Preparation method of refractory metal reinforced copper-based composite material EBSD sample

Abstract

The invention discloses a preparation method of a refractory metal reinforced copper-based composite material EBSD sample. The method comprises the following steps: 1, carrying out linear cutting to obtain a to-be-treated original sample; 2, performing thermal inlaying on the sample; 3, mechanical grinding; 4, vibration polishing; 5, chemically and mechanically polishing; and sixthly, cleaning and blow-drying are conducted, and the refractory metal reinforced copper-based composite EBSD sample is obtained. Scratches and defects of the sample are removed through vibration polishing, and synergistic regulation and control of the corrosion rate are achieved and tiny corrosion pit defects on the surface of the sample are eliminated by means of the oxidation effect, the complexing effect and the corrosion inhibition effect of the chemical mechanical polishing solution on the two phases of the heterogeneous refractory metal reinforced copper-based composite material. The sample surface is kept in a flat, smooth and low-stress state, the sample surface quality is remarkably improved, the analysis rate of the obtained EBSD sample is high, and the method has the advantages of being practical, efficient and low in cost.

Description

Technical Field

[0001] The invention belongs to the technical field of metal material tissue texture characterization, and particularly relates to a method for preparing an EBSD sample of a refractory metal reinforced copper-based composite material. Background Art

[0002] Refractory metals (such as niobium (Nb), tantalum (Ta), molybdenum (Mo), and tungsten (W)) possess high melting points, high hardness, corrosion resistance, and resistance to high-temperature softening. High-purity copper (Cu) possesses excellent electrical and thermal conductivity and good ductility. Combining these two materials to create refractory metal-reinforced copper-based composites can fully leverage their advantages in high shear modulus and high conductivity, offering broad application prospects in power electronics, aerospace, nuclear power, and defense industries. For example, niobium / tantalum / molybdenum / tungsten phase-reinforced copper alloy sheets can be used in nuclear reactors, semiconductor heat sinks, and transformer circuit breakers, while wires can be used in pulsed high-magnetic field devices (such as copper-niobium conductors used at the Wuhan National Pulsed Magnetic Field Center) and electromagnetic gun coils. This places higher demands on the mechanical and functional properties of refractory metal-reinforced copper-based composites. Although researchers at home and abroad have studied the microstructure, properties, and mechanisms of refractory metal-reinforced copper-based composites, systematic and in-depth correlations between composition and interface orientation characteristics, dislocations, and grain boundary motion remain fundamental research areas. Therefore, there is an urgent need to combine advanced characterization methods to reveal the interface evolution characteristics during material deformation, and provide guidance for the subsequent optimization of its service performance by regulating the interface structure and orientation of the material.

[0003] Basic research plays a crucial role in the development of high-performance refractory metal-reinforced copper-based composites. Electron backscatter diffraction (EBSD) technology is particularly crucial for analyzing the microstructure and texture evolution of composites. High-quality EBSD samples must be smooth, flat, free of oxide layers, free of residual stress, and exhibit good electrical conductivity to ensure subsequent high-precision analysis. Currently, commonly used surface treatment methods for metal EBSD sample preparation include mechanical polishing, electrolytic polishing, and argon ion beam polishing. However, due to the significant differences in physical properties such as hardness and corrosion resistance among the components of refractory metal-reinforced copper-based composites, as well as the significant internal stresses introduced by deformation processing, the preparation of high-quality EBSD samples using these conventional methods faces numerous challenges. Specifically, mechanical polishing, due to its long polishing time, can introduce a deformation layer on the sample surface. Furthermore, the EBSD pattern indexing rate obtained by this method for demarcating heterogeneous interface regions is low and cannot meet testing requirements. For electrolytic polishing, the large corrosion potential difference between the refractory metal and the copper substrate makes it difficult to balance the corrosion rate during electrolysis, resulting in difficulty in simultaneously acquiring crystallographic information from both phases. Although argon ion beam polishing can achieve a high pattern index rate on heterogeneous phases, it may cause ion implantation damage and introduce an amorphous layer, affecting the accuracy of the analysis results. In addition, this method has a long sample preparation cycle (usually several hours), a small calibration area, and high cost.

[0004] Therefore, developing a convenient, efficient, high-pattern indexing rate and low-cost EBSD sample preparation method for refractory metal reinforced copper-based composites is of great significance for promoting the basic research of this material. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to address the deficiencies of the above-mentioned prior art and provide a method for preparing EBSD samples of refractory metal-reinforced copper-based composite materials. This method vibrates and polishes the mechanically ground refractory metal-reinforced copper-based composite material to remove surface grinding scratches, alleviate stress layer defects, and reduce surface roughness. Subsequently, the chemical reaction between the polishing liquid and the sample surface during chemical mechanical polishing triggers the adaptive passivation and synergistic removal of the corrosion inhibitor / complexing agent on the heterogeneous surface, thereby obtaining a high-quality sample surface. While ensuring high resolution, this method solves the problems of difficult composite material EBSD sample preparation, complex procedures, and long cycles caused by the large differences in hardness and corrosion rate between the two phases.

[0006] To solve the above technical problems, the present invention adopts a technical solution: a method for preparing an EBSD sample of a refractory metal reinforced copper-based composite material, characterized in that the method comprises the following steps: Step 1: Cutting the sample: Cut the refractory metal reinforced copper-based composite material into a size that meets the EBSD characterization size to obtain the original sample to be processed; Step 2, hot mounting: hot mounting the original sample to be processed obtained in step 1 to obtain a mounted sample; Step 3: Mechanical grinding: Use 200 # ~2500 # The mounted sample in step 2 is mechanically ground with sandpaper from coarse to fine until the surface is smooth and free of visible scratches, thereby obtaining a ground sample; Step 4, vibration polishing: performing vibration polishing on the ground sample in step 3 to obtain a vibration polished sample; Step 5, chemical mechanical polishing: chemical mechanical polishing is performed on the vibration polished sample in step 4 to obtain a chemical polished sample; the polishing solution used in the chemical mechanical polishing is a mixture of guanidine hydrochloride, silica suspension, hydrogen peroxide, chelating agent, surfactant and deionized water; Step 6: Cleaning: The chemically polished sample in step 5 is ultrasonically cleaned in an ethanol bath and blown dry to obtain an EBSD sample of a refractory metal reinforced copper-based composite material.

[0007] The present invention first performs vibration polishing on the refractory metal reinforced copper-based composite material sample after mechanical grinding, and utilizes the high-frequency friction between the polishing liquid and the sample surface during the vibration polishing process to remove scratches and stress layer defects on the sample surface and reduce the surface roughness. Then, chemical mechanical polishing is introduced for fine processing. The polishing liquid of the chemical mechanical polishing has an oxidation, complexation and corrosion inhibition effect on the two phases in the refractory metal reinforced copper-based composite material, namely the copper matrix and the refractory metal, thereby triggering adaptive passivation and synergistic removal of the heterogeneous surface, effectively regulating the copper removal rate, and realizing synergistic regulation of the corrosion rate and intensity of the heterogeneous two-phase, so that the heterogeneous two-phase corrosion rate is close to 1:1, effectively eliminating the tiny corrosion pit defects generated on the sample surface after grinding, ensuring that the sample surface remains flat, smooth and in a low-stress state, thereby significantly improving the surface quality of the EBSD sample.

[0008] The above-mentioned method for preparing an EBSD sample of a refractory metal reinforced copper-based composite material is characterized in that the dimensions of the original sample to be processed in step 1 are no more than 10 mm × 10 mm × 8 mm in length × width × height.

[0009] The above-mentioned method for preparing an EBSD sample of a refractory metal reinforced copper-based composite material is characterized in that the mounting material used for the hot mounting in step 2 is a conductive hot mounting resin.

[0010] The above-mentioned method for preparing EBSD samples of refractory metal reinforced copper-based composite materials is characterized in that the mechanical grinding process in step 3 is carried out in sequence using 200# , 400 # , 800 # , 1500 # , 2000 # , 2500 # The surface of the mounted sample was ground step by step with sandpaper until the surface was smooth, without pits and visible scratches. The sandpaper and the mounted sample were continuously rinsed with tap water during the step-by-step grinding to remove abrasive particles. The force was applied evenly at each level of grinding until the scratch direction was uniform. Then, the next level of sandpaper was used. The grinding direction was rotated 90° when the next level of sandpaper was used for grinding. The speed of the metallographic grinding and polishing machine used for mechanical grinding was 600 rpm~1000 rpm.

[0011] The above-mentioned method for preparing an EBSD sample of a refractory metal reinforced copper-based composite material is characterized in that the polishing liquid used in the vibration polishing in step 4 is a mixture of a silica suspension and a hydrogen peroxide solution, wherein the silica particle size in the silica suspension is 0.2 μm; the frequency of the vibration polishing is 50 Hz and the time is 60 min.

[0012] The above-mentioned method for preparing EBSD samples of refractory metal reinforced copper-based composite materials is characterized in that the polishing liquid used in the chemical mechanical polishing in step five is composed of: 0.5wt%~1wt% of guanidine hydrochloride, 20wt%~40wt% of silica suspension with a silica particle size of 40nm, 0.1vol%~0.5vol%, 1vol%~3vol% of chelating agent, 1vol%~2vol% of surfactant, and the rest is deionized water. In the polishing liquid used in the chemical mechanical polishing of the present invention, silica is used as an abrasive to remove substances, hydrogen peroxide is used as an oxidizing material to form a soft phase oxide film (such as Cu2O, CuO, Ta2O5) that is easy to remove, guanidine hydrochloride is used as a chelating agent to inhibit copper transition corrosion, and promote the copper-tantalum corrosion rate ratio to be closer, and the chelating agent (glycine) is used as a chelating agent mainly to react with Ta. 5+ Ions form aqueous complexes (Ta2O5· x H2O2), thereby making it easier to expose the new surface of the sample after the removal of silicon dioxide, and the surfactant (betaine) improves the wettability of the polishing liquid, reduces the surface tension and promotes the simultaneous removal of copper and tantalum phases.

[0013] The above-mentioned method for preparing an EBSD sample of a refractory metal reinforced copper-based composite material is characterized in that the polishing disk speed used in the chemical mechanical polishing in step five is 100 rpm~200 rpm, and the polishing time is 30 min~60 min.

[0014] The above-mentioned method for preparing an EBSD sample of a refractory metal reinforced copper-based composite material is characterized in that in step six, the chemically polished sample is ultrasonically cleaned in an ethanol bath, then rinsed with deionized water, and then dehydrated with ethanol and dried with cold air.

[0015] The refractory metal reinforced copper-based composite material of the present invention is derived from at least one of a Cu-Nb composite material with different Nb contents, a Cu-Ta composite material with different Ta contents, a Cu-Mo composite material with different Mo contents, and a Cu-W composite material with different W contents.

[0016] Compared with the prior art, the present invention has the following advantages: 1. The present invention sequentially performs mechanical grinding, vibration polishing, and chemical mechanical polishing on a refractory metal-reinforced copper-based composite material, effectively balancing the corrosion rate difference between the copper matrix and the refractory metal, while ensuring a smooth and flat sample surface and significantly suppressing the relief phenomenon of the heterogeneous interface. The resulting EBSD sample has a Kikuchi pattern calibration rate of greater than 90%, meeting the requirements of high-precision EBSD characterization.

[0017] 2. The present invention performs vibration polishing on the refractory metal reinforced copper-based composite material after mechanical grinding to remove surface grinding scratches, alleviate stress layer defects and reduce surface roughness. By introducing chemical mechanical polishing after vibration polishing to achieve coordinated regulation of heterogeneous structure removal rate, it ensures that the sample surface remains flat, smooth and in a low-stress state, thereby significantly improving the surface quality of EBSD samples.

[0018] 3. The EBSD sample prepared by the present invention has a high resolution rate, is practical, efficient, and low-cost, and is suitable for wide application.

[0019] The technical solution of the present invention is further described in detail below through the accompanying drawings and embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 This is the organizational diagram of the EBSD sample of the tantalum particle reinforced copper-based composite material prepared in Example 2 of the present invention.

[0021] Figure 2 This is the organizational diagram of the EBSD sample of the tantalum particle reinforced copper-based composite material prepared in Comparative Example 1 of the present invention. DETAILED DESCRIPTION

[0022] Example 1 This embodiment includes the following steps: Step 1: Cut the sample: The niobium particle reinforced copper matrix composite material was cut to a size that meets the EBSD characterization requirements by wire-cutting, and the surface oil was cleaned to remove the oil stains. The original sample to be processed was obtained with a size of 10 mm in length × width × height of 10 mm × 10 mm × 5 mm. Step 2, hot mounting: hot mounting the original sample to be processed obtained in step 1 using a conductive hot mounting resin to obtain a mounted sample; Step 3: Mechanical grinding: Place the mounted sample in step 2 on a metallographic grinding and polishing machine, using 200 # , 400 # , 800 # , 1500 # , 2000 # , 2500 # The surface of the mounted sample is ground step by step from coarse to fine with silicon carbide sandpaper until the surface is smooth, without pits and scratches visible to the naked eye. During the step-by-step grinding, the sandpaper and the mounted sample are continuously rinsed with tap water to remove abrasive particles. The force is evenly applied at each level of grinding until the scratch direction is uniform. Then, the next level of sandpaper is used, and the grinding direction is rotated 90° when grinding with the next level of sandpaper. The speed of the metallographic grinder and polisher used for mechanical grinding is 600 rpm to obtain a ground sample. Step 4, vibration polishing: The ground sample in step 3 was cleaned and then vibrated and polished at a frequency of 50 Hz for 60 min. During the vibration polishing process, a mixture of a silica suspension and a hydrogen peroxide solution was added dropwise, wherein the silica particle size in the silica suspension was 0.2 μm and the proportion of the hydrogen peroxide solution was 5 vol%, to obtain a vibration polished sample; Step 5, chemical mechanical polishing: chemical mechanical polishing was performed on the vibration polishing sample in step 4 using a velvet polishing cloth. The polishing disk speed was 100 rpm, the polishing time was 30 min, and the composition of the polishing solution was as follows: 0.5 wt % guanidine hydrochloride, 30 wt % silica suspension with a silica particle size of 40 nm, 0.1 vol % hydrogen peroxide, 3 vol % chelating agent glycine, 1.5 vol % surfactant betaine, and the remainder was deionized water to obtain a chemically polished sample; Step 6: Cleaning: The chemically polished sample in step 5 is ultrasonically cleaned in an ethanol bath, then rinsed with deionized water, dehydrated with ethanol, and dried with cold air to obtain an EBSD sample of a niobium particle reinforced copper-based composite material.

[0023] Example 2 This embodiment includes the following steps: Step 1: Cut the sample: The tantalum particle reinforced copper matrix composite material is cut to a size that meets the EBSD characterization requirements by wire-cutting, and the surface oil is cleaned to remove the oil stains. The original sample to be processed is obtained with a size of 10 mm in length × width × height of 10 mm × 10 mm × 5 mm. Step 2, hot mounting: hot mounting the original sample to be processed obtained in step 1 using a conductive hot mounting resin to obtain a mounted sample; Step 3: Mechanical grinding: Place the mounted sample in step 2 on a metallographic grinding and polishing machine, using 200 # , 400 # , 800 # , 1500 # , 2000 # , 2500 # The surface of the mounted sample is ground step by step from coarse to fine with silicon carbide sandpaper until the surface is flat, without pits and visible scratches. During the step-by-step grinding, the sandpaper and the mounted sample are continuously rinsed with tap water to remove abrasive particles. The force is evenly applied at each level of grinding until the scratch direction is uniform. Then, the next level of sandpaper is used, and the grinding direction is rotated 90° when grinding with the next level of sandpaper. The speed of the metallographic grinder and polisher used for mechanical grinding is 800 rpm to obtain a ground sample. Step 4, vibration polishing: The ground sample in step 3 was cleaned and then vibrated and polished at a frequency of 50 Hz for 60 min. During the vibration polishing process, a mixture of a silica suspension and a hydrogen peroxide solution was added dropwise, wherein the silica particle size in the silica suspension was 0.2 μm and the proportion of the hydrogen peroxide solution was 5 vol%, to obtain a vibration polished sample; Step 5, chemical mechanical polishing: chemical mechanical polishing is performed on the vibration polishing sample in step 4 using a velvet polishing cloth. The polishing disk speed is 200 rpm, the polishing time is 30 min, and the composition of the polishing solution is as follows: 1 wt % guanidine hydrochloride, 20 wt % of a silica suspension with a silica particle size of 40 nm, 0.3 vol % hydrogen peroxide, 3 vol % glycine as a chelating agent, 1 vol % betaine as a surfactant, and the remainder is deionized water to obtain a chemically polished sample; Step 6: Cleaning: The chemically polished sample in step 5 is ultrasonically cleaned in an ethanol bath, then rinsed with deionized water, dehydrated with ethanol, and dried with cold air to obtain an EBSD sample of a tantalum particle reinforced copper-based composite material.

[0024] Figure 1 This is the organizational diagram of the EBSD sample of the tantalum particle reinforced copper-based composite material prepared in this example. The step size is 0.1μm and the resolution is 97.1%. Figure (a) is the IPF map, and Figure (b) shows the Kikuchi band contrast. Figure 1 It can be seen that the grain distribution in the EBSD sample of the tantalum particle reinforced copper-based composite material is relatively uniform, and the analysis results of fine tantalum particles are better.

[0025] Comparative Example 1 This comparative example comprises the following steps: Step 1: Cut the sample: The tantalum particle reinforced copper matrix composite material is cut to a size that meets the EBSD characterization requirements by wire-cutting, and the surface oil is cleaned to remove the oil stains. The original sample to be processed is obtained with a size of 10 mm in length × width × height of 10 mm × 10 mm × 5 mm. Step 2, hot mounting: hot mounting the original sample to be processed obtained in step 1 using a conductive hot mounting resin to obtain a mounted sample; Step 3: Mechanical grinding: Place the mounted sample in step 2 on a metallographic grinding and polishing machine, using 200 # , 400 # , 800 # , 1500 # , 2000 # , 2500 # The surface of the mounted sample is ground step by step from coarse to fine with silicon carbide sandpaper until the surface is flat, without pits and visible scratches. During the step-by-step grinding, the sandpaper and the mounted sample are continuously rinsed with tap water to remove abrasive particles. The force is evenly applied at each level of grinding until the scratch direction is uniform. Then, the next level of sandpaper is used, and the grinding direction is rotated 90° when grinding with the next level of sandpaper. The speed of the metallographic grinder and polisher used for mechanical grinding is 800 rpm to obtain a ground sample. Step 4, vibration polishing: The ground sample in step 3 was cleaned and then vibrated and polished at a frequency of 50 Hz for 60 min. During the vibration polishing process, a mixture of a silica suspension and a hydrogen peroxide solution was added dropwise, wherein the silica particle size in the silica suspension was 0.2 μm and the proportion of the hydrogen peroxide solution was 5 vol%, to obtain a vibration polished sample; Step 5, cleaning: The vibration-polished sample in step 4 is ultrasonically cleaned in an ethanol bath, then rinsed with deionized water, dehydrated with ethanol, and dried with cold air to obtain an EBSD sample of a tantalum particle reinforced copper-based composite material.

[0026] Figure 2 The organizational map step size of the EBSD sample of the tantalum particle reinforced copper-based composite material prepared in this comparative example is 0.1μm, and the resolution is 78.2%. Figure (a) is the IPF map, and Figure (b) shows the Kikuchi band contrast. Figure 2 It can be seen that compared with Example 1, since Comparative Example 1 does not use chemical mechanical polishing, and due to the physical property differences between the copper substrate and the tantalum phase, over-etching pits exist in local copper areas, forming scattered unresolved areas.

[0027] Example 3 This embodiment includes the following steps: Step 1: Cut the sample: The tantalum particle reinforced copper matrix composite material is cut to a size that meets the EBSD characterization requirements by wire-cutting, and the surface oil is cleaned to remove the oil stains. The original sample to be processed is obtained with a size of 10 mm in length × width × height of 10 mm × 10 mm × 5 mm. Step 2, hot mounting: hot mounting the original sample to be processed obtained in step 1 using a conductive hot mounting resin to obtain a mounted sample; Step 3: Mechanical grinding: Place the mounted sample in step 2 on a metallographic grinding and polishing machine, using 200 # , 400 # , 800 # , 1500 # , 2000 # , 2500 # The surface of the mounted sample is ground step by step from coarse to fine with silicon carbide sandpaper until the surface is flat, without pits and visible scratches. During the step-by-step grinding, the sandpaper and the mounted sample are continuously rinsed with tap water to remove abrasive particles. The force is evenly applied at each level of grinding until the scratch direction is uniform. Then, the next level of sandpaper is used, and the grinding direction is rotated 90° when grinding with the next level of sandpaper. The speed of the metallographic grinding and polishing machine used for mechanical grinding is 1000 rpm to obtain a ground sample. Step 4, vibration polishing: The ground sample in step 3 was cleaned and then vibrated and polished at a frequency of 50 Hz for 60 min. During the vibration polishing process, a mixture of a silica suspension and a hydrogen peroxide solution was added dropwise, wherein the silica particle size in the silica suspension was 0.2 μm and the proportion of the hydrogen peroxide solution was 5 vol%, to obtain a vibration polished sample; Step 5, chemical mechanical polishing: chemical mechanical polishing was performed on the vibration polishing sample in step 4 using a velvet polishing cloth. The polishing disk speed was 200 rpm, the polishing time was 60 min, and the composition of the polishing solution was as follows: 1 wt % guanidine hydrochloride, 40 wt % of a silica suspension with a silica particle size of 40 nm, 0.5 vol % hydrogen peroxide, 1 vol % glycine as a chelating agent, 2 vol % betaine as a surfactant, and the remainder was deionized water to obtain a chemically polished sample; Step 6. Cleaning: The chemically polished sample in step 5 is ultrasonically cleaned in an ethanol bath, then rinsed with deionized water, dehydrated with ethanol and dried with cold air to obtain an EBSD sample of a tantalum particle reinforced copper-based composite material.

[0028] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any way. Any simple modification, change and equivalent variation made to the above embodiment based on the essence of the invention technology shall still fall within the scope of protection of the technical solution of the present invention.

Claims

1. A method for preparing EBSD samples of refractory metal reinforced copper-based composite materials, characterized in that: The method comprises the following steps: Step 1: Cutting the sample: Cut the refractory metal reinforced copper-based composite material into a size that meets the EBSD characterization size to obtain the original sample to be processed; Step 2, hot mounting: hot mounting the original sample to be processed obtained in step 1 to obtain a mounted sample; Step 3: Mechanical grinding: Use 200 # ~2500 # The mounted sample in step 2 is mechanically ground with sandpaper from coarse to fine until the surface is smooth and free of visible scratches, thereby obtaining a ground sample; Step 4, vibration polishing: performing vibration polishing on the ground sample in step 3 to obtain a vibration polished sample; Step 5, chemical mechanical polishing: chemical mechanical polishing is performed on the vibration polished sample in step 4 to obtain a chemical polished sample; the polishing solution used in the chemical mechanical polishing is a mixture of guanidine hydrochloride, silica suspension, hydrogen peroxide, chelating agent, surfactant and deionized water; Step 6: Cleaning: The chemically polished sample in step 5 is ultrasonically cleaned in an ethanol bath and blown dry to obtain an EBSD sample of a refractory metal reinforced copper-based composite material.

2. The method for preparing an EBSD sample of a refractory metal reinforced copper-based composite material according to claim 1, wherein: The dimensions of the original sample to be processed in step 1 are no more than 10 mm in length × 10 mm in width × 8 mm in height.

3. The method for preparing an EBSD sample of a refractory metal reinforced copper-based composite material according to claim 1, wherein: The embedding material used in the hot embedding in step 2 is a conductive hot embedding resin.

4. The method for preparing an EBSD sample of a refractory metal reinforced copper-based composite material according to claim 1, wherein: In the mechanical grinding process described in step 3, 200 # , 400 # , 800 # , 1500 # , 2000 # , 2500 # The surface of the mounted sample was ground step by step with sandpaper until the surface was smooth, without pits and visible scratches. The sandpaper and the mounted sample were continuously rinsed with tap water during the step-by-step grinding to remove abrasive particles. The force was applied evenly at each level of grinding until the scratch direction was uniform. Then, the next level of sandpaper was used. The grinding direction was rotated 90° when the next level of sandpaper was used for grinding. The speed of the metallographic grinding and polishing machine used for mechanical grinding was 600 rpm~1000 rpm.

5. The method for preparing an EBSD sample of a refractory metal reinforced copper-based composite material according to claim 1, wherein: The polishing liquid used in the vibration polishing in step 4 is a mixture of a silica suspension and a hydrogen peroxide solution, wherein the silica particle size in the silica suspension is 40 nm; the frequency of the vibration polishing is 50 Hz, and the time is 60 min.

6. The method for preparing an EBSD sample of a refractory metal reinforced copper-based composite material according to claim 1, wherein: The polishing liquid used in the chemical mechanical polishing in step 5 is composed of: 0.5wt%~1wt% of guanidine hydrochloride, 20wt%~40wt% of a silica suspension with a silica particle size of 40nm, 0.1vol%~0.5vol% of hydrogen peroxide, 1vol%~3vol% of a chelating agent, 1vol%~2vol% of a surfactant, and the rest is deionized water.

7. The method for preparing an EBSD sample of a refractory metal reinforced copper-based composite material according to claim 1, characterized in that: The chemical mechanical polishing in step 5 uses a polishing disc with a rotation speed of 100 rpm to 200 rpm, and a polishing time of 30 min to 60 min.

8. The method for preparing an EBSD sample of a refractory metal reinforced copper-based composite material according to claim 1, characterized in that: In step six, the chemically polished sample is ultrasonically cleaned in an ethanol bath, then rinsed with deionized water, dehydrated with ethanol, and dried with cold air.

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