A method for preparing micro EBSD specimens by mechanical and electrolytic polishing

Abstract

The purpose of the present invention is to provide a method for preparing a micro EBSD sample by mechanical and electrolytic polishing. The method forms a larger-sized sample by mounting the micro sample at the center of the mounting sample, takes out the micro sample using a sampling platform after mechanical polishing, and then places the micro sample in an acid electrolytic polishing solution using special clamping tweezers for special electrolytic polishing, and obtains a micro EBSD sample of a metal material after cleaning and drying. The method mainly solves the problem of micro sample being difficult to grind and polish, and also solves the problem of micro sample being fastened during the electrolytic polishing process, and further solves the problem of micro sample being difficult to electrolytically polish by a special electrolytic method. The method is simple to operate, has high preparation efficiency, and excellent sample preparation effect, and the sample resolution rate is more than 90%. It has a wide range of applications and is suitable for promotion and application.

Description

Technical Field

[0001] The invention belongs to the technical field of metal material analysis, and in particular provides a method for preparing a micro EBSD sample by mechanical and electrolytic polishing. Background Art

[0002] Since the advent of EBSD technology in the 1980s, EBSD technology has gradually been applied in metal materials, ceramic materials, compounds, etc. EBSD technology can obtain information such as material grains, substructures, precipitated phases, microstructures, and grain orientation differences, which is of great significance for material performance research and has now been widely used in microscopic research of different structural materials.

[0003] Since electron back diffraction only occurs within a few tens of nanometers on the surface of the material, strict requirements are placed on the preparation of EBSD samples, that is, the sample surface must be flat, stress-free, and free of severe corrosion pits. Because of stress on the sample surface, the lattice will be distorted, and the EBSD system will not be able to obtain accurate Kikuchi patterns, resulting in reduced resolution. If severe corrosion pits occur, they will exceed the range of electron back diffraction, which can easily lead to reduced sample resolution. Therefore, EBSD testing has relatively high requirements for sample preparation. Secondly, the preparation requirements for micro EBSD samples are even higher. The difficulty lies in the grinding and mechanical polishing of micro samples, as well as the tightening of micro samples during electrolytic polishing. At the same time, it is difficult to find the most suitable electrolytic polishing process for micro EBSD samples.

[0004] At present, there are few technologies for preparing micro EBSD samples, and the general method for preparing EBSD samples is mainly through mechanical polishing + electrolytic polishing. For conventional mechanical + electrolytic polishing, micro EBSD samples are often difficult to prepare. For example, for micro samples, mechanical polishing is not easy to operate, and because the sample is very small, the requirements for electrolytic polishing of the sample are more stringent, that is, micro EBSD samples are difficult to prepare, and the prepared samples often have poor results. The invention patent with application number 201710695101.9 provides a method for preparing multiphase alloy EBSD analysis test samples. The sample preparation cost of this method is high, and the sample must be prepared on an ion thinning instrument. In addition, the sample preparation time is long and the sample preparation efficiency is low.

[0005] The method of preparing micro EBSD samples by mechanical + electrolytic polishing is a simple, easy to operate, low-cost and efficient method for preparing micro EBSD samples. Summary of the invention

[0006] The purpose of the present invention is to provide a method for preparing a micro EBSD sample by electrolytic polishing. The method mainly solves the problem that the micro sample is difficult to grind and polish, and also solves the problem of sample fastening during the electrolytic polishing process of the micro sample. The problem that the micro sample is difficult to electrolytic polish is solved by a special electrolytic method. The method has a wide range of applications and is suitable for the preparation of both small-sized micro samples and large-sized samples.

[0007] The technical solution of the present invention is as follows:

[0008] A method for preparing a micro EBSD sample by electrolytic polishing, the specific steps are as follows:

[0009] ① Mounting:

[0010] Cut the metal material into micro-samples 2, mount the micro-samples 2 to the center of the mounting sample on the mounting machine, and finally form the mounting sample 1. Do not mount the sample too tightly when mounting.

[0011] ② Open V-shaped groove:

[0012] Two V-shaped grooves 3 are symmetrically opened on the mounted sample 1 in a direction perpendicular to the micro-specimen 2 (such as Figure 1 As shown), the micro-sample 2 is located on the connecting line of the tips of two V-shaped grooves 3;

[0013] ③ Mechanically polishing the mounted sample 1;

[0014] ④ A protective layer is attached to the surface of the micro-sample 2 (e.g., a transparent adhesive is used to attach the protective layer to the surface) to prevent the micro-sample 2 from being scratched when the mounted sample 1 is broken open; and then the mounted sample 1 is placed in the sampling platform;

[0015] ⑤ Fasten the mounted sample 1 in the sampling platform, apply downward force to the center of the mounted sample 1, so that the sample is broken along the line connecting the tips of the V-shaped grooves 3, take out the micro-sample 2, and remove the protective layer thereon;

[0016] ⑥ Place the micro sample 2 on an ultrasonic instrument and clean it with alcohol ultrasonic vibration;

[0017] ⑦ Place the micro sample 2 in an acidic electrolytic polishing solution for electrolytic polishing:

[0018] First, the voltage is used as the main factor, and then the current is used as the main factor: the power supply current is set to 0.8A, the voltage is set to the maximum, which is 60V, and then the electrolytic polishing liquid is cooled to minus 70°C with a refrigerant (preferably liquid ammonia), and the power supply is connected. At this time, the power supply is mainly voltage, and the current is 0.1A. As the temperature rises, the current gradually increases, and the voltage remains unchanged until the current reaches 0.8A. The power supply becomes mainly current, and the current remains unchanged at 0.8A, and the voltage begins to decrease until the voltage is reduced to 50V, then the power supply is turned off, and the micro-sample 2 is taken out; during the electrolytic polishing process, the electrolyte is surrounded by plastic foam for heat preservation;

[0019] ⑧ Rinse the micro sample 2 with water, then rinse it with alcohol and blow it dry, and finally obtain a micro EBSD sample of the metal material.

[0020] As the preferred technical solution:

[0021] In step ①, the micro-specimen 2 is rectangular, square, circular, rhombus or pentagonal (preferably rectangular). For rectangular or square specimens, the size range is: length = 0.5-10 mm, width = 0.3-10 mm, thickness = 0.5-3 mm (generally when cutting samples, if the sample width is small, the sample length needs to be set longer). The thickness of the mounted sample 1 is 2-3 times the thickness of the micro-specimen 2.

[0022] In step ③, the sample is ground on a grinder using 150#, 320#, 800#, and 2000# sandpaper in sequence; the ground sample is mechanically polished on a polishing machine using a polishing liquid (the corresponding polishing liquid is selected for different alloys).

[0023] In step ④, the sampling platform consists of two symmetrical clamps 4 and two arc columns 5; a groove hole 6 is provided in the height direction of the clamp 4, and the cross-sectional diameter of the groove hole 6 is larger than the diameter of the mounted sample 1; the arc column 5 can be stuck in the groove hole 6, and its height is smaller than the height of the clamp 4, and the arc column 5 is used to support the mounted sample 1; the arc column 5 is fastened to the clamp 4 by bolts 7, and the two symmetrical clamps 4 are fastened together by bolts 7.

[0024] A bolt 7 is provided at the upper position of the groove hole 6 of the clamp 4. The bolt 7 is arranged parallel to the horizontal direction and is used to fasten the mounted sample 1 placed on the arc column 5 to prevent the mounted sample 1 from moving and scratching the micro-specimen 2 during the smashing process.

[0025] The arc column 5 is clamped in the groove hole 6, and then the two clamps 4 are arranged with the groove holes 6 on one side facing each other, leaving a gap 8 between the clamps 4, and the mounted sample 1 is placed on the two relatively arranged arc columns 5, so that the tip connection line of the V-shaped groove 3 on the mounted sample 1 is located in the gap 8 between the clamps 4, so that the place is suspended in the air, which is conducive to the sample being disconnected along the direction of the tip connection line of the V-shaped groove 3; tighten the bolts 7 between the two clamps 4 to clamp the mounted sample 1.

[0026] The present invention provides a special sampling platform, which greatly improves the preparation efficiency of micro-samples.

[0027] In step ⑦, the micro-sample 2 is placed in the acid electrolytic polishing solution using clamping tweezers, and the clamping tweezers are composed of left and right parts:

[0028] In the left part: the first tweezer handle 11 and the first tweezer head 12 are a straight structure as a whole, a sample-laying platform 13 is provided at the tail of the first tweezer head 12, a baffle plate 14 is provided on the sample-laying platform 13, and the baffle plate 14 is arranged perpendicular to the width direction of the first tweezer head 12;

[0029] In the right part: the second tweezers handle 21 and the second tweezers head 22 are in a broken line structure as a whole. When the tail ends of the first tweezers handle 11 and the second tweezers handle 22 are close to each other, the second tweezers head 22 with the same width as the first tweezers head 12 can be placed on the sample placement platform 13 and parallel to the first tweezers head 12 to ensure effective holding of the sample;

[0030] After the micro sample 2 is placed on the sample placement platform 13, the left and right parts of the clamping tweezers are fastened together by the clamp 10. The clamping tweezers can prevent the micro sample 2 from falling during the cleaning and polishing process, and also ensure the flatness of the polished surface of the micro sample 2.

[0031] The method of the present invention solves the problems of complicated sample preparation process and low sample resolution of micro samples. The method has a wide range of applications and can be used for samples of all sizes, especially micro EBSD samples. The method is simple to operate, has high preparation efficiency, excellent sample preparation effect, and a sample resolution rate of more than 90%. The method of the present invention has predictable and relatively huge economic and social value. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 Schematic diagram of the V-shaped groove of the mounted sample with the micro-specimen;

[0033] Figure 2 Schematic diagram of the sampling platform structure;

[0034] Figure 3 Schematic diagram of the clamping tweezers structure;

[0035] Figure 4 Schematic diagram of the electrolytic polishing device;

[0036] Figure 5 Schematic diagram of special electrolytic polishing method;

[0037] Figure 6 Schematic diagram of pipe material and sampling method;

[0038] Figure 7 IPF map of EBSD of the sample prepared in Example 1 (resolution: 97%);

[0039] Figure 8 The Kikuchi diffraction pattern of the EBSD analysis of the sample prepared in Example 1;

[0040] Fig. 9 IPF image of EBSD analysis of the sample prepared in Example 2 (resolution: 95%)

[0041] Figure numerals: 1. mounted sample, 2. miniature specimen, 3. V-shaped groove, 4. clamp, 5. arc column, 6. groove hole, 7. bolt, 8. gap, 10. clamp, 11. first tweezers handle, 12. first tweezers head, 13. sample placement platform, 14. baffle plate, 21. second tweezers handle, 22. second tweezers head. DETAILED DESCRIPTION

[0042] Sampling platform structure:

[0043] like Figure 2 As shown, the sampling platform used in the embodiment is composed of two symmetrical clamps 4 and two arc columns 5; a groove hole 6 is provided in the height direction of the clamp 4, and the cross-sectional diameter of the groove hole 6 is larger than the diameter of the mounted sample 1; the arc column 5 can be clamped in the groove hole 6, and its height is smaller than the height of the clamp 4, and the arc column 5 is used to support the mounted sample 1; the arc column 5 is fastened to the clamp 4 by bolts 7, and the two symmetrical clamps 4 are fastened together by bolts 7.

[0044] A bolt 7 is provided at the upper position of the groove hole 6 of the clamp 4. The bolt 7 is arranged parallel to the horizontal direction and is used to fasten the mounted sample 1 placed on the arc column 5 to prevent the mounted sample 1 from moving and scratching the micro-specimen 2 during the smashing process.

[0045] When in use, the arc column 5 is clamped in the groove hole 6, and then the two clamps 4 are arranged with the groove holes 6 on one side facing each other, leaving a gap 8 between the clamps 4, and the mounted sample 1 is placed on the two oppositely arranged arc columns 5, so that the tip connecting line of the V-shaped groove 3 on the mounted sample 1 is located in the gap 8 between the clamps 4; tighten the bolt 7 between the two clamps 4 to clamp the mounted sample 1.

[0046] Clamping tweezers structure:

[0047] like Figure 3As shown, the clamping tweezers used in the embodiment are composed of left and right parts:

[0048] In the left part: the first tweezer handle 11 and the first tweezer head 12 are a straight structure as a whole, a sample-laying platform 13 is provided at the tail of the first tweezer head 12, a baffle plate 14 is provided on the sample-laying platform 13, and the baffle plate 14 is arranged perpendicular to the width direction of the first tweezer head 12;

[0049] In the right part: the second tweezers handle 21 and the second tweezers head 22 are in a broken line structure as a whole. When the tail ends of the first tweezers handle 11 and the second tweezers handle 22 are close to each other, the second tweezers head 22 with the same width as the first tweezers head 12 can be placed on the sample placement platform 13 and parallel to the first tweezers head 12 to ensure effective holding of the sample;

[0050] After the micro-sample 2 is placed on the sample placement platform 13, the left and right parts of the clamping tweezers are fastened together using the clamp 10.

[0051] Example 1

[0052] The nominal composition of Zr-4 alloy is Zr-1.5Sn-0.2Fe-0.1Cr. The alloy has a very low thermal neutron absorption cross section, high hardness, ductility and excellent corrosion resistance. It is mainly used as fuel cladding material in pressurized water reactors, boiling water reactors and heavy water reactors.

[0053] Since the shape of Zr-4 pipe is cylindrical, in order to observe the real grain orientation and structure of the pipe, the surface of the pipe must be tested with the help of EBSD technology, so it is necessary to cut a very small size (pipe sampling such as Figure 6 The sample size is as follows: length = 6mm, width = 0.5mm, thickness = tube thickness. The sample preparation method includes the following steps:

[0054] ① Mounting:

[0055] Use a wire cutting machine to cut out micro sample 2 on the Zr-4 pipe, take a resin amount about twice the thickness of micro sample 2 and put it into the mounting machine to mount it together with the micro sample, mount the micro sample 2 to the center of the mounting, and finally form the mounting sample 1. Do not mount the sample too tightly when mounting;

[0056] ② Open V-shaped groove:

[0057] Two V-shaped grooves 3 similar to those in the impact test are symmetrically opened on the mounted sample 1 by a grinder in a direction perpendicular to the micro-specimen 2. The micro-specimen 2 is located on the line connecting the tips of the two V-shaped grooves 3, which is perpendicular to the length direction of the micro-specimen 2 (e.g. Figure 1 shown);

[0058] ③ Polishing the mounted sample 1: grinding it in turn with 150#, 320#, 800#, and 2000# sandpaper on a grinder; mechanically polishing the ground sample with nano-particle SiO2 polishing liquid on a polisher;

[0059] ④ Stick transparent tape on the surface of micro-specimen 2 and place the mounted sample 1 on the sampling platform;

[0060] ⑤ Fasten the mounted sample 1 in the sampling platform, apply downward force to the center of the mounted sample 1, so that the mounted sample 1 is broken along the line connecting the tips of the V-shaped grooves 3, take out the micro-sample 2, and remove the transparent glue on it;

[0061] ⑥ Place the micro sample 2 on an ultrasonic instrument and clean it with alcohol ultrasonic vibration;

[0062] ⑦ Place the micro sample 2 in an acidic electrolytic polishing solution for electrolytic polishing:

[0063] First, the voltage is used as the main factor, and then the current is used as the main factor: the power supply current is set to 0.8A, the voltage is set to the maximum, which is 60V, and then the electrolytic polishing liquid is cooled to minus 70°C with a refrigerant (preferably liquid ammonia), and the power supply is connected. At this time, the power supply is mainly voltage, and the current is 0.1A. As the temperature rises, the current gradually increases, and the voltage remains unchanged until the current reaches 0.8A. The power supply becomes mainly current, and the current remains unchanged at 0.8A, and the voltage begins to decrease until the voltage is reduced to 50V, then the power supply is turned off, and the micro-sample 2 is taken out; during the electrolytic polishing process, the electrolyte is surrounded by plastic foam for heat preservation;

[0064] ⑧ Rinse the micro sample 2 with water, then rinse it with alcohol and blow it dry, and finally obtain the micro EBSD sample of Zr-4 pipe.

[0065] The IPF image of the Zr-4 pipe micro-sample determined by EBSD technology and the Kikuchi diffraction pattern image of the prepared sample by EBSD analysis are shown as follows: Figure 7 , 8 shown.

[0066] Example 2

[0067] The content of this embodiment is basically the same as that of embodiment 1, except that: the EBSD sample is then prepared in the thickness direction (thickness is 0.3 mm) of the Zr-2 alloy strip by the method described in embodiment 1.

[0068] Zr-2 alloy has good corrosion resistance, moderate mechanical properties, and low atomic thermal neutron absorption cross section (0.18 barns for zirconium) under high temperature and high pressure of 300-400°C and water vapor, and has good compatibility with nuclear fuel. Therefore, it can be used as the core structural material (fuel cladding, pressure tube, bracket and channel tube) of water-cooled nuclear reactors. This is the main use of Zr-2 alloy.

[0069] Since the Zr-2 strip is a thin plate with a thickness of 0.3mm, in order to observe the grain orientation, structure and other information on the thickness surface of the strip, the surface in the thickness direction of the strip must be tested with the help of EBSD technology. The difficulty in preparing the surface EBSD sample in the thickness direction of the strip is that the thickness of the strip is only 0.3mm. The sample size cut this time is: length = 6mm, width = 0.5mm, thickness = thickness of the strip = 0.3mm. The sample preparation method includes the following steps:

[0070] ① Mounting:

[0071] Use a wire cutting machine to cut out micro sample 2 on the Zr-2 alloy strip, take a resin amount about twice the thickness of micro sample 2 and put it into the mounting machine to mount it together with the micro sample, mount the micro sample 2 to the center of the mounting, and finally form the mounting sample 1. Do not mount the sample too tightly when mounting;

[0072] ② Open V-shaped groove:

[0073] Two V-shaped grooves 3 similar to those in the impact test are symmetrically opened on the mounted sample 1 by a grinder in a direction perpendicular to the micro-specimen 2. The micro-specimen 2 is located on the line connecting the tips of the two V-shaped grooves 3, which is perpendicular to the length direction of the micro-specimen 2 (e.g. Figure 1 shown);

[0074] ③ Polishing the mounted sample 1: grinding it in turn with 150#, 320#, 800#, and 2000# sandpaper on a grinder; mechanically polishing the ground sample with nano-particle SiO2 polishing liquid on a polisher;

[0075] ④ Stick transparent tape on the surface of micro-specimen 2 and place the mounted sample 1 on the sampling platform;

[0076] ⑤ Fasten the mounted sample 1 in the sampling platform, apply downward force to the center of the mounted sample 1, so that the mounted sample 1 is broken along the line connecting the tips of the V-shaped grooves 3, take out the micro-sample 2, and remove the transparent glue on it;

[0077] ⑥ Place the micro sample 2 on an ultrasonic instrument and clean it with alcohol ultrasonic vibration;

[0078] ⑦ Place the micro sample 2 in an acidic electrolytic polishing solution for electrolytic polishing:

[0079] First, the voltage is used as the main factor, and then the current is used as the main factor: the power supply current is set to 0.8A, the voltage is set to the maximum, which is 60V, and then the electrolytic polishing liquid is cooled to minus 70°C with a refrigerant (preferably liquid ammonia), and the power supply is connected. At this time, the power supply is mainly voltage, and the current is 0.1A. As the temperature rises, the current gradually increases, and the voltage remains unchanged until the current reaches 0.8A. The power supply becomes mainly current, and the current remains unchanged at 0.8A, and the voltage begins to decrease until the voltage is reduced to 50V, then the power supply is turned off, and the micro-sample 2 is taken out; during the electrolytic polishing process, the electrolyte is surrounded by plastic foam for heat preservation;

[0080] ⑧ Rinse micro sample 2 with water, then rinse with alcohol and blow dry, and finally obtain the micro EBSD sample of Zr-2 strip.

[0081] The IPF image of the Zr-2 strip micro-sample measured by EBSD technology is shown in Fig. 9 shown.

[0082] Matters not covered by the present invention are known technologies.

[0083] The above embodiments are only for illustrating the technical concept and features of the present invention, and their purpose is to enable people familiar with the technology to understand the content of the present invention and implement it accordingly, and they cannot be used to limit the protection scope of the present invention. Any equivalent changes or modifications made according to the spirit of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing a micro EBSD sample by mechanical and electrolytic polishing, characterized in that: The specific steps are as follows: ① Mounting: Cutting the metal material into micro-samples (2), mounting the micro-samples (2) at the center of the mounting sample on a mounting machine, and finally forming a mounting sample (1); ② Open V-shaped groove: Two V-shaped grooves (3) are symmetrically opened on the mounted sample 1 in a direction perpendicular to the micro-specimen (2), and the micro-specimen (2) is located on the connecting line of the tips of the two V-shaped grooves (3); ③ Mechanically polishing the mounted sample (1); ④ A protective layer is applied to the surface of the micro-specimen (2) to prevent scratches, and then the mounted sample (1) is placed in the sampling platform; ⑤ Fasten the mounted sample (1) in the sampling platform, apply downward force to the center of the mounted sample (1), so that the sample is broken along the line connecting the tips of the V-shaped groove (3), take out the micro-sample (2), and remove the protective layer thereon; ⑥ Place the micro sample (2) on an ultrasonic instrument and clean it with alcohol ultrasonic vibration; ⑦ Place the micro sample (2) in an acidic electrolytic polishing solution for electrolytic polishing: The power supply current is set to 0.8A, and the voltage is set to the maximum, which is 60V. Then, the electrolytic polishing liquid is cooled to -70°C with a refrigerant, and the power supply is connected. At this time, the power supply is mainly voltage-based, and the current is 0.1A. As the temperature rises, the current gradually increases, and the voltage remains unchanged until the current reaches 0.8A. The power supply becomes mainly current-based, and the current remains unchanged at 0.8A. The voltage begins to decrease until the voltage is reduced to 50V. Then, the power supply is turned off and the micro-sample (2) is taken out. ⑧ Rinse the micro sample (2) with water and then with alcohol and blow dry, finally obtaining a micro EBSD sample of the metal material; In step ④, the sampling platform is composed of two symmetrical clamps (4) and two arc columns (5); the clamp (4) is provided with a groove hole (6) in the height direction, and the cross-sectional diameter of the groove hole (6) is larger than the diameter of the mounted sample (1); the arc column (5) can be clamped in the groove hole (6), and its height is smaller than the height of the clamp (4), and the arc column (5) is used to support the mounted sample (1); the arc column (5) is fastened to the clamp (4) by bolts (7), and the two symmetrical clamps (4) are fastened together by bolts (7).

2. The method for preparing a micro EBSD sample according to claim 1, characterized in that: In step ①, the micro-sample (2) is rectangular, square, circular, rhombus or pentagonal, and its size range is: length = 0.5-10mm, width = 0.3-10mm, thickness = 0.5-3mm.

3. The method for preparing a micro EBSD sample according to claim 1, characterized in that: In step ①, the thickness of the mounted sample (1) is 2-3 times the thickness of the micro-specimen (2).

4. The method for preparing a micro EBSD sample according to claim 1, characterized in that: In step ③, the sample is ground on a grinder using 150#, 320#, 800#, and 2000# sandpaper in sequence; the ground sample is mechanically polished using a polishing liquid on a polishing machine.

5. The method for preparing a micro EBSD sample according to claim 1, characterized in that: A bolt (7) is provided at an upper position of the groove hole (6) of the clamp (4), and the bolt (7) is arranged parallel to the horizontal direction and is used to fasten the mounted sample (1) placed on the arc column (5).

6. The method for preparing a micro EBSD sample according to claim 1 or 5, characterized in that: The arc column (5) is clamped in the groove hole (6), and then the two clamps (4) are arranged with the sides of the groove holes (6) facing each other, leaving a gap (8) between the clamps (4), and the mounted sample (1) is placed on the two oppositely arranged arc columns (5) so that the tip connecting line of the V-shaped groove (3) of the mounted sample (1) is located at the gap (8) between the clamps (4), and the bolt (7) between the two clamps (4) is tightened so that the mounted sample (1) is clamped.

7. The method for preparing a micro EBSD sample according to claim 1, characterized in that: In step ⑦, the micro-sample (2) is placed in the acid electrolytic polishing solution using clamping tweezers, wherein the clamping tweezers are composed of left and right parts: In the left part: the first tweezer handle (11) and the first tweezer head (12) are integrally a linear structure, a sample-laying platform (13) is provided at the tail of the first tweezer head (12), a baffle plate (14) is provided on the sample-laying platform (13), and the baffle plate (14) is arranged perpendicular to the width direction of the first tweezer head (12); In the right part: the second tweezer handle (21) and the second tweezer head (22) are integrally in a folded line structure. When the tail ends of the first tweezer handle (11) and the second tweezer handle (21) are close together, the second tweezer head (22) having the same width as the first tweezer head (12) can be placed on the sample placement platform (13) and parallel to the first tweezer head (12); After the micro sample (2) is placed on the sample placement platform (13), the left and right parts of the clamping tweezers are fastened together using a clamp (10).

8. The method for preparing a micro EBSD sample according to claim 1, characterized in that: In step ⑦, the electrolyte is surrounded by plastic foam for heat preservation.

9. The method for preparing a micro EBSD sample according to claim 1, characterized in that: In step ⑦, the refrigerant is liquid ammonia.

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