CN113670962A - Method for preparing high-calibration-rate pure magnesium EBSD sample at room temperature - Google Patents
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Abstract
The invention provides a method for preparing a high-calibration-rate pure magnesium EBSD sample at room temperature, belonging to the technical field of preparation of metal material analysis samples. Placing a pure magnesium sample as an anode in an electrolytic polishing solution for electrolytic polishing to obtain a pure magnesium EBSD sample; the electrolytic polishing is carried out at room temperature; the voltage of the electrolytic polishing is 0.2-1V, and the time is 45-60 s; the electrolytic polishing solution comprises phosphoric acid and ethanol; the volume ratio of the phosphoric acid to the ethanol is (35-40) to (60-65). The method can effectively remove the surface stress layer and the oxide layer of the pure magnesium, does not need low-temperature media such as liquid nitrogen and the like for cooling, and can be operated at room temperature; and the preparation cost and the equipment requirement are low, and the obtained pure magnesium EBSD sample has a smooth and clean surface and a high calibration rate, and is suitable for coarse-grained, fine-grained and ultra-fine-grained pure magnesium samples.
Description
Technical Field
The invention relates to the technical field of preparation of metal material analysis samples, in particular to a method for preparing a high-calibration-rate pure magnesium EBSD sample at room temperature.
Background
Magnesium is the least dense and the highest specific strength structural metal material, which has been reputed by the "time metal" of the 21 st century. The high-strength steel has good machinability and shock absorption, and excellent thermal conductivity and casting performance, is widely applied to the fields of automobile manufacturing industry, electronic industry, aerospace industry, medical rehabilitation instruments and the like, and plays an important role in reducing environmental pollution, reducing energy consumption, saving energy and the like. However, pure magnesium has poor plastic deformability at room temperature, and is not highly used as a plate, a bar and a pipe. In recent years, large plastic deformation technologies (such as extrusion, rolling, drawing and the like) provide a new technical approach for remarkably improving the mechanical properties of pure magnesium, and attract attention. The properties of the deformed pure magnesium are influenced by the microstructure, so that the plastic deformation mechanism of the deformed pure magnesium needs to be researched on the micro scale, and the plastic forming mechanism of the deformed pure magnesium needs to be deeply understood.
The Electron Backscattered Diffraction (Electron Back Diffraction-EBSD) technique is one of the most effective methods for carrying out the above studies. At present, the application of EBSD in material research is very wide, and it is an important tool for researching the relationship between components, tissues, processes and properties in materials. Compared with X-ray diffraction (acquiring macroscopic statistical information) and a transmission electron microscope (acquiring micro-area information), the EBSD technology can provide a great deal of valuable information such as the type and distribution of a phase, the size, the shape and the defect of grains, the type of a grain boundary, local crystal orientation, preferred orientation and the like in the range from micron to millimeter, and makes up for the vacancy of micron-scale structure and orientation representation.
The EBSD technology has extremely strict requirements on samples, and requires no stress layer on the surface of a metal sample, so that the samples need to be subjected to electrolytic polishing treatment. In the case of pure magnesium, the electrolytic polishing is more difficult because of the higher chemical activity, so that a dense oxide film is very easily formed in the electrolytic process, thereby causing the EBSD calibration rate to be reduced. At present, the most commonly used electrolyte is a perchloric acid system, but the electrolytic polishing must be carried out at a low temperature (generally 0 ℃ to-30 ℃, and cooling media such as liquid nitrogen, dry ice and the like are needed for cooling) to inhibit the formation of an oxide film, and meanwhile, the voltage must be increased to improve the conductivity of the electrolyte, so that the preparation method has the defects of complex operation, difficult temperature control, high voltage (generally 5-15V) and the like.
Disclosure of Invention
The invention aims to provide a method for preparing a high-calibration-rate pure magnesium EBSD sample at room temperature, which can be operated at room temperature without cooling by low-temperature media such as liquid nitrogen, dry ice and the like, and has the advantages of low polishing voltage, stable effect and high calibration rate.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for preparing a high-calibration-rate pure magnesium EBSD sample at room temperature, which comprises the following steps:
placing a pure magnesium sample as an anode in an electrolytic polishing solution for electrolytic polishing to obtain a pure magnesium EBSD sample;
the electrolytic polishing is carried out at room temperature;
the voltage of the electrolytic polishing is 0.2-1V, and the time is 45-60 s;
the electrolytic polishing solution comprises phosphoric acid and ethanol; the volume ratio of the phosphoric acid to the ethanol is (35-40) to (60-65).
Preferably, the electrolytic polishing uses a 304 stainless steel plate as a cathode and a pure magnesium sample as an anode.
Preferably, the ratio of the volume of the electrolytic polishing solution to the area of the surface to be tested of the pure magnesium sample is 100 mL: (1 to 2) cm2。
Preferably, the phosphoric acid is analytically pure phosphoric acid, and the ethanol is absolute ethanol.
Preferably, before the electrolytic polishing, the method further comprises the step of sequentially polishing and mechanically polishing the surface to be tested of the pure magnesium sample.
Preferably, the step-by-step grinding comprises: and sequentially using 400#, 600#, 800#, 1000# and 1500# silicon carbide abrasive paper to polish the surface to be tested of the pure magnesium sample, and rotating the sample by 90 degrees when the abrasive paper is replaced until all grinding marks of the previous time are removed.
Preferably, the mechanical polishing process comprises: firstly, roughly polishing by adopting an alumina polishing powder suspension with the particle size of 0.5 mu m; and then, finely polishing by adopting an alumina polishing powder suspension with the particle size of 0.05 mu m until the surface of the sample presents a mirror surface.
Preferably, after the electrolytic polishing is finished, the method further comprises the step of carrying out ultrasonic vibration cleaning on the pure magnesium sample after the electrolytic polishing by adopting absolute ethyl alcohol.
Preferably, after the ultrasonic vibration cleaning is finished, the cleaned pure magnesium sample is quickly dried and stored in absolute ethyl alcohol to obtain a pure magnesium EBSD sample.
Preferably, the calibration ratio of the pure magnesium EBSD sample is 80% or more.
The invention provides a method for preparing a high-calibration-rate pure magnesium EBSD sample at room temperature, which comprises the following steps: placing a pure magnesium sample as an anode in an electrolytic polishing solution for electrolytic polishing to obtain a pure magnesium EBSD sample; the electrolytic polishing is carried out at room temperature; the voltage of the electrolytic polishing is 0.2-1V, and the time is 45-60 s; the electrolytic polishing solution comprises phosphoric acid and ethanol; the volume ratio of the phosphoric acid to the ethanol is (35-40) to (60-65).
The method takes the mixture of phosphoric acid and ethanol as electrolytic polishing solution, and phosphoric acid can dissolve the oxide film on the surface of pure magnesium at room temperature, so that the method can effectively remove the oxide layer and the stress layer on the surface of pure magnesium at room temperature without cooling by low-temperature media such as liquid nitrogen, dry ice and the like; moreover, the reaction intensity of the electrolytic polishing solution is less than that of a perchloric acid system, and the pure magnesium surface can be prevented from being over-corroded, so that the electrolytic polishing effect is stable, and the pure magnesium EBSD sample with a bright and flat surface, no corrosion pit and high calibration rate can be obtained. In addition, since the polishing solution of the present invention can be performed at room temperature, it is not necessary to increase the voltage to improve the conductivity of the electrolyte, and thus, it has an advantage of low polishing voltage.
The method is suitable for coarse-grained, fine-grained and ultra-fine-grained pure magnesium samples.
The electrolytic polishing solution adopted by the invention has low cost and simple preparation.
Drawings
FIG. 1 is a polar view of an as-cast pure magnesium EBSD sample prepared in example 1 of the present invention;
FIG. 2 is a polar view of a hot rolled pure magnesium EBSD sample prepared in example 2 of the present invention;
FIG. 3 is a pole figure of a hot-extruded pure magnesium EBSD sample prepared in example 3 of the present invention.
Detailed Description
The invention provides a method for preparing a high-calibration-rate pure magnesium EBSD sample at room temperature, which comprises the following steps:
placing a pure magnesium sample as an anode in an electrolytic polishing solution for electrolytic polishing to obtain a pure magnesium EBSD sample;
the electrolytic polishing is carried out at room temperature;
the voltage of the electrolytic polishing is 0.2-1V, and the time is 45-60 s;
the electrolytic polishing solution comprises phosphoric acid and ethanol; the volume ratio of the phosphoric acid to the ethanol is (35-40) to (60-65).
In the present invention, the starting materials used are all commercially available products well known in the art, unless otherwise specified.
Before electrolytic polishing, the invention preferably performs step-by-step grinding and mechanical polishing treatment on the surface to be tested of the pure magnesium sample in sequence.
The invention has no special requirements on the pure magnesium sample, and any pure magnesium sample needing EBSD test can be used. The invention has no special requirement on the state of the pure magnesium sample, and can be specifically but not limited to an as-cast state, a hot rolling state and a hot extrusion state. The invention has no special requirement on the size of the pure magnesium sample, and the pure magnesium sample can be prepared by adopting the size well known in the field. In the examples of the present invention, the dimensions of the pure magnesium sample were 10mm × 10mm × 2 mm.
In the present invention, the stepwise grinding preferably includes: and sequentially using 400#, 600#, 800#, 1000# and 1500# silicon carbide abrasive paper to polish the surface to be tested of the pure magnesium sample, and rotating the sample by 90 degrees when the abrasive paper is replaced until all grinding marks of the previous time are removed. The invention utilizes progressive grinding to remove surface scratches and prepares for mechanical polishing.
In the present invention, the mechanical polishing process preferably includes: firstly, roughly polishing by adopting an alumina polishing powder suspension with the particle size of 0.5 mu m; and then, finely polishing by adopting an alumina polishing powder suspension with the particle size of 0.05 mu m until the surface of the sample presents a mirror surface.
The invention has no special requirements on the rough polishing and the fine polishing, and the rough polishing and the fine polishing which are well known in the field can be adopted. The invention utilizes mechanical polishing treatment to make the surface of the pure magnesium sample smooth and flat, and improves the electrolytic polishing efficiency.
After mechanical polishing treatment, the obtained pure magnesium sample is preferably washed by absolute ethyl alcohol, and then the pure magnesium sample is used as an anode and placed in an electrolytic polishing solution for electrolytic polishing.
In the present invention, the electrolytic polishing solution includes phosphoric acid and ethanol; the volume ratio of the phosphoric acid to the ethanol is (35-40) to (60-65) based on the volume of the phosphoric acid to the ethanol being 100. In embodiments of the invention, the volume ratio of phosphoric acid to ethanol is 35:65, 37:63 or 40: 60. In the present invention, the phosphoric acid is preferably an analytically pure phosphoric acid, and the ethanol is preferably anhydrous ethanol. In the present invention, the ratio of the volume of the electrolytic polishing solution to the area of the surface to be tested of the pure magnesium sample is preferably 100 mL: (1 to 2) cm2。
In the invention, the electrolytic polishing is carried out at room temperature, wherein the room temperature is 10-30 ℃, and preferably 15-25 ℃. In the invention, the voltage of the electrolytic polishing is 0.2-1V, preferably 0.3-0.8V; the time of the electrolytic polishing is 45-60 s, preferably 50-55 s. The invention ensures high calibration rate by controlling the composition of the electrolytic polishing solution and matching the voltage, temperature and time of electrolytic polishing.
The method takes the mixture of phosphoric acid and ethanol as electrolytic polishing solution, and phosphoric acid can dissolve the oxide film on the surface of pure magnesium at room temperature, so that the method can effectively remove the oxide layer and the stress layer on the surface of pure magnesium at room temperature without cooling by low-temperature media such as liquid nitrogen, dry ice and the like; moreover, the reaction intensity of the electrolytic polishing solution is less than that of a perchloric acid system, and the pure magnesium surface can be prevented from being over-corroded, so that the electrolytic polishing effect is stable, and the pure magnesium EBSD sample with a bright and flat surface, no corrosion pit and high calibration rate can be obtained. In addition, the polishing solution can be carried out at room temperature, and the conductivity of the electrolyte is improved without enhancing the voltage, so the polishing solution has the advantages of low polishing voltage and short sample preparation time.
In the present invention, the electrolytic polishing uses a 304 stainless steel plate as a cathode.
After the electrolytic polishing is finished, the invention preferably also comprises the step of carrying out ultrasonic vibration cleaning on the pure magnesium sample after the electrolytic polishing by adopting absolute ethyl alcohol. In the present invention, the number of times of the ultrasonic vibration cleaning is preferably 3 times. The invention preferably replaces the absolute ethyl alcohol with new absolute ethyl alcohol every time the ultrasonic vibration cleaning is carried out. In the present invention, the time for each ultrasonic vibration cleaning is preferably 2 min. The power of the ultrasonic vibration cleaning is not particularly required, and the power well known in the field can be adopted.
After the ultrasonic vibration cleaning is finished, the method quickly dries the cleaned pure magnesium sample, and stores the pure magnesium sample in absolute ethyl alcohol to obtain the pure magnesium EBSD sample.
In the invention, the drying mode is preferably to suck surface liquid by using dust-free paper and naturally dry in the air. The invention uses the dust-free paper to wipe off the polluted absolute ethyl alcohol remained on the surface, thereby preventing the surface from being damaged. The drying process of the invention is fast and short in time, so that the drying process can not be oxidized.
The calibration rate of the pure magnesium EBSD sample obtained by the method of the invention reaches more than 80 percent.
The method for preparing high-calibration pure magnesium EBSD samples at room temperature provided by the invention is described in detail with reference to the following examples, but the method should not be construed as limiting the scope of the invention.
Example 1
The preparation of the as-cast pure magnesium EBSD sample in this example comprises the following specific steps:
(1) cutting a sample with the size of 10mm multiplied by 2mm from the cast pure magnesium by using a linear cutting machine, and polishing the surface to be tested of the sample: the silicon carbide abrasive paper of 400#, 600#, 800#, 1000# and 1500# is used for polishing in sequence, and when the abrasive paper is replaced, a test sample needs to be rotated by 90 degrees until all the polishing marks of the previous time are removed. The sample is uniformly stressed and has a flat surface in the polishing process.
(2) Carrying out mechanical polishing treatment on the surface to be tested of the as-cast pure magnesium sample: firstly, carrying out rough polishing treatment by adopting an alumina polishing powder suspension with the particle size of 0.5 mu m to remove surface grinding marks; and then, carrying out fine polishing treatment by adopting an alumina polishing powder suspension with the particle size of 0.05 mu m until the surface of the sample presents a mirror surface. After polishing, the surface of the sample is washed by absolute ethyl alcohol.
(3) Electrolytic polishing treatment was performed at room temperature (30 ℃): preparing 100mL of electrolytic polishing mixed solution with 35% phosphoric acid and 65% absolute ethyl alcohol by volume fraction; and (3) performing electrolytic polishing treatment by taking the pure magnesium sample subjected to mechanical polishing in the step (2) as an anode and a 304 stainless steel plate as a cathode. Wherein, the voltage of the direct current power supply is set to be 0.2V, and the electrolysis time is set to be 60 s.
(4) And after the electrolytic polishing is finished, quickly putting the sample into a container containing 15mL of absolute ethyl alcohol for ultrasonic cleaning, wherein the cleaning frequency is 3 times, and the absolute ethyl alcohol is replaced by new absolute ethyl alcohol every time, and the cleaning time is 2 minutes every time. And finally, taking out the sample, absorbing surface liquid by adopting dust-free paper and naturally drying in the air. And (4) storing the sample in absolute ethyl alcohol to obtain an as-cast pure magnesium EBSD sample.
The EBSD analysis of the as-cast pure magnesium EBSD sample prepared in this example was carried out, the pole figure of the EBSD sample is shown in FIG. 1, and the software shows a calibration rate of 92.4%.
Example 2
The specific steps for preparing the hot-rolled pure magnesium EBSD sample in the embodiment are as follows:
(1) cutting a test sample with the size of 10mm multiplied by 2mm from the hot-rolled pure magnesium by using a linear cutting machine, and polishing the surface to be tested of the test sample: the silicon carbide abrasive paper of 400#, 600#, 800#, 1000# and 1500# is used for polishing in sequence, and when the abrasive paper is replaced, a test sample needs to be rotated by 90 degrees until all the polishing marks of the previous time are removed. The sample is uniformly stressed and has a flat surface in the polishing process.
(2) Carrying out mechanical polishing treatment on the surface to be tested of the hot-rolled pure magnesium sample: firstly, carrying out rough polishing treatment by adopting an alumina polishing powder suspension with the particle size of 0.5 mu m to remove surface grinding marks; and then, carrying out fine polishing treatment by adopting an alumina polishing powder suspension with the particle size of 0.05 mu m until the surface of the sample presents a mirror surface. After polishing, the surface of the sample is washed by absolute ethyl alcohol.
(3) The electrolytic polishing treatment was carried out at room temperature (25 ℃): preparing 100mL of electrolytic polishing mixed solution with the volume fraction of 37% phosphoric acid and 63% absolute ethyl alcohol; and (3) performing electrolytic polishing treatment by taking the pure magnesium sample subjected to mechanical polishing in the step (2) as an anode and a 304 stainless steel plate as a cathode. Wherein, the voltage of the direct current power supply is set to be 0.5V, and the electrolysis time is set to be 50 s.
(4) And after the electrolytic polishing is finished, quickly putting the sample into a container containing 15mL of absolute ethyl alcohol for ultrasonic cleaning, wherein the cleaning frequency is 3 times, and the absolute ethyl alcohol is replaced by new absolute ethyl alcohol every time, and the cleaning time is 2 minutes every time. And finally, taking out the sample, absorbing surface liquid by adopting dust-free paper and naturally drying in the air. And (4) storing the sample in absolute ethyl alcohol to obtain a hot-rolled pure magnesium EBSD sample.
The EBSD analysis of the hot-rolled pure magnesium EBSD sample prepared in this example showed that the pole figure of the EBSD sample is shown in FIG. 2, and the software showed that the calibration rate is 87.1%.
Example 3
The specific steps for preparing the hot-extruded pure magnesium EBSD sample in the embodiment are as follows:
(1) cutting a test sample with the size of 10mm multiplied by 2mm from the hot extrusion state pure magnesium by using a linear cutting machine, and polishing the surface to be tested of the test sample: the silicon carbide abrasive paper of 400#, 600#, 800#, 1000# and 1500# is used for polishing in sequence, and when the abrasive paper is replaced, a test sample needs to be rotated by 90 degrees until all the polishing marks of the previous time are removed. The sample is uniformly stressed and has a flat surface in the polishing process.
(2) Carrying out mechanical polishing treatment on the surface to be tested of the hot extrusion state pure magnesium sample: firstly, carrying out rough polishing treatment by adopting an alumina polishing powder suspension with the particle size of 0.5 mu m to remove surface grinding marks; and then, carrying out fine polishing treatment by adopting an alumina polishing powder suspension with the particle size of 0.05 mu m until the surface of the sample presents a mirror surface. After polishing, the surface of the sample is washed by absolute ethyl alcohol.
(3) Electrolytic polishing treatment was performed at room temperature (10 ℃): preparing 100mL of electrolytic polishing mixed solution with the volume fraction of 40% phosphoric acid and 60% absolute ethyl alcohol; and (3) performing electrolytic polishing treatment by taking the pure magnesium sample subjected to mechanical polishing in the step (2) as an anode and a 304 stainless steel plate as a cathode. Wherein, the voltage of the direct current power supply is set to be 1V, and the electrolysis time is set to be 45 s.
(4) And after the electrolytic polishing is finished, quickly putting the sample into a container containing 15mL of absolute ethyl alcohol for ultrasonic cleaning, wherein the cleaning frequency is 3 times, and the absolute ethyl alcohol is replaced by new absolute ethyl alcohol every time, and the cleaning time is 2 minutes every time. And finally, taking out the sample, absorbing surface liquid by adopting dust-free paper and naturally drying in the air. And (4) storing the sample in absolute ethyl alcohol to obtain an extruded EBSD sample.
The EBSD analysis of the hot-extruded pure magnesium EBSD sample prepared in this example is carried out, the pole figure of the EBSD sample is shown in FIG. 3, and the software shows that the calibration rate is 82.3%.
Comparative example 1
The Chinese patent with the application number of 201910988922.0 discloses a preparation method for a magnesium alloy EBSD sample. The method adopts a perchloric acid-absolute ethyl alcohol electrolyte system, the temperature of the electrolytic polishing solution is 0 ℃, the polishing voltage is 5-10V, the polishing time is 8-15 s, and an OPS polishing step is added, so that the cost and the sample preparation time are increased. Finally, the calibration rate is 73 to 88.9 percent.
Comparative example 2
The only difference from example 3 was that the dc power supply voltage in step (3) of example 3 was set to 1.5V, the electrolysis time was set to 60s, and the calibration rate was measured to be 55.6%.
From the above example and comparative example 1, it can be seen that the present invention provides a method for preparing a high calibration rate pure magnesium EBSD sample at room temperature, compared to the existing preparation method, the present invention does not require low temperature media such as liquid nitrogen, dry ice, etc. to cool, and can be operated at room temperature, the polishing voltage is low, the effect is stable, and the calibration rate is high. As is apparent from the results of example and comparative example 2, the present invention is advantageous in obtaining pure American EBSD samples at a high calibration rate by controlling the conditions of electropolishing.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for preparing a high-calibration-rate pure magnesium EBSD sample at room temperature comprises the following steps:
placing a pure magnesium sample as an anode in an electrolytic polishing solution for electrolytic polishing to obtain a pure magnesium EBSD sample;
the electrolytic polishing is carried out at room temperature;
the voltage of the electrolytic polishing is 0.2-1V, and the time is 45-60 s;
the electrolytic polishing solution comprises phosphoric acid and ethanol; the volume ratio of the phosphoric acid to the ethanol is (35-40) to (60-65).
2. The method of claim 1, wherein the electropolishing is cathode on a 304 stainless steel plate.
3. The method of claim 1, wherein the ratio of the volume of the electrolytic polishing solution to the area of the surface to be tested of the pure magnesium sample is 100 mL: (1 to 2) cm2。
4. The method of claim 1, wherein the phosphoric acid is an analytically pure phosphoric acid and the ethanol is absolute ethanol.
5. The method as claimed in claim 1, wherein before the electrolytic polishing, the method further comprises the step-by-step grinding and mechanical polishing treatment of the surface to be tested of the pure magnesium sample.
6. The method of claim 5, wherein the progressive grinding comprises: and sequentially using 400#, 600#, 800#, 1000# and 1500# silicon carbide abrasive paper to polish the surface to be tested of the pure magnesium sample, and rotating the sample by 90 degrees when the abrasive paper is replaced until all grinding marks of the previous time are removed.
7. The method of claim 5, wherein the mechanical polishing process comprises: firstly, roughly polishing by adopting an alumina polishing powder suspension with the particle size of 0.5 mu m; and then, finely polishing by adopting an alumina polishing powder suspension with the particle size of 0.05 mu m until the surface of the sample presents a mirror surface.
8. The method of claim 1, further comprising ultrasonically vibrating and cleaning the electropolished pure magnesium sample with absolute ethyl alcohol after the electropolishing is finished.
9. The method according to claim 8, wherein after the ultrasonic vibration cleaning is completed, the cleaned pure magnesium sample is rapidly dried and stored in absolute ethyl alcohol to obtain a pure magnesium EBSD sample.
10. The method of claim 1, wherein the pure magnesium EBSD sample is normalized to 80% or greater.
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|---|---|---|---|---|
| CN103163003A (en) * | 2013-03-18 | 2013-06-19 | 燕山大学 | Metallographic phase display method used for different microstructure conditions of wrought magnesium alloy |
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| CN110618149A (en) * | 2019-10-17 | 2019-12-27 | 江苏理工学院 | Preparation method of magnesium alloy EBSD sample |
| CN110726743A (en) * | 2019-11-13 | 2020-01-24 | 河北科技大学 | Method for preparing pure titanium EBSD sample at room temperature |
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2021
- 2021-08-23 CN CN202110965700.4A patent/CN113670962A/en active Pending
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|---|---|---|---|---|
| CN103163003A (en) * | 2013-03-18 | 2013-06-19 | 燕山大学 | Metallographic phase display method used for different microstructure conditions of wrought magnesium alloy |
| CN105063739A (en) * | 2015-09-19 | 2015-11-18 | 太原理工大学 | Preparation method of magnesium alloy electron back-scattered diffraction (EBSD) sample and special electrolytic polishing solution thereof |
| CN110618149A (en) * | 2019-10-17 | 2019-12-27 | 江苏理工学院 | Preparation method of magnesium alloy EBSD sample |
| CN110726743A (en) * | 2019-11-13 | 2020-01-24 | 河北科技大学 | Method for preparing pure titanium EBSD sample at room temperature |
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