Sample preparation method for CoZrTaB target material SEM detection

Abstract

The invention relates to a CoZrTaB target material SEM detection sample preparation method, which comprises: sequentially carrying out linear cutting, first grinding, second grinding, mechanical polishing, chemical polishing and surface electric conduction treatment on a CoZrTaB target material to obtain a to-be-detected sample, according to the sample preparation method, the surface flatness of the obtained to-be-detected sample is improved, the surface roughness is preferably as low as 5.0 nm or below, no impurity is introduced, the edge of the sample is not cracked or deformed, and the analysis requirement of the CoZrTaB target material on a high-precision microstructure structure is met.

Description

Technical Field

[0001] This invention relates to the field of target material and SEM sample preparation technology, and in particular to a sample preparation method for SEM detection of CoZrTaB target material. Background Technology

[0002] CoZrTaB targets have broad application prospects in electronic components, high-frequency magnetic devices, and advanced electronic devices due to their excellent magnetic properties, tunable thin film performance, and good synergistic effects with other non-magnetic materials (such as SiO2 or Al2O3). The microstructure, surface quality, and compositional uniformity of CoZrTaB targets directly affect their performance. Therefore, SEM inspection of CoZrTaB targets is an indispensable step, providing important technical support for target preparation, performance optimization, and quality control.

[0003] Currently, the main methods for preparing SEM samples of traditional metal targets involve mechanical cutting, progressive grinding, and mechanical polishing. Specifically, mechanical cutting typically uses ordinary metal cutting machines with cutting fluid as the cooling medium; during grinding, silicon carbide sandpaper of varying coarseness is used for manual grinding; and polishing is accomplished solely by using a mechanical polishing machine in conjunction with diamond polishing paste. However, although this method can prepare samples that can be observed by SEM to a certain extent, it has defects in various aspects such as cutting, cleaning, demagnetizing, chemical etching, ion beam treatment and coating due to insufficient consideration of the special characteristics of CoZrTaB target. Specifically: (1) Ordinary cutting fluid cannot effectively suppress the generation of high temperature when cutting CoZrTaB target, and some chemical components in the cutting fluid may react with the target and contaminate the sample surface; (2) Manual grinding is difficult to control the pressure and grinding direction precisely, resulting in poor sample surface flatness and uneven removal of the damaged layer; (3) Simple mechanical polishing cannot completely eliminate the small deformation layer generated during the grinding process. Under high magnification SEM observation, the residual defects on the sample surface will still have a significant impact on the imaging quality, and cannot provide high-quality SEM observation samples that meet the requirements of high-precision analysis for CoZrTaB target.

[0004] For example, CN112067643A discloses a sample preparation method for SEM detection of the welding diffusion layer of a high-purity aluminum target assembly. The sample preparation method includes the following steps: first, the sample is polished sequentially in the first, second, and third stages until the surface is free of scratches; then, the polished sample is placed in a copper-containing solution for treatment, followed by cleaning to obtain the sample to be tested. The first, second, and third polishing stages are performed using sandpaper from coarse to fine, which can easily damage the sample surface and cannot meet the requirements of high-precision analysis of CoZrTaB target materials. Therefore, it is not suitable for the preparation of CoZrTaB target material SEM samples.

[0005] Therefore, how to develop a sample preparation method specifically for SEM detection of high-purity CoZrTaB targets, and prepare high-quality SEM samples that allow clear observation of the microstructure of CoZrTaB targets without introducing additional impurities, is a technical problem that urgently needs to be solved in this field. Summary of the Invention

[0006] To address the aforementioned technical problems, this invention provides a sample preparation method for SEM detection of CoZrTaB targets. Specifically for high-purity CoZrTaB targets, this method prepares SEM samples with high surface smoothness, no impurity introduction, and no edge chipping or deformation. This solves the problems of existing general metal target SEM detection sample preparation methods, which suffer from easy sample damage, low surface smoothness, easy introduction of impurities, and easy edge chipping or deformation when applied to high-purity CoZrTaB targets due to impurities.

[0007] To achieve this objective, the present invention adopts the following technical solution:

[0008] This invention provides a sample preparation method for SEM detection of CoZrTaB target material, the sample preparation method comprising the following steps:

[0009] The CoZrTaB target material is sequentially subjected to wire cutting, first grinding, second grinding, mechanical polishing, chemical polishing, and surface conductive treatment to obtain the sample to be tested.

[0010] For high-purity CoZrTaB targets, this invention employs a series of processes including wire cutting, first grinding, second grinding, mechanical polishing, chemical polishing, and surface conductive treatment. These processes work synergistically to improve the surface smoothness of the prepared sample, prevent the introduction of additional impurities, enhance SEM imaging results, and ensure that there is no chipping or deformation at the edges. This solves the problem that existing SEM sample preparation methods for general metal targets cannot meet the requirements for high-quality, high-precision microstructure analysis of high-purity CoZrTaB targets.

[0011] The high-purity CoZrTaB target material mentioned in this invention refers to CoZrTaB target material with a purity of 4N or higher. It has special characteristics such as complex composition, easy oxidation, sensitivity to surface damage, and high requirements for microstructure analysis. Therefore, it is necessary to provide a sample preparation method suitable for SEM detection of high-purity CoZrTaB target material.

[0012] Specifically, this includes: (1) CoZrTaB is a multi-element alloy, in which Zr and Ta are highly active metals that easily form oxide films in the air (such as ZrO2 and Ta2O5), and the presence of B element will enhance the chemical activity of the material; if the heat dissipation during the grinding / polishing process is insufficient in the conventional sample preparation (such as dry grinding or insufficient cooling), the surface oxidation will be accelerated due to frictional heat generation, and the formed oxide layer will cover the true microstructure of the target material (such as grain boundaries and phase distribution), resulting in the distortion of SEM observation results; (2) High purity is sensitive to impurity contamination. When the purity of the target material reaches 4N or above, any external impurities (such as abrasive particles from sandpaper, polishing paste residue, or minerals in the cleaning water) will become "interference sources" for SEM observation. In the conventional sample preparation process, if the cleaning is not thorough (such as only (Using tap water to rinse) or using low-purity grinding media can easily introduce micron- or even nano-sized impurities. Under high-magnification SEM (such as 100,000 times or more), these impurities will be misjudged as the second phase or defects of the target material itself; (3) High precision requirements for microstructure analysis. The application scenarios of the high-purity CoZrTaB target material (such as sputtering to prepare thin films) have extremely high requirements for the uniformity of its internal microstructure (such as grain size, phase uniformity or porosity). It is necessary to observe submicron- or even nano-sized details through SEM; In conventional sample preparation, if the mechanical polishing pressure is too high or the sandpaper mesh is insufficient, a "deformation layer" (the plastic deformation area of ​​the material caused by mechanical stress) will be formed on the surface, or deep scratches will remain. These defects will cover up the true microstructure, leading to misjudgment of grain size and phase distribution.

[0013] Preferably, the purity of the CoZrTaB target is ≥4N, for example, it can be 4N, 4.2N, 4.5N, 4.8N or 5N.

[0014] Preferably, the density of the CoZrTaB target is ≥98%, for example, it can be 98%, 98.5%, 99% or 99.5%, etc.

[0015] Preferably, the mass ratio of Co, Zr, Ta and B in the CoZrTaB target is (60-70):(10-15):(15-20):(1-5), for example, it can be 60:10:15:1, 65:12:18:5, 60:15:20:5, 70:10:18:2 or 70:15:20:5, etc.

[0016] Preferably, the cooling medium used in the wire cutting includes deionized water.

[0017] Preferably, the wire cutting speed is 10-20 mm / min, for example, it can be 10 mm / min, 12 mm / min, 14 mm / min, 16 mm / min, 18 mm / min or 20 mm / min, etc.

[0018] The present invention further preferably uses deionized water as the cooling medium for wire cutting, and further preferably uses a cutting speed of 10-20 mm / min. The two work synergistically to improve sample quality. Compared with chemical cutting fluid, it can remove heat during the cutting process in a timely manner, avoiding thermal damage to the sample. At the same time, it avoids the problem of chemical components reacting with the CoZrTaB target to generate impurities that interfere with SEM imaging. If the cutting speed of the wire cutting is too fast, it is easy to cause chipping and deformation of the sample edges; if the cutting speed of the wire cutting is too slow, it consumes a lot of time and reduces efficiency.

[0019] Preferably, the first grinding and the second grinding are performed on a grinding disc.

[0020] The present invention further preferably performs the first grinding and the second grinding on a grinding disc. Compared with the traditional method of directly grinding by hand with sandpaper, the present invention can reasonably control the grinding pressure and grinding direction, so that the grinding is more uniform and further improves the surface flatness of the sample.

[0021] Preferably, the rotational speed of the grinding disc during the first grinding process is 150 to 250 r / min, for example, it can be 150 r / min, 170 r / min, 200 r / min, 220 r / min or 250 r / min, etc.

[0022] Preferably, the sandpaper used for the first grinding has a grit size of 200 to 400 mesh, such as 200 mesh, 220 mesh, 250 mesh, 280 mesh, 300 mesh, 320 mesh, 350 mesh, 380 mesh or 400 mesh, etc.

[0023] Preferably, a first pressure is applied during the first grinding process, and the first pressure is preferably 50 to 150 Pa, for example, it can be 50 Pa, 80 Pa, 100 Pa, 120 Pa or 150 Pa.

[0024] Preferably, the first grinding time is 5 to 10 minutes, for example, it can be 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes or 10 minutes.

[0025] Preferably, the rotational speed of the grinding disc during the second grinding process is 100-150 r / min, for example, it can be 100 r / min, 110 r / min, 120 r / min, 130 r / min, 140 r / min or 150 r / min, etc.

[0026] Preferably, the sandpaper used for the second grinding has a grit size of 800 to 1200 mesh, such as 800 mesh, 900 mesh, 1000 mesh, 1100 mesh or 1200 mesh.

[0027] Preferably, a second pressure is applied during the second grinding process, and the second pressure is preferably 30 to 80 Pa, for example, 30 Pa, 50 Pa, 60 Pa, 70 Pa or 80 Pa.

[0028] Preferably, the second grinding time is 10 to 15 minutes, for example, 10 minutes, 11 minutes, 12 minutes, 13 minutes, 14 minutes or 15 minutes.

[0029] Preferably, the polishing medium used in the mechanical polishing has a particle size of 0.5 to 1 μm, such as 0.5 μm, 0.6 μm, 0.7 μm, 0.8 μm, 0.9 μm or 1 μm.

[0030] Preferably, the mechanical polishing speed is 80-120 r / min, for example, it can be 80 r / min, 90 r / min, 100 r / min, 110 r / min or 120 r / min.

[0031] Preferably, the mechanical polishing time is 15 to 20 minutes, for example, 15 minutes, 16 minutes, 17 minutes, 18 minutes, 19 minutes, or 20 minutes.

[0032] Preferably, the polishing media used in the chemical polishing include hydrofluoric acid, nitric acid, and water.

[0033] Preferably, the volume ratio of the hydrofluoric acid, the nitric acid, and the water is 1:(2-5):(8-12), for example, it can be 1:2:8, 1:3:9, 1:3:10, 1:4:10, 1:4:12, 1:5:8, 1:5:10, or 1:5:12, etc.

[0034] The present invention further preferably uses a volume ratio of hydrofluoric acid, nitric acid and water of 1:(2-5):(8-12) to ensure that the micro-scratches and deformation layers generated during mechanical polishing are fully removed and the surface smoothness of the sample is improved. If the proportion of water is too small, the polishing liquid will cause a certain degree of corrosion to the CoZrTaB target, and the surface roughness of the sample will increase. If the proportion of water is too large, the micro-scratches and deformation layers generated during mechanical polishing cannot be fully removed, and the surface roughness of the sample will increase.

[0035] Preferably, the chemical polishing time is 30 to 60 seconds, for example, 30 seconds, 35 seconds, 40 seconds, 45 seconds, 50 seconds, 55 seconds, or 60 seconds.

[0036] Preferably, the sample preparation method further includes sequentially performing ultrasonic cleaning and vacuum drying on the chemically polished sample.

[0037] Preferably, the vacuum degree of the vacuum drying is 10 to 100 Pa, for example, it can be 10 Pa, 30 Pa, 50 Pa, 70 Pa or 100 Pa.

[0038] Preferably, the vacuum drying temperature is 50-60°C, for example, 50°C, 52°C, 55°C, 58°C or 60°C.

[0039] Preferably, the vacuum drying time is 1 to 2 hours, for example, 1 hour, 1.2 hours, 1.5 hours, 1.8 hours or 2 hours.

[0040] Preferably, the surface conductive treatment includes ion sputtering the surface of the vacuum-dried sample to deposit a conductive film.

[0041] Preferably, the current of the ion sputtering is 10 to 20 mA, for example, it can be 10 mA, 12 mA, 15 mA, 18 mA or 20 mA, etc.

[0042] Preferably, the ion sputtering time is 3 to 5 minutes, for example, 3 minutes, 3.5 minutes, 4 minutes, 4.5 minutes or 5 minutes.

[0043] Preferably, the thickness of the conductive film is 10-20 nm, for example, it can be 10 nm, 12 nm, 14 nm, 16 nm, 18 nm or 20 nm.

[0044] As a further preferred technical solution of the present invention, the sample preparation method includes the following steps:

[0045] First, the CoZrTaB target is wire-cut using deionized water as the cooling medium at a cutting speed of 10–20 mm / min. Then, it is first-grinded for 5–10 minutes on a grinding disc with a first pressure of 50–150 Pa and 200–400 grit sandpaper. Next, the grinding disc speed is adjusted to 100–150 r / min, a second pressure of 30–80 Pa is applied, and a second grinding is performed for 10–15 minutes using 800–1200 grit sandpaper. Finally, the grinding is performed at a speed of 80–120 r / min… Mechanical polishing was performed for 15–20 min using a polishing medium with a particle size of 0.5–1 μm under the specified conditions. Then, chemical polishing was performed for 30–60 s using a polishing medium composed of hydrofluoric acid, nitric acid, and water in a volume ratio of 1:(2–5):(8–12). After ultrasonic cleaning, the sample was vacuum dried at a vacuum degree of 10–100 Pa and a temperature of 50–60 °C for 1–2 h. Finally, surface conductivity treatment was performed, i.e., ion sputtering was performed on the surface of the vacuum-dried sample for 3–5 min using a current of 10–20 mA to deposit a conductive film with a thickness of 10–20 nm. The final sample to be tested was obtained.

[0046] The CoZrTaB target material has a mass ratio of Co, Zr, Ta and B of (60-70):(10-15):(15-20):(1-5), and the purity of the CoZrTaB target material is ≥4N and the density is ≥98%.

[0047] Compared with the prior art, the present invention has at least the following beneficial effects:

[0048] The sample preparation method for SEM detection of CoZrTaB target material provided by this invention is specifically designed for CoZrTaB target material, especially high-purity CoZrTaB target material (purity ≥ 4N). The method involves sequential wire cutting, first grinding, second grinding, mechanical polishing, chemical polishing, and surface conductive treatment. Furthermore, the cooling medium and cutting speed for wire cutting, the methods of the first and second grinding, and the component ratio of the polishing medium for chemical polishing are optimized to ensure that the surface roughness of the prepared sample is preferably as low as below 5.0 nm, with no impurities introduced and no edge chipping or deformation. This improves the sample preparation effect and meets the analytical requirements for high-precision microstructure of high-purity CoZrTaB target material. Attached Figure Description

[0049] Figure 1 This is a process flow diagram of the sample preparation method for SEM detection of CoZrTaB target material provided in Embodiment 1 of the present invention. Detailed Implementation

[0050] The technical solution of the present invention will be further described below with reference to the accompanying drawings and specific embodiments. However, the following examples are merely simplified examples of the present invention and do not represent or limit the scope of protection of the present invention. The scope of protection of the present invention is determined by the claims.

[0051] I. Implementation Examples

[0052] Example 1

[0053] This embodiment provides a sample preparation method for SEM detection of CoZrTaB target material, such as... Figure 1 As shown, the sample preparation method includes the following steps:

[0054] First, the CoZrTaB target was wire-cut at a cutting speed of 15 mm / min using deionized water as the cooling medium. Then, it was ground for 8 minutes on a grinding disc with a first pressure of 100 Pa and a grinding speed of 200 r / min using 300-mesh silicon carbide abrasive paper. The grinding disc speed was then adjusted to 120 r / min, a second pressure of 50 Pa was applied, and a second grinding was performed for 12 minutes using 1000-mesh silicon carbide abrasive paper. Finally, it was mechanically polished for 18 minutes at a grinding speed of 100 r / min using a polishing cloth and 0.8 μm diamond polishing paste. The sample was then chemically polished for 45 seconds using a polishing solution composed of hydrofluoric acid (40wt%), nitric acid (65wt%), and water in a volume ratio of 1:3:10. Following this, it was ultrasonically cleaned alternately with deionized water and anhydrous ethanol for 8 minutes each time, until all residual polishing paste and polishing solution were completely removed from the sample surface. The sample was then vacuum-dried at 50 Pa and 55°C for 1.5 hours. Finally, a surface conductivity treatment was performed, i.e., ion sputtering of the vacuum-dried sample surface with a current of 15 mA for 4 minutes to deposit a conductive film with a thickness of 15 nm, thus obtaining the sample to be tested.

[0055] The CoZrTaB target material has a mass ratio of Co, Zr, Ta and B of 65:12:18:5, a purity of 4N and a density of 99%.

[0056] Example 2

[0057] This embodiment provides a sample preparation method for SEM detection of CoZrTaB target material, the sample preparation method including the following steps:

[0058] First, the CoZrTaB target was wire-cut at a cutting speed of 10 mm / min using deionized water as the cooling medium. Then, it was ground for 10 minutes on a grinding disc with a first pressure of 50 Pa and 200-mesh silicon carbide abrasive paper. The grinding disc speed was then adjusted to 100 r / min, a second pressure of 30 Pa was applied, and a second grinding was performed for 15 minutes using 800-mesh silicon carbide abrasive paper. Finally, it was mechanically polished for 20 minutes at a speed of 80 r / min using a polishing cloth and 0.5 μm diamond polishing paste. The sample was then chemically polished for 60 seconds using a polishing solution composed of hydrofluoric acid (40wt%), nitric acid (65wt%), and water in a volume ratio of 1:2:8. Following this, it was ultrasonically cleaned alternately with deionized water and anhydrous ethanol for 5 minutes each time, until all residual polishing paste and polishing solution were completely removed from the sample surface. The sample was then vacuum-dried at 10 Pa and 50 °C for 2 hours. Finally, a surface conductivity treatment was performed, i.e., ion sputtering of the vacuum-dried sample surface with a current of 10 mA for 3 minutes to deposit a conductive film with a thickness of 10 nm, thus obtaining the sample to be tested.

[0059] The CoZrTaB target material has a mass ratio of Co, Zr, Ta and B of 65:15:20:5, a purity of 4N and a density of 98%.

[0060] Example 3

[0061] This embodiment provides a sample preparation method for SEM detection of CoZrTaB target material, the sample preparation method including the following steps:

[0062] First, the CoZrTaB target was wire-cut at a cutting speed of 20 mm / min using deionized water as the cooling medium. Then, it was first ground for 5 minutes on a grinding disc with a first pressure of 150 Pa and a grinding speed of 250 r / min using 400-mesh silicon carbide abrasive paper. The grinding disc speed was then adjusted to 150 r / min, a second pressure of 80 Pa was applied, and a second grinding was performed for 10 minutes using 1200-mesh silicon carbide abrasive paper. Finally, it was mechanically polished for 20 minutes at a grinding speed of 120 r / min using a polishing cloth and 1 μm diamond polishing paste. Then, a polishing solution composed of hydrofluoric acid (40wt%), nitric acid (65wt%) and water in a volume ratio of 1:5:12 is used for chemical polishing for 30s. Then, ultrasonic cleaning is performed alternately with deionized water and anhydrous ethanol for 10min each time until the polishing paste and polishing solution remaining on the sample surface are completely removed. The sample is then vacuum dried at a vacuum degree of 100Pa and a temperature of 60℃ for 1h. Finally, surface conductivity treatment is performed, that is, the vacuum-dried sample surface is ion sputtered with a current of 20mA for 5min to deposit a conductive film with a thickness of 20nm, and the final sample to be tested is obtained.

[0063] The CoZrTaB target material has a mass ratio of Co, Zr, Ta, and B of 70:10:18:2, a purity of 4.5N, and a density of 99.5%.

[0064] Example 4

[0065] This embodiment provides a sample preparation method for SEM detection of CoZrTaB target material. Except for the wire cutting speed of 8 mm / min, the sample preparation method is the same as that in Embodiment 1.

[0066] Example 5

[0067] This embodiment provides a sample preparation method for SEM detection of CoZrTaB target material. Except for the wire cutting speed of 22 mm / min, the sample preparation method is the same as that in Embodiment 1.

[0068] Example 6

[0069] This embodiment provides a sample preparation method for SEM detection of CoZrTaB target material. Except for the fact that the cutting fluid used in the wire cutting is a common industrial chemical cutting fluid (Beijing Zhubao New Technology Co., Ltd., model DZ-1130), the sample preparation method is the same as in Embodiment 1.

[0070] Example 7

[0071] This embodiment provides a sample preparation method for SEM detection of CoZrTaB target material. The sample preparation method is the same as in Example 1, except that the volume ratio of hydrofluoric acid, nitric acid and water in the polishing solution of the chemical polishing is 1:3:6.

[0072] Example 8

[0073] This embodiment provides a sample preparation method for SEM detection of CoZrTaB target material. The sample preparation method is the same as in Example 1, except that the volume ratio of hydrofluoric acid, nitric acid and water in the polishing solution of the chemical polishing is 1:3:12.

[0074] Example 9

[0075] This embodiment provides a sample preparation method for SEM detection of CoZrTaB target material. The sample preparation method is the same as in Embodiment 1, except that the first and second grinding are not performed on a grinding disc, but are performed by hand grinding with 300-mesh silicon carbide sandpaper for 8 minutes and then by hand grinding with 1000-mesh silicon carbide sandpaper for 12 minutes.

[0076] II. Comparative Example

[0077] Comparative Example 1

[0078] This comparative example provides a sample preparation method for SEM detection of CoZrTaB target material. The sample preparation method is the same as in Example 1, except that the wire cutting is replaced with mechanical cutting.

[0079] Comparative Example 2

[0080] This comparative example provides a sample preparation method for SEM detection of CoZrTaB target material. The sample preparation method is the same as that in Example 1 except that the chemical polishing is not performed.

[0081] Comparative Example 3

[0082] This comparative example provides a sample preparation method for SEM detection of CoZrTaB target material. The sample preparation method omits the first grinding, second grinding, and chemical polishing, and the mechanical polishing adopts the polishing steps described in step (1) of Example 1 in CN112067643A, that is, the sample is sequentially polished in the first, second, and third stages until there are no scratches on the surface; wherein, the first polishing refers to polishing with 240# sandpaper for 2 minutes; the second polishing refers to polishing with 1000# sandpaper for 4 minutes; and the third polishing refers to polishing with 2000# sandpaper for 3 minutes, the rest are the same as in Example 1.

[0083] III. Tests and Results

[0084] The surface roughness of the samples prepared by the CoZrTaB target material SEM detection method provided in the above embodiments or comparative examples was tested, and the edge cracking or deformation was observed. The results are shown in Table 1.

[0085] Table 1

[0086] project Surface roughness Ra / nm Edge chipping or deformation Example 1 3.2 No cracks, no deformation Example 2 4.5 No cracks, no deformation Example 3 4.8 No cracks, no deformation Example 4 6.1 There are cracks and deformations. Example 5 5.8 There are cracks and deformations. Example 6 7.5 No cracks, no deformation Example 7 8.3 No cracks, no deformation Example 8 6.5 No cracks, no deformation Example 9 9.2 No cracks, but some deformation Comparative Example 1 10.5 There are cracks and deformations. Comparative Example 2 12.8 No cracks, no deformation Comparative Example 3 15.6 No cracks, no deformation

[0087] The data in Table 1 shows that:

[0088] (1) As can be seen from the comprehensive examples 1 to 3, the sample preparation method for SEM detection of CoZrTaB target material provided by the present invention has the synergistic effect of each process, so that the surface of the sample to be tested is high, the surface roughness is low (below 5.0 nm), and there is no chipping or deformation at the edge, which can meet the requirements of fine analysis of the microstructure of CoZrTaB target material.

[0089] (2) It can be seen from the combined examples 1 and 4 to 6 that: the wire cutting speed in example 4 is relatively slow and takes a long time; the wire cutting speed in example 5 is relatively fast, which leads to chipping and deformation of the sample edges; the use of the chemical cutting fluid in example 6 leads to an increase in the surface roughness of the sample. This indicates that the present invention further preferably uses deionized water as the cooling medium for wire cutting and the cutting speed of the wire cutting is 10 to 20 mm / min, which further improves the sample preparation effect of CoZrTaB target material.

[0090] (3) It can be seen from the comprehensive examples 1 and 7 to 9 that: in the chemical polishing of example 7, the volume ratio of water in the polishing solution was too small, which led to an increase in the surface roughness of the sample; in the chemical polishing of example 8, the volume ratio of water in the polishing solution was too large, which also led to an increase in the surface roughness of the sample; in example 9, grinding was not performed on a grinding disc, so the grinding pressure and grinding could not be reasonably controlled, resulting in uneven grinding, damage to the sample surface, and reduction of surface smoothness; thus, it is indicated that the present invention further preferably uses a volume ratio of hydrofluoric acid, nitric acid and water of 1:(2~5):(8~12); further preferably, the first grinding and the second grinding are performed on a grinding disc to achieve reasonable control of grinding pressure and grinding direction, further reducing the surface roughness of the obtained sample and improving the sample preparation effect.

[0091] (4) It can be seen from the comprehensive comparison of Example 1 and Comparative Examples 1 to 3 that: due to the mechanical cutting method used in Comparative Example 1, the edges are prone to cracking and deformation; due to the mechanical polishing only performed without chemical polishing in Comparative Example 2, the surface roughness of the sample increased to 12.8 nm; due to the manual polishing with sandpaper in Comparative Example 3 without grinding, the polishing was insufficient, and the surface roughness of the sample increased to 15.6 nm, resulting in poor sample preparation effect. This shows that the sample preparation method provided by the present invention for a specific CoZrTaB target material, which sequentially performs wire cutting, first grinding, second grinding, mechanical polishing, chemical polishing and surface conductive treatment, has the synergistic effect of each process, so that the prepared sample can meet the requirements of fine analysis of the microstructure of CoZrTaB target material.

[0092] The applicant declares that the above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.

Claims

1. A sample preparation method for CoZrTaB target material SEM detection, characterized in that, The sample preparation method comprises the following steps: The CoZrTaB target material is sequentially subjected to wire cutting, first grinding, second grinding, mechanical polishing, chemical polishing and surface conductive treatment to obtain a sample to be detected.

2. The sample preparation method of claim 1, wherein The purity of the CoZrTaB target material is greater than or equal to 4N; Preferably, the compactness of the CoZrTaB target material is greater than or equal to 98%. Preferably, the mass ratio of Co, Zr, Ta and B in the CoZrTaB target material is (60-70):(10-15):(15-20):(1-5).

3. The sample preparation method according to claim 1 or 2, characterized by, The cooling medium used in the wire cutting comprises deionized water. Preferably, the cutting speed of the wire cutting is 10-20 mm / min.

4. The sample preparation method according to any one of claims 1 to 3, characterized by, The first grinding and the second grinding are performed on a grinding disc. Preferably, the rotating speed of the grinding disc during the first grinding is 150-250 r / min. Preferably, the granularity of the sandpaper used in the first grinding is 200-400 mesh. Preferably, a first pressure is applied during the first grinding, and preferably the first pressure is 50-150 Pa. Preferably, the time for the first grinding is 5-10 min.

5. The sample preparation method of claim 4, wherein The rotating speed of the grinding disc during the second grinding is 100-150 r / min. Preferably, the granularity of the sandpaper used in the second grinding is 800-1200 mesh. Preferably, a second pressure is applied during the second grinding, and preferably the second pressure is 30-80 Pa. Preferably, the time for the second grinding is 10-15 min.

6. The sample preparation method according to any one of claims 1 to 5, characterized by, The granularity of the polishing medium used in the mechanical polishing is 0.5-1 μm. Preferably, the rotating speed of the mechanical polishing is 80-120 r / min. Preferably, the time for the mechanical polishing is 15-20 min.

7. The sample preparation method according to any one of claims 1 to 6, characterized by, The polishing medium used in the chemical polishing comprises hydrofluoric acid, nitric acid and water. Preferably, the volume ratio of the hydrofluoric acid, the nitric acid and the water is 1:(2-5):(8-12). Preferably, the time for the chemical polishing is 30-60 s.

8. The sample preparation method according to any one of claims 1 to 7, characterized by, The sample preparation method further comprises sequentially performing ultrasonic cleaning and vacuum drying on the sample after the chemical polishing. Preferably, the vacuum degree of the vacuum drying is 10-100 Pa. Preferably, the temperature of the vacuum drying is 50-60 °C. Preferably, the time for the vacuum drying is 1-2 h.

9. The method of claim 8, wherein, The surface conductive treatment comprises performing ion sputtering on the surface of the sample after the vacuum drying to plate a conductive film. Preferably, the current of the ion sputtering is 10-20 mA. Preferably, the time for the ion sputtering is 3-5 min. Preferably, the thickness of the conductive film is 10-20 nm.

10. The sample preparation method according to any one of claims 1 to 9, characterized by, The sample preparation method comprises the following steps: The CoZrTaB target material is first linearly cut at a cutting speed of 10-20 mm / min with deionized water as a cooling medium, then is first ground on a grinding disc with a rotation speed of 150-250 r / min and a first pressure of 50-150 Pa applied thereon for 5-10 min using sandpaper with a granularity of 200-400 mesh, then the rotation speed of the grinding disc is adjusted to 100-150 r / min, a second pressure of 30-80 Pa is applied thereon, and second grinding is performed for 10-15 min using sandpaper with a granularity of 800-1200 mesh, then mechanical polishing is performed for 15-20 min using a polishing medium with a granularity of 0.5-1 μm at a rotation speed of 80-120 r / min, then chemical polishing is performed for 30-60 s using a polishing medium composed of hydrofluoric acid, nitric acid and water in a volume ratio of 1:(2-5):(8-12), then ultrasonic cleaning is performed and vacuum drying is performed at a vacuum degree of 10-100 Pa and a temperature of 50-60 ℃ for 1-2 h, finally, surface conductive treatment is performed, that is, ion sputtering is performed for 3-5 min on the surface of the vacuum dried sample using a current of 10-20 mA to plate a conductive film with a thickness of 10-20 nm, and finally a sample to be detected is obtained. In the CoZrTaB target material, the mass ratio of Co, Zr, Ta and B is (60-70):(10-15):(15-20):(1-5), the purity of the CoZrTaB target material is ≥4N, and the density is ≥98%.

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