A method for preparing EBSD analysis samples of nickel-based resistance alloy foil.

Abstract

This invention discloses a method for preparing EBSD analysis samples of nickel-based resistance alloy foil, comprising: using stainless steel as the cathode and nickel-based resistance alloy foil as the anode, connected to the negative and positive terminals of a constant current and voltage regulated power supply, respectively; immersing the anode and cathode in an electrolytic polishing solution for electrolytic polishing; the raw materials of the electrolytic polishing solution include phosphoric acid, sulfuric acid, hydrochloric acid, hexadecyltrimethylammonium bromide, and water; after completion, removing the nickel-based resistance alloy foil, washing, and drying. The electrolytic polishing solution used in this invention can effectively remove the stress layer on the surface of the foil, resulting in a smooth and clean surface without continuous corrosion pits. It has advantages such as wide availability of materials, simple preparation, low price, and high calibration rate. The electrolytic polishing method of this invention is easy to operate, requires short sample preparation time, has low cost, and stable results, effectively reducing the hardware requirements for foil EBSD sample preparation and facilitating widespread application.

Description

Technical Field

[0001] This invention relates to the field of material surface treatment technology, specifically to a method for preparing EBSD analysis samples of nickel-based resistance alloy foil. Background Technology

[0002] Nickel-chromium precision resistance alloys possess advantages such as high and stable resistivity, small temperature coefficient of resistance, high thermoelectric potential to copper, and excellent machinability, and have been widely used in aerospace, automotive, and electronic communications fields. As a key material for resistive elements, nickel-chromium-based precision resistance alloys play a decisive role in the performance of the finished product, and the material's properties are closely related to its microstructure.

[0003] EBSD (Electromagnetic Embedded Staining) analysis first requires sample preparation that meets the analytical requirements. The sample surface must be clean, flat, and free of residual stress. Due to the tilt of the sample stage, appropriate size and shape are necessary. Furthermore, good conductivity is crucial for electron microscopy observation; poor conductivity will negatively impact EBSD results. EBSD sample preparation methods include mechanical, chemical, electrolytic, and ion bombardment methods. While numerous methods exist, differences in microstructure and composition exist for each material, leading to varying preparation results. Some methods are even unsuitable for samples of certain shapes and sizes. For foil samples, due to their thinness, mechanical and ion polishing are not feasible. Chemical methods, electrolytic dual-jet methods, or electrolytic polishing are typically chosen. Chemical methods often produce unstable samples, while electrolytic dual-jet methods yield smaller samples, hindering preparation. Therefore, electrolytic polishing is generally preferred. Electrolytic sample preparation plays a decisive role in EBSD experiments, directly impacting the calibration rate. The first factor affecting electrolytic sample preparation is the electrolytic polishing solution, and the second is the electrolytic polishing method, particularly the selection of voltage and current. Currently, domestic researchers mainly use their own prepared electropolishing solutions and electropolishing methods to prepare nickel-chromium precision resistance alloy EBSD samples, but most of these are still in the exploratory stage, with uncertain electrolytic component ratios, uncertain electropolishing parameters, and poor electropolishing effects.

[0004] Chinese patent application CN102539216A discloses a method for preparing electron backscatter diffraction (EBSD) samples of nickel alloys. The process steps are: rough grinding, cleaning, electrolytic polishing, and cleaning. The electrolytic polishing solution is formulated as sulfuric acid:phosphoric acid:methanol = 3-5:0.8-1.2:13-17 (volume ratio). This process is simple and can easily prepare nickel alloy EBSD samples, obtaining clear EBSD orientation images on a scanning electron microscope. However, the foil alloy sample is too thin to undergo extensive mechanical polishing. Furthermore, the polishing solution and method are for bulk materials, and the electrolytic method can lead to excessive corrosion or even melting of the alloy foil during electrolytic polishing. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to provide a method for preparing nickel-based resistance alloy foil EBSD analysis samples, thereby improving the quality and stability of foil EBSD sample preparation.

[0006] The present invention solves the above-mentioned technical problems through the following technical means:

[0007] A method for preparing a nickel-based resistance alloy foil sample for EBSD analysis includes the following steps:

[0008] S1. Stainless steel is used as the cathode and connected to the negative terminal of the constant current regulated power supply; nickel-based resistance alloy foil is used as the anode and connected to the positive terminal of the constant current regulated power supply.

[0009] S2. Immerse the anode and cathode in an electrolytic polishing solution, and then perform electrolytic polishing; the raw materials of the electrolytic polishing solution include phosphoric acid, sulfuric acid, hydrochloric acid, hexadecyltrimethylammonium bromide and water;

[0010] S3. After electrolytic polishing, the nickel-based resistance alloy foil is taken out, washed, and dried to obtain the EBSD analysis sample of the nickel-based resistance alloy foil.

[0011] Preferably, in S2, during the electropolishing process, the electropolishing time is 10-20s, the polishing voltage is 10-15V, the polishing current is 0.5-1A, and the polishing temperature is -20-0℃.

[0012] Preferably, in S2, electropolishing is carried out under stirring conditions, with a stirring speed of 300-350 r / min.

[0013] Preferably, in S2, during the electropolishing process, the distance between the cathode and anode is maintained at 20-30 mm.

[0014] Preferably, in S2, the mass concentration of phosphoric acid is 85%, the mass concentration of sulfuric acid is 98%, the mass concentration of hydrochloric acid is 36%-38%, and per liter of electrolytic polishing solution, the amount of phosphoric acid is 600-650 ml, the amount of sulfuric acid is 150-200 ml, the amount of hydrochloric acid is 10-50 ml, the amount of hexadecyltrimethylammonium bromide is 5-10 mg, and the balance is water.

[0015] Preferably, step S2 further includes pouring liquid nitrogen into the electropolishing solution.

[0016] Preferably, in S1, a nickel-based resistance alloy foil is attached to a glass plate as the anode.

[0017] Preferably, in S2, the anode and cathode are placed parallel to each other and immersed in the electrolytic polishing solution.

[0018] Preferably, in S1, the stainless steel is 304 stainless steel; in S3, the washing includes rinsing with deionized water, rinsing with anhydrous ethanol, and then ultrasonic cleaning in anhydrous ethanol; the drying temperature is 30-50°C.

[0019] The advantages of this invention are:

[0020] The electrolytic polishing solution used in this invention can effectively remove the stress layer on the surface of the foil. After polishing, the surface is smooth and clean, without continuous corrosion pits. It has the advantages of wide material availability, simple preparation, low price, and high calibration rate. The electrolytic polishing method of this invention is easy to operate, requires a short sample preparation time, has low cost, and stable effect. It can effectively reduce the hardware requirements for foil EBSD sample preparation and is easy to promote. Attached Figure Description

[0021] Figure 1 The image quality (IQ) map of the 20μm cold-rolled nickel-chromium-aluminum-copper resistance alloy foil sample after electrolytic polishing in Example 1 of this invention is shown in the EBSD analysis.

[0022] Figure 2 This is an image quality (IQ) plot of the EBSD analysis of the 20μm annealed nickel-chromium-aluminum-copper resistance alloy foil sample after electrolytic polishing in Example 2 of the present invention;

[0023] Figure 3 This is an image quality (IQ) plot of the EBSD analysis of the 50μm cold-rolled nickel-chromium-aluminum-copper resistance alloy foil sample after electrolytic polishing in Example 3 of the present invention;

[0024] Figure 4 This is an image quality (IQ) plot of the EBSD analysis of the 5μm cold-rolled nickel-chromium-aluminum-copper resistance alloy foil sample after electrolytic polishing in Example 4 of this invention;

[0025] Figure 5 The image quality (IQ) map of the EBSD analysis of the 100μm cold-rolled nickel-chromium-aluminum-copper resistance alloy foil sample after electrolytic polishing in Example 5 of the present invention;

[0026] Figure 6 The image quality (IQ) of the EBSD analysis of the 20μm annealed nickel-chromium-aluminum-copper resistance alloy foil sample after electropolishing in Comparative Example 1 of this invention;

[0027] Figure 7 The image quality (IQ) map of the 20μm cold-rolled nickel-chromium-aluminum-copper resistance alloy foil sample after chemical polishing in Comparative Example 2 of this invention is shown in the EBSD analysis.

[0028] Figure 8 The image quality (IQ) map of the 5μm cold-rolled nickel-chromium-aluminum-copper resistance alloy foil sample after electrolytic polishing in Comparative Example 3 of this invention is shown in the EBSD analysis.

[0029] Figure 9 This is an image quality (IQ) plot of the EBSD analysis of the 20μm cold-rolled nickel-chromium-aluminum-copper resistance alloy foil sample after electrolytic polishing in Comparative Example 4 of this invention. Detailed Implementation

[0030] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0031] Unless otherwise specified, all test materials and reagents used in the following examples are commercially available.

[0032] Unless otherwise specified in the embodiments, the techniques or conditions described in the literature in this field or in accordance with the product manual may be followed.

[0033] Example 1

[0034] In this embodiment, a 20μm thick cold-rolled nickel-chromium-aluminum-copper precision resistance alloy foil was electropolished to obtain an EBSD analysis sample. The composition of each component in the electropolishing solution was as follows: 650ml of 85% phosphoric acid, 200ml of 98% sulfuric acid, 50ml of 36%–38% hydrochloric acid, 5mg of hexadecyltrimethylammonium bromide, and the remainder being deionized water. The process included the following steps:

[0035] (1) Place the magnetic stirrer rotor in a beaker, pour the electrolytic polishing solution into the beaker, and the polishing solution should be able to completely immerse the sample without affecting the height of the magnetic stirrer rotor. Place the beaker on the magnetic stirrer and pour liquid nitrogen into the electrolytic polishing solution to control the temperature of the electrolytic polishing solution at -20℃.

[0036] (2) Using a 304 stainless steel sheet as the cathode, connect it to the negative terminal of the constant current regulated power supply, and attach the foil to the glass plate and connect it to the positive terminal of the constant current regulated power supply.

[0037] (3) Before electropolishing, place the foil attached to the glass plate and the stainless steel plate in parallel and immerse them in the electropolishing solution. Maintain a distance of 20 mm between the two electrodes. Control the voltage of the constant current and voltage power supply at 15V. Then start electropolishing. During the electropolishing process, control the current at 0.8A and the electropolishing time at 10s. Use magnetic stirring at a stirring speed of 350r / min.

[0038] (4) After electropolishing, the foil sample is quickly taken out, rinsed with deionized water 3 times, then rinsed with anhydrous ethanol 3 times, then ultrasonically cleaned for 20 seconds, and then dried in a drying oven at 30°C.

[0039] Figure 1 This is the IQ plot of the EBSD analysis of the 20μm cold-rolled nickel-chromium-aluminum-copper resistance alloy foil sample after electrolytic polishing in Example 1. Figure 1 It can be seen that the image is clear and the representation effect is good.

[0040] Example 2

[0041] In this embodiment, an EBSD analysis sample was obtained by electropolishing a 20μm thick annealed nickel-chromium-aluminum-copper precision resistance alloy foil. The composition of each component in the electropolishing solution was as follows: 600ml of 85% phosphoric acid, 150ml of 98% sulfuric acid, 10ml of 36%–38% hydrochloric acid, 8mg of hexadecyltrimethylammonium bromide, and the remainder being deionized water. The process included the following steps:

[0042] (1) Place the magnetic stirrer rotor in a beaker, pour the electrolytic polishing solution into the beaker, and the polishing solution should be able to completely immerse the sample without affecting the height of the magnetic stirrer rotor. Place the beaker on the magnetic stirrer and pour liquid nitrogen into the electrolytic polishing solution to control the temperature of the electrolytic polishing solution at 0℃.

[0043] (2) Using a 304 stainless steel sheet as the cathode, connect it to the negative terminal of the constant current regulated power supply, and attach the foil to the glass plate and connect it to the positive terminal of the constant current regulated power supply.

[0044] (3) Before electropolishing, place the foil attached to the glass plate and the stainless steel plate in parallel and immerse them in the electropolishing solution. Maintain a distance of 20 mm between the two electrodes. Control the voltage of the constant current and voltage power supply at 10V. Then start electropolishing. During the electropolishing process, control the current at 0.5A and the electropolishing time at 10s. Use magnetic stirring at a speed of 300r / min.

[0045] (4) After electrolytic polishing, the foil sample is quickly taken out, rinsed with deionized water 3 times, then rinsed with anhydrous ethanol 3 times, then ultrasonically cleaned for 20 seconds, and then dried in a drying oven at 50°C.

[0046] Figure 2 The image is the IQ plot of the EBSD analysis of the 20μm annealed nickel-chromium-aluminum-copper resistance alloy foil sample after electrolytic polishing in Example 2. The image is clear and the characterization effect is good.

[0047] Example 3

[0048] In this embodiment, a 50μm thick cold-rolled nickel-chromium-aluminum-copper precision resistance alloy foil was electropolished to obtain an EBSD analysis sample. The composition of each component in the electropolishing solution was as follows: 650ml of 85% phosphoric acid, 180ml of 98% sulfuric acid, 30ml of 36%–38% hydrochloric acid, 6mg of hexadecyltrimethylammonium bromide, and the remainder being deionized water. The process included the following steps:

[0049] (1) Place the magnetic stirrer rotor in a beaker, pour the electrolytic polishing solution into the beaker, and the polishing solution should be able to completely immerse the sample without affecting the height of the magnetic stirrer rotor. Place the beaker on the magnetic stirrer and pour liquid nitrogen into the electrolytic polishing solution to control the temperature of the electrolytic polishing solution at -10℃.

[0050] (2) Using a 304 stainless steel sheet as the cathode, connect it to the negative terminal of the constant current regulated power supply, and attach the foil to the glass plate and connect it to the positive terminal of the constant current regulated power supply.

[0051] (3) Before electropolishing, place the foil attached to the glass plate and the stainless steel plate in parallel and immerse them in the electropolishing solution. Maintain a distance of 20 mm between the two electrodes. Control the voltage of the constant current and voltage power supply at 15V. Then start electropolishing. During the electropolishing process, control the current at 1.0A and the electropolishing time at 15s. Use magnetic stirring at a stirring speed of 350r / min.

[0052] (4) After electrolytic polishing, the foil sample is quickly taken out, rinsed with deionized water 3 times, then rinsed with anhydrous ethanol 3 times, then ultrasonically cleaned for 20 seconds, and then dried in a drying oven at 50°C.

[0053] Figure 3 The image is an IQ plot of the EBSD analysis of the 50μm cold-rolled nickel-chromium-aluminum-copper resistance alloy foil sample after electrolytic polishing in Example 3. The image is clear and the characterization effect is good.

[0054] Example 4

[0055] In this embodiment, a 5μm thick cold-rolled nickel-chromium-aluminum-copper precision resistance alloy foil was electropolished to obtain an EBSD analysis sample. The composition of each component in the electropolishing solution was as follows: 650ml of 85% phosphoric acid, 180ml of 98% sulfuric acid, 30ml of 36%–38% hydrochloric acid, 5mg of cetyltrimethylammonium bromide, and the remainder being deionized water. The process included the following steps:

[0056] (1) Place the magnetic stirrer rotor in a beaker, pour the electrolytic polishing solution into the beaker, and the polishing solution should be able to completely immerse the sample without affecting the height of the magnetic stirrer rotor. Place the beaker on the magnetic stirrer and pour liquid nitrogen into the electrolytic polishing solution to control the temperature of the electrolytic polishing solution at -15℃.

[0057] (2) Using a 304 stainless steel sheet as the cathode, connect it to the negative terminal of the constant current regulated power supply, and attach the foil to the glass plate and connect it to the positive terminal of the constant current regulated power supply.

[0058] (3) Before electropolishing, place the foil attached to the glass plate and the stainless steel plate in parallel and immerse them in the electropolishing solution. Maintain a distance of 30 mm between the two electrodes. Control the voltage of the constant current and voltage power supply at 10V. Then start electropolishing. During the electropolishing process, control the current at 0.5A and the electropolishing time at 15s. Use magnetic stirring at a speed of 300r / min.

[0059] (4) After electropolishing, the foil sample is quickly taken out, rinsed with deionized water 3 times, then rinsed with anhydrous ethanol 3 times, then ultrasonically cleaned for 20 seconds, and then dried in a drying oven at 50°C.

[0060] Figure 4 The image shows the IQ plot of the EBSD analysis of the 5μm cold-rolled nickel-chromium-aluminum-copper resistance alloy sample after electrolytic polishing in Example 4. The image is clear and the characterization effect is good.

[0061] Example 5

[0062] In this embodiment, a 100μm thick cold-rolled nickel-chromium-aluminum-copper precision resistance alloy foil was electropolished to obtain an EBSD analysis sample. The composition of each component in the electropolishing solution was as follows: 650ml of 85% phosphoric acid, 150ml of 98% sulfuric acid, 30ml of 36%–38% hydrochloric acid, 10mg of hexadecyltrimethylammonium bromide, and the remainder being deionized water. The process included the following steps:

[0063] (1) Place the magnetic stirrer rotor in a beaker, pour the electrolytic polishing solution into the beaker, and the polishing solution should be able to completely immerse the sample without affecting the height of the magnetic stirrer rotor. Place the beaker on the magnetic stirrer and pour liquid nitrogen into the electrolytic polishing solution to control the temperature of the electrolytic polishing solution at -20℃.

[0064] (2) Using a 304 stainless steel sheet as the cathode, connect it to the negative terminal of the constant current regulated power supply, and attach the foil to the glass plate and connect it to the positive terminal of the constant current regulated power supply.

[0065] (3) Before electropolishing, place the foil attached to the glass plate and the stainless steel plate in parallel and immerse them in the electropolishing solution. Maintain a distance of 25mm between the two electrodes. Control the voltage of the constant current and voltage power supply at 15V. Then start electropolishing. During the electropolishing process, control the current at 1A and the electropolishing time at 20s. Use magnetic stirring at a speed of 320r / min.

[0066] (4) After electropolishing, the foil sample is quickly taken out, rinsed with deionized water 3 times, then rinsed with anhydrous ethanol 3 times, then ultrasonically cleaned for 20 seconds, and then dried in a drying oven at 50°C.

[0067] Figure 5 The image shown is the IQ plot of the EBSD analysis of the 100μm cold-rolled nickel-chromium-aluminum-copper resistance alloy foil sample after electrolytic polishing in Example 5. The image is clear and the characterization effect is good.

[0068] Comparative Example 1

[0069] In this comparative example, 20 μm thick annealed nickel-chromium-aluminum-copper precision resistance alloy foil was electropolished using the method reported in the literature "Preparation and Microstructure and Properties Study of NiCrAlFe Alloy Thin Strips" (Master's Thesis, Lanzhou University of Technology, Zhou Shengrui). The composition of each component in the electropolishing solution was: perchloric acid 50 ml / L, with the remainder being anhydrous ethanol. The process included the following steps:

[0070] (1) Place the magnetic stirrer rotor in the beaker, pour the electrolytic polishing solution into the beaker, and the polishing solution should be able to completely immerse the sample without affecting the height of the magnetic stirrer rotor. Place the beaker on the magnetic stirrer and pour liquid nitrogen into the beaker to control the temperature of the electrolytic polishing solution at -20℃.

[0071] (2) Using a 304 stainless steel sheet as the cathode, connect it to the negative terminal of the constant current regulated power supply, and attach the foil to the glass plate and connect it to the positive terminal of the constant current regulated power supply.

[0072] (3) Before electropolishing, place the foil attached to the glass plate and the stainless steel plate in parallel and immerse them in the electropolishing solution. Maintain a distance of 20 mm between the two electrodes. Control the voltage of the constant current and voltage power supply at 30 V. Then start electropolishing. Control the electropolishing time at 10 s and use magnetic stirring at a stirring speed of 400 r / min.

[0073] (4) After electrolytic polishing, the foil sample is quickly taken out, rinsed with deionized water 3 times, then rinsed with anhydrous ethanol 3 times, then ultrasonically cleaned for 20 seconds, and then dried in a drying oven at 50°C.

[0074] Figure 6 The image is an IQ plot of the EBSD analysis of the 20μm annealed nickel-chromium-aluminum-copper resistance alloy foil sample after electropolishing in Comparative Example 1. The image is not clear and the characterization effect is not good.

[0075] Comparative Example 2

[0076] In this comparative example, a 20μm thick cold-rolled nickel-chromium-aluminum-copper precision resistance alloy foil was chemically polished using the method reported in the literature "Study on the Microstructure Evolution and Mechanical Properties of Cr20Ni80 Electrothermal Alloy Wire during Processing" (Master's Thesis, Lanzhou University of Technology, Zhao Langlang). The composition of each component in the chemical polishing solution was: 600 ml / L of 85% phosphoric acid, 200 ml / L of 69% nitric acid, and 200 ml / L of 98% sulfuric acid. The process included the following steps:

[0077] (1) Add the above chemical polishing liquid to a beaker, place the beaker in a water bath furnace, and ensure the temperature is 80℃;

[0078] (2) During chemical polishing, the foil is immersed in the chemical polishing solution and kept for about 30 seconds.

[0079] (3) After chemical polishing, the foil sample is quickly taken out, rinsed with deionized water 3 times, then rinsed with anhydrous ethanol 3 times, then ultrasonically cleaned for 20 seconds, and then dried in a drying oven at 50°C.

[0080] Figure 7The image shown is the IQ plot of the EBSD analysis of the 20μm cold-rolled nickel-chromium-aluminum-copper resistance alloy foil sample in Comparative Example 2 after chemical polishing. The image is not clear and the characterization effect is not good.

[0081] Comparative Example 3

[0082] In this comparative example, a 5μm thick cold-rolled nickel-chromium-aluminum-copper precision resistance alloy foil was electropolished. The electropolishing solution used was formulated as follows: 98% sulfuric acid: 85% phosphoric acid: methanol = 5:1.2:17 (volume ratio). The process included the following steps:

[0083] (1) Place the magnetic stirrer rotor in a beaker, pour the electrolytic polishing solution into the beaker, and the polishing solution should be able to completely immerse the sample without affecting the height of the magnetic stirrer rotor. Place the beaker on the magnetic stirrer and pour liquid nitrogen into the electrolytic polishing solution to control the temperature of the electrolytic polishing solution at -20℃.

[0084] (2) Using a 304 stainless steel sheet as the cathode, connect it to the negative terminal of the constant current regulated power supply, and attach the foil to the glass plate and connect it to the positive terminal of the constant current regulated power supply.

[0085] (3) Before electropolishing, place the foil attached to the glass plate and the stainless steel plate in parallel and immerse them in the electropolishing solution. Maintain a distance of 20 mm between the two electrodes. Control the voltage of the constant current and voltage power supply at 15V. Then start electropolishing. During the electropolishing process, control the current at 0.8A and the electropolishing time at 10s. Use magnetic stirring at a stirring speed of 350r / min.

[0086] (4) After electrolytic polishing, the foil sample is quickly taken out, rinsed with deionized water 3 times, then rinsed with anhydrous ethanol 3 times, then ultrasonically cleaned for 20 seconds, and then dried in a drying oven at 50°C.

[0087] Figure 8 The image shows the IQ plot of the EBSD analysis of the 5μm cold-rolled nickel-chromium-aluminum-copper resistance alloy foil sample after electrolytic polishing in Comparative Example 3. Figure 8 It can be seen that the image is not clear and the representation effect is poor.

[0088] Comparative Example 4

[0089] In this comparative example, 20μm thick annealed nickel-chromium-aluminum-copper precision resistance alloy foil was electrolytically polished. The composition of each liter of the electrolytic polishing solution was: 650ml of 85% phosphoric acid, 200ml of 98% sulfuric acid, and the remainder being deionized water. The process included the following steps:

[0090] (1) Place the magnetic stirrer rotor in a beaker, pour the electrolytic polishing solution into the beaker, and the polishing solution should be able to completely immerse the sample without affecting the height of the magnetic stirrer rotor. Place the beaker on the magnetic stirrer and pour liquid nitrogen into the electrolytic polishing solution to control the temperature of the electrolytic polishing solution at -20℃.

[0091] (2) Using a 304 stainless steel sheet as the cathode, connect it to the negative terminal of the constant current regulated power supply, and attach the foil to the glass plate and connect it to the positive terminal of the constant current regulated power supply.

[0092] (3) Before electropolishing, place the foil attached to the glass plate and the stainless steel plate in parallel and immerse them in the electropolishing solution. Maintain a distance of 20 mm between the two electrodes. Control the voltage of the constant current and voltage power supply at 15V. Then start electropolishing. During the electropolishing process, control the current at 0.8A and the electropolishing time at 10s. Use magnetic stirring at a stirring speed of 350r / min.

[0093] (4) After electrolytic polishing, the foil sample is quickly taken out, rinsed with deionized water 3 times, then rinsed with anhydrous ethanol 3 times, then ultrasonically cleaned for 20 seconds, and then dried in a drying oven at 50°C.

[0094] Figure 9 The image shows the IQ plot of the EBSD analysis of the 20μm annealed nickel-chromium-aluminum-copper resistance alloy foil sample from Example 4 after electrolytic polishing. Figure 9 It can be seen that the image is clear, but the calibration rate is not high.

[0095] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing EBSD analysis samples of nickel-based resistance alloy foil, characterized in that: Includes the following steps: S1. Stainless steel is used as the cathode and connected to the negative terminal of the constant current regulated power supply; nickel-based resistance alloy foil is used as the anode and connected to the positive terminal of the constant current regulated power supply. S2. Immerse the anode and cathode in the electrolytic polishing solution, and then perform electrolytic polishing. The raw materials of the electrolytic polishing solution include phosphoric acid, sulfuric acid, hydrochloric acid, hexadecyltrimethylammonium bromide, and water. The content of each component per liter of electrolytic polishing solution is as follows: 600-650 ml of phosphoric acid with a mass concentration of 85%, 150-200 ml of sulfuric acid with a mass concentration of 98%, 10-50 ml of hydrochloric acid with a mass concentration of 36%~38%, 5-10 mg of hexadecyltrimethylammonium bromide, and the remainder is water. S3. After electrolytic polishing, the nickel-based resistance alloy foil is taken out, washed, and dried to obtain the EBSD analysis sample of the nickel-based resistance alloy foil.

2. The method for preparing EBSD analysis samples of nickel-based resistance alloy foil according to claim 1, characterized in that: In S2, during the electropolishing process, the electropolishing time is 10~20s, the polishing voltage is 10~15V, the polishing current is 0.5~1A, and the polishing temperature is -20~0℃.

3. The method for preparing EBSD analysis samples of nickel-based resistance alloy foil according to claim 1, characterized in that: In S2, electropolishing is carried out under stirring conditions at a stirring speed of 300~350 r / min.

4. The method for preparing EBSD analysis samples of nickel-based resistance alloy foil according to claim 1, characterized in that: In S2, during the electropolishing process, a distance of 20-30 mm is maintained between the cathode and anode.

5. The method for preparing EBSD analysis samples of nickel-based resistance alloy foil according to claim 1, characterized in that: S2 also includes pouring liquid nitrogen into the electropolishing solution.

6. The method for preparing EBSD analysis samples of nickel-based resistance alloy foil according to claim 1, characterized in that: In S1, a nickel-based resistance alloy foil is attached to a glass plate as the anode.

7. The method for preparing EBSD analysis samples of nickel-based resistance alloy foil according to claim 1, characterized in that: In S2, the anode and cathode are placed parallel to each other and immersed in the electrolytic polishing solution.

8. The method for preparing EBSD analysis samples of nickel-based resistance alloy foil according to any one of claims 1-7, characterized in that: In S1, the stainless steel is 304 stainless steel; in S3, the washing includes rinsing with deionized water, rinsing with anhydrous ethanol, and then ultrasonic cleaning in anhydrous ethanol; the drying temperature is 30~50℃.

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