheet in the sample holder and shields the double nozzle holes on the conductive metal sheet, and a transparent, flexible, acid-corrosive plastic sheet with a thickness of 0.4mm is taken to cover the pure titanium On the rougher side of the sample, the main material of the transparent flexible acid corrosion resistant plastic sheet is polyethylene terephthalate. The length and width of the transparent flexible acid corrosion resistant plastic sheet are 6×6mm. The pure titanium sample is electrolytically polished. During the polishing process, the composition of the electrolyte is perchloric acid, n-butanol and methanol. The volume ratio of perchloric acid, n-butanol and methanol is 1:7:10. The electrolyte is preferably prepared with 25mL perchloric acid, 175mL n-butanol and 250mL methanol, the voltage is 22V, the current is 20mA, the electrolysis time is 45s, and the electrolysis temperature is minus 25℃. Take out the pure titanium sample after electrolytic polishing and put it in the container. Clean the beaker of alcohol once, and the cleaning time is 30s. After removing it, put it into another beaker containing alcohol for a second cleaning. The second cleaning time is 50s. After removing it, blow dry to get pure titanium EBSD The sample, the backscattered electron diffraction experiment was performed on the obtained pure titanium EBSD sample, the calibration rate was 96.43%, and the experimental results are shown in the figure figure 1 Shown.

[0030] Example 2:

[0031] Use wire-cutting technology to take Ti-10V-2Fe-3Al flakes with a thickness of 1mm from the Ti-10V-2Fe-3Al sample to be tested, and use 280# and 400# silicon carbide dry sandpaper to test Ti-10V-2Fe. Grind both sides of the -3Al sheet until its thickness is reduced to 0.25mm. The side of the obtained Ti-10V-2Fe-3Al sheet that has been ground with 400# silicon carbide dry sandpaper is then sequentially used 600#, 800#, 1000# and 1200 #Silicon carbide dry sandpaper to grind and control its thickness to 0.14mm, and then from the Ti-10V-2Fe-3Al flakes obtained after grinding, take 5 samples of length × width 4×5mm, and use 1200# silicon carbide dry sandpaper Grind the burrs of the sample smoothly, and place the removed Ti-10V-2Fe-3Al sample in the sample holder of the magnetodynamic double-jet thinner, where the smoother side of the Ti-10V-2Fe-3Al sample is attached to the sample The conductive metal sheet in the clip is placed and shields the double nozzle holes on the conductive metal sheet, and a transparent flexible acid corrosion resistant plastic sheet with a thickness of 0.5mm is taken to cover the rougher side of the Ti-10V-2Fe-3Al sample, which is transparent, flexible and acid resistant The main material of the corroded plastic sheet is polyethylene terephthalate. The length and width of the transparent flexible acid-corrosive plastic sheet are 5×6mm. After closing the sample holder, electropolishing the Ti-10V-2Fe-3Al sample During the polishing process, the electrolyte is composed of perchloric acid, n-butanol, and methanol. The volume ratio of perchloric acid, n-butanol and methanol is 1:7:10. The electrolyte in this embodiment is preferably 20 mL of high chlorine Prepared with acid, 140mL n-butanol and 200mL methanol, the voltage is 30V, the current is 25mA, the electrolysis time is 40s, and the electrolysis temperature is minus 30℃. Take out the electropolished Ti-10V-2Fe-3Al sample and put it in the alcohol Clean the inside of the beaker once, and the cleaning time is 40s. After removing it, put it into another beaker containing alcohol for a second cleaning. The second cleaning time is 60s. After removing it, blow dry to get Ti-10V- 2Fe-3AlEBSD sample, the obtained Ti-10V-2Fe-3AlEBSD sample is subjected to backscattered electron diffraction experiment, the calibration rate is 92.35%, the experimental result is as shown in the figure figure 2 Shown.

[0032] Example 3:

[0033] Use wire cutting technology to take Ti-20Mo flakes with a thickness of 0.8mm from the Ti-20Mo sample that needs to be observed, and use 280# and 400# silicon carbide dry sandpaper to grind the two sides of the Ti-20Mo flakes until the thickness is reduced. The thickness of the Ti-20Mo flake that has been ground with 400# silicon carbide dry sandpaper is then ground with 600#, 800#, 1000# and 1200# silicon carbide dry sandpaper in turn and the thickness is controlled to 0.1mm. Then take 4 samples of length x width 4 x 4mm from the Ti-20Mo flakes obtained after grinding, grind the burrs of the samples smoothly with 1200# silicon carbide dry sandpaper, and place the taken Ti-20Mo sample on the magnetic double In the sample holder of the spray thinner, the smoother side of the Ti-20Mo sample is placed on the conductive metal sheet in the sample holder and covers the double nozzle holes on the conductive metal sheet, and the thickness is 0.3mm. The acid corrosion resistant plastic sheet covers the rougher side of the Ti-20Mo sample. The main material of the transparent flexible acid corrosion resistant plastic sheet is polyethylene terephthalate. The length and width of the transparent flexible acid corrosion resistant plastic sheet are 5× 5mm. After closing the sample holder, electropolishing the Ti-20Mo sample. During the polishing process, the composition of the electrolyte is perchloric acid, n-butanol and methanol. The volume ratio of perchloric acid, n-butanol and methanol is 1: 7:10. The electrolyte in this embodiment is preferably prepared with 27mL perchloric acid, 189mL n-butanol and 270mL methanol. The voltage is 20V, the current is 30mA, the electrolysis time is 60s, and the electrolysis temperature is minus 20°C. After electropolishing, The Ti-20Mo sample was taken out and put into a beaker filled with alcohol for cleaning once, and the cleaning time was 60s. After being removed, it was put into another beaker filled with alcohol for a second cleaning. The time for the second cleaning was 30s. Take it out and blow dry to obtain Ti-20Mo sample. Perform backscattered electron diffraction experiment on the obtained Ti-20Mo sample. The calibration rate is 93.21%. image 3 Shown.