Sample preparation method for EBSD detection of MoSi target material

Abstract

The invention relates to a sample preparation method for EBSD detection of a MoSi target material, and the sample preparation method comprises the following steps: carrying out cutting, grinding treatment, mechanical polishing and chemical mechanical polishing on the MoSi target material in sequence to obtain a to-be-detected sample; a polishing solution adopted in the chemical mechanical polishing treatment comprises a basic solution, an acid solution and colloidal silicon dioxide, the polishing solution comprises 0.5-1 part by weight of the acid solution based on 100 parts by weight of the basic solution, and the concentration of the acid solution is 5-10 wt%; the MoSi target material sample prepared through the sample preparation method is smooth in surface, the roughness is as low as nanoscale, no obvious scratches exist, when the MoSi target material sample is used for EBSD detection, a diffraction Kikuchi zone is clear, the sample calibration rate reaches up to 90% or above, and a reliable detection sample is provided for research of microstructure characteristics of the MoSi material.

Description

Technical Field

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

[0002] MoSi sputtering targets are a core raw material for thin film deposition, and their microstructure and crystallographic characteristics directly determine the growth mode, structural stability, and final performance of sputtered films. For example, parameters such as crystal orientation distribution, texture type, and grain boundary characteristics of MoSi sputtering targets significantly affect the density, adhesion, and electrical properties of the film, while phase composition and phase transition behavior relate to the compositional uniformity and long-term reliability of the film. Therefore, in-depth research into the microstructural characteristics of MoSi sputtering targets is of great significance for optimizing the sputtering target preparation process and improving the quality of thin film products.

[0003] Electron backscatter diffraction (EBSD) is an in-situ, rapid method for microstructure analysis. It can simultaneously acquire key information such as crystal orientation, orientation difference, orientation distribution function, grain boundary type, interfacial crystal plane index, and phase identification, and has been widely used in the microstructure characterization of materials such as metals, alloys, and ceramics. However, EBSD research on MoSi targets is relatively scarce. This is because there is a contradiction between the inherent properties of MoSi and the technical requirements of EBSD detection. For example, EBSD technology has strict requirements for sample quality, requiring nanoscale surface flatness, absence of oxidation contamination, absence of mechanical damage layers, and good conductivity. MoSi, on the other hand, has high hardness, high brittleness, and is easily oxidized, making conventional sample preparation methods unsuitable for it.

[0004] The high hardness and brittleness of MoSi targets make machining difficult, resulting in low efficiency in mechanical grinding and polishing. This leads to edge chipping, grain shedding, and surface microcracks, which damage the integrity of the sample surface and fail to meet the surface quality requirements for EBSD testing. The easy oxidation of MoSi materials causes them to form a dense oxide layer (mainly SiO2 and Mo oxides) in the air (especially the heat generated during polishing accelerates surface oxidation), which severely hinders electron backscattering. In addition, MoSi targets often contain multiple phases such as MoSi2, Mo5Si3, and Mo3Si. The hardness and chemical stability of different phases vary significantly, and selective corrosion is prone to occur during chemical polishing or electrolytic polishing, resulting in undulations on the sample surface and making it difficult to obtain a uniform and flat detection surface.

[0005] Therefore, providing a sample preparation method suitable for EBSD detection of MoSi target materials to fill the gap in EBSD research on MoSi materials is of great research significance for revealing relevant information such as crystal orientation, interfacial crystal plane index, and phase composition. Summary of the Invention

[0006] To address the aforementioned technical problems, this invention provides a sample preparation method for EBSD detection of MoSi target materials. The resulting MoSi target material sample has an efficient removal of the oxide layer on its surface, resulting in a smooth and flat surface with a surface roughness as low as the nanometer level and no obvious scratches. When used for EBSD detection, the diffraction Kikuchi band is clear, and the sample calibration rate is high. This method is beneficial for studying the microstructure and crystal characteristics of MoSi materials and is of great significance for optimizing the target material preparation process and improving the quality of thin film products.

[0007] To achieve this objective, the present invention adopts the following technical solution: This invention provides a sample preparation method for EBSD detection of MoSi target material, the sample preparation method comprising the following steps: The MoSi target material is sequentially cut, ground, mechanically polished, and chemically mechanically polished to obtain the sample to be tested. The polishing slurry used in the chemical mechanical polishing treatment includes a base liquid, an acid solution, and colloidal silica. Based on 100 parts by weight of the base liquid, the polishing slurry includes 0.5 to 1 part of acid solution (e.g., 0.5, 0.6, 0.7, 0.8, 0.9, or 1 part, etc.), and the concentration of the acid solution is 5 to 10 wt%, for example, 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt%, or 10 wt%, etc.

[0008] This invention employs a polishing method that combines mechanical polishing with chemical mechanical polishing, and selects polishing solutions with specific acid concentrations. The chemical mechanical polishing, through the synergistic effect of mechanical grinding and chemical etching, efficiently removes the 10-50 nm stress layer remaining from the mechanical polishing process, while reducing surface roughness to the nanometer level. This results in clear diffraction Kikuchi bands, high sample calibration rate, and high detection accuracy when used for EBSD detection.

[0009] Preferably, the size of the cut MoSi target sample is 10mm×10mm×(2~5)mm, for example, it can be 10mm×10mm×2mm, 10mm×10mm×3mm, 10mm×10mm×4mm or 10mm×10mm×5mm, etc.

[0010] Preferably, the sample preparation method further includes cleaning after cutting and before the grinding process.

[0011] The sample preparation method of the present invention involves cleaning before the grinding process after cutting, in order to remove residual oil and metal debris from the cutting process.

[0012] Preferably, the cleaning process includes ultrasonic cleaning with an organic solvent followed by ultrasonic cleaning with water.

[0013] Preferably, the cleaning is performed 2 or 3 times.

[0014] Preferably, the cleaning time is 10-15 minutes, for example, 10 minutes, 11 minutes, 12 minutes, 13 minutes, 14 minutes or 15 minutes.

[0015] Preferably, the organic solvent includes ethanol and / or acetone.

[0016] Preferably, the power of the ultrasonic cleaning is 300~500W, for example, it can be 300W, 350W, 400W, 450W or 500W.

[0017] Preferably, the frequency of the ultrasonic cleaning is 28~60kHz, for example, it can be 28kHz, 40kHz, 45kHz, 50kHz, 55kHz or 60kHz.

[0018] Preferably, the polishing solution comprises 100 parts by weight of base liquid, 0.5 to 1 part by weight of acid liquid and 10 to 15 parts by weight of colloidal silica.

[0019] The components include 0.5 to 1 part acid solution, such as 0.5, 0.6, 0.7, 0.8, 0.9 or 1 part; and 10 to 15 parts colloidal silica, such as 10, 11, 12, 13, 14 or 15 parts.

[0020] Preferably, the base fluid includes a solvent and a lubricant.

[0021] Preferably, the volume ratio of solvent to lubricant in the base fluid is (2~4):1, for example, it can be 2:1, 2.5:1, 3:1, 3.5:1 or 4:1, etc.

[0022] Preferably, the lubricant comprises ethylene glycol and / or polyethylene glycol.

[0023] It is worth noting that the lubricant in the base liquid of the present invention can inhibit sample oxidation and improve the lubricity of the polishing liquid, thereby improving the polishing effect.

[0024] Preferably, the acid solution includes a nitric acid solution and / or a phosphoric acid solution. Preferably, the colloidal silica has a particle size of 50-100 nm, for example, 50 nm, 60 nm, 70 nm, 80 nm, 90 nm, or 100 nm.

[0025] Preferably, the hardness of the colloidal silica is less than the hardness of the MoSi target material.

[0026] Preferably, the rotational speed of the polishing disc during chemical mechanical polishing 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, etc.

[0027] Preferably, the pressure on the MoSi target sample during the chemical mechanical polishing process is 1~2N, for example, it can be 1N, 1.2N, 1.4N, 1.6N, 1.8N or 2N.

[0028] Preferably, the chemical mechanical polishing time is 20-30 minutes, for example, 20 minutes, 22 minutes, 25 minutes, 28 minutes or 30 minutes.

[0029] Preferably, the polishing liquid is continuously added during the chemical mechanical polishing process, and the dropping rate is 5~10 mL / min, for example, it can be 5 mL / min, 6 mL / min, 7 mL / min, 8 mL / min, 9 mL / min or 10 mL / min, etc.

[0030] Preferably, the sample preparation method further includes washing with water and then with ethanol after chemical mechanical polishing, followed by drying with nitrogen.

[0031] Preferably, the polishing process includes a first polishing process and a second polishing process performed sequentially.

[0032] Preferably, the surface roughness of the MoSi target sample after the first polishing treatment is ≤1μm, for example, it can be 1μm, 0.9μm, 0.8μm, 0.7μm, 0.6μm, 0.5μm, 0.4μm, 0.3μm or 0.2μm, etc.

[0033] Preferably, the surface roughness of the MoSi target sample after the second polishing treatment is ≤0.1μm, for example, it can be 0.1μm, 0.09μm, 0.08μm, 0.07μm, 0.06μm, 0.05μm or 0.04μm, etc.

[0034] It is worth noting that the sample preparation method described in this invention does not impose any special restrictions on the total time of the first and second grinding processes, as long as the required surface roughness is met.

[0035] Preferably, the first polishing includes polishing with 400-grit, 800-grit, and 1200-grit sandpaper in sequence.

[0036] Preferably, the grinding machine pressure during the first grinding process is 5~10N, for example, it can be 5N, 6N, 7N, 8N, 9N or 10N.

[0037] Preferably, the rotation speed of the grinding machine during the first grinding process is 50~100 r / min, for example, it can be 50 r / min, 60 r / min, 70 r / min, 80 r / min, 90 r / min or 100 r / min, etc.

[0038] Preferably, the sanding time for each level of sandpaper during the first sanding process is 5 to 8 minutes, for example, 5 minutes, 6 minutes, 7 minutes or 8 minutes.

[0039] Preferably, the second polishing process includes polishing with 2000-grit and 5000-grit sandpaper in sequence.

[0040] Preferably, the grinding machine pressure during the second grinding process is 3~5N, for example, it can be 3N, 3.5N, 4N, 4.5N or 5N.

[0041] Preferably, the rotation speed of the grinding machine during the second grinding process is 50~100 r / min, for example, it can be 50 r / min, 60 r / min, 70 r / min, 80 r / min, 90 r / min or 100 r / min, etc.

[0042] Preferably, the second polishing process uses 5000-grit sandpaper for polishing time of ≥10 minutes, for example, 10 minutes, 12 minutes, 15 minutes, 18 minutes or 20 minutes.

[0043] Preferably, the mechanical polishing is performed using a wool polishing disc and / or a polyurethane polishing disc.

[0044] Preferably, the polishing disc rotates at a speed of 100-150 r / min during the mechanical polishing process, for example, 100 r / min, 110 r / min, 120 r / min, 130 r / min, 140 r / min or 150 r / min, etc.

[0045] Preferably, the pressure on the MoSi target sample during the mechanical polishing process is 2~3N, for example, it can be 2N, 2.2N, 2.5N, 2.8N or 3N.

[0046] Preferably, the polishing fluid used for mechanical polishing includes 1μm diamond polishing fluid and / or 0.5μm diamond polishing fluid.

[0047] Preferably, the concentration of the polishing slurry for mechanical polishing is 5-10 wt%, for example, it can be 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt%, or 10 wt%.

[0048] Preferably, the sample preparation method further includes cleaning after the chemical mechanical polishing.

[0049] Preferably, the cleaning includes plasma cleaning.

[0050] Preferably, the power of the plasma cleaning is 100~200W, for example, it can be 100W, 120W, 150W, 180W or 200W.

[0051] Preferably, the plasma cleaning time is 30-60 seconds, for example, 30 seconds, 40 seconds, 50 seconds or 60 seconds.

[0052] Preferably, the cleaning process further includes wiping the surface of the MoSi target with isopropanol.

[0053] The purpose of cleaning after chemical mechanical polishing is to remove organic contaminants from the clothing on the sample surface. A lint-free cloth is used during wiping to avoid fiber residue.

[0054] Preferably, the sample preparation method further includes an anti-oxidation treatment after the cleaning.

[0055] If the sample needs to be stored for ≤24 hours, it should be treated with anti-oxidation measures. If it is to be used directly for EBSD testing, this step can be omitted and the test can be performed directly.

[0056] Preferably, the anti-oxidation treatment includes immersion in ethanol or placement in a vacuum dryer with a vacuum degree ≤1 Pa, such as 1 Pa, 0.8 Pa, 0.6 Pa, 0.4 Pa, or 0.2 Pa.

[0057] Compared with the prior art, the present invention has at least the following beneficial effects: The sample preparation method for EBSD detection of MoSi target material provided by this invention adopts a polishing method combining mechanical polishing and chemical mechanical polishing, and further selects a chemical mechanical polishing solution with specific components to efficiently remove the oxide layer on the surface of MoSi target material sample, making its surface smooth and flat without obvious scratches. It has high resolution and stability when performing EBSD detection, the sample diffraction kimonozone is clear, and the sample calibration rate is as high as 90% or more, which improves the test results and provides reliable detection data for the study of the microstructure characteristics of MoSi material. Detailed Implementation

[0058] The technical solution of the present invention will be further illustrated below through 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.

[0059] In the following embodiments or comparative examples, during the first polishing process, each level of silicon carbide sandpaper needs to polish until the scratches of the previous level completely disappear. Furthermore, each time a level of sandpaper is changed, the MoSi target sample is rotated 90° to facilitate observation of the scratch removal. In the following examples or comparative examples, nitrogen drying was performed using a nitrogen gun, and the nitrogen purity was ≥99.99%.

[0060] All organic reagents used in the following examples or comparative examples are of analytical grade and can be purchased commercially available. The water used is deionized water for laboratory use.

[0061] I. Implementation Examples Example 1 This embodiment provides a sample preparation method for EBSD detection of MoSi target material, the sample preparation method including the following steps: First, the MoSi target material is cut to a size of 10mm×10mm×4mm. Then, it is ultrasonically cleaned twice with alternating anhydrous ethanol and acetone, each time for 10 minutes. Then, it is ultrasonically cleaned with deionized water for 5 minutes. The ultrasonic power of each ultrasonic cleaning is 400W and the frequency is 40kHz. After that, it is quickly dried with a nitrogen gun (purity ≥99.99%). The MoSi target sample was then subjected to a first polishing treatment to a surface roughness of 0.8 μm, including polishing with 400-grit, 800-grit, and 1200-grit silicon carbide sandpaper in sequence, with a polishing machine pressure of 8 N and a rotation speed of 70 r / min. After polishing, the sample was rinsed with anhydrous ethanol to remove polishing debris. The MoSi target sample was then subjected to a second polishing treatment to a surface roughness of 0.08 μm, including polishing with 2000-grit and 5000-grit silicon carbide sandpaper in sequence, with a polishing machine pressure of 4 N and a rotation speed of 80 r / min. The polishing time with 5000-grit silicon carbide sandpaper was 15 min to ensure no obvious scratches. The sample was then ultrasonically cleaned with anhydrous ethanol for 5 min and dried with nitrogen. Subsequently, mechanical polishing was performed using a wool polishing pad until the surface was free of scratches and had a mirror-like finish. The mechanical polishing included polishing at 120 r / min with 1 μm diamond polishing fluid (8 wt%) for 15 min, followed by polishing with 0.5 μm diamond polishing fluid (5 wt%) for 20 min, with anhydrous ethanol continuously added during the process. The MoSi target sample was then subjected to chemical mechanical polishing. The polishing solution used for chemical mechanical polishing consisted of 100 parts by weight of base solution (water and ethylene glycol in a volume ratio of 3:1), 0.8 parts by weight of nitric acid solution (8 wt%), and 12 parts by weight of colloidal silica (particle size of 50-100 nm). The polishing solution was continuously added dropwise at a flow rate of 8 mL / min. The polishing disc rotation speed was 100 r / min, the sample pressure was 1.5 N, and the time was 25 min. Subsequently, the sample was ultrasonically cleaned with deionized water for 10 min, then ultrasonically cleaned with anhydrous ethanol for 5 min, and finally dried with nitrogen. Finally, the MoSi target material is subjected to plasma cleaning (oxygen plasma, power 150W, time 40s) to obtain the sample to be tested and then immersed in anhydrous ethanol.

[0062] Example 2 This embodiment provides a sample preparation method for EBSD detection of MoSi target material, the sample preparation method including the following steps: First, the MoSi target material is cut to a size of 10mm×10mm×5mm. Then, it is ultrasonically cleaned three times with alternating anhydrous ethanol and acetone, each time for 15 minutes. Then, it is ultrasonically cleaned with deionized water for 8 minutes. The ultrasonic power of each ultrasonic cleaning is 300W and the frequency is 40kHz. After that, it is quickly dried with nitrogen. The MoSi target sample was then subjected to a first polishing treatment to a surface roughness of 0.9 μm, including polishing with 400-grit, 800-grit, and 1200-grit silicon carbide sandpaper in sequence, with a polishing machine pressure of 5 N and a rotation speed of 100 r / min. After polishing, the sample was rinsed with anhydrous ethanol to remove polishing debris. The MoSi target sample was then subjected to a second polishing treatment to a surface roughness of 0.07 μm, including polishing with 2000-grit and 5000-grit silicon carbide sandpaper in sequence, with a polishing machine pressure of 3 N and a rotation speed of 50 r / min. The polishing time with 5000-grit silicon carbide sandpaper was 10 min to ensure no obvious scratches. The sample was then ultrasonically cleaned with anhydrous ethanol for 5 min and dried with nitrogen. Subsequently, mechanical polishing was performed using a polyurethane polishing pad until the surface was free of scratches and had a mirror-like finish. The mechanical polishing included polishing at 100 r / min with 1 μm diamond polishing slurry (5 wt%) for 18 min, followed by polishing with 0.5 μm diamond polishing slurry (8 wt%) for 20 min, with anhydrous ethanol continuously added during the process. The MoSi target sample was then subjected to chemical mechanical polishing. The polishing solution used for chemical mechanical polishing consisted of 100 parts by weight of base solution (water and ethylene glycol in a volume ratio of 2:1), 0.5 parts by weight of nitric acid solution (5 wt%), and 10 parts by weight of colloidal silica (particle size of 50-100 nm). The polishing solution was continuously added dropwise at a flow rate of 5 mL / min. The polishing disc rotation speed was 80 r / min, the sample pressure was 1 N, and the time was 20 min. Subsequently, the sample was ultrasonically cleaned with deionized water for 10 min, then ultrasonically cleaned with anhydrous ethanol for 5 min, and finally dried with nitrogen. Finally, the surface of the MoSi target material is quickly wiped with isopropanol to obtain the sample to be tested, which is then placed in a vacuum dryer with a vacuum degree of 1 Pa.

[0063] Example 3 This embodiment provides a sample preparation method for EBSD detection of MoSi target material, the sample preparation method including the following steps: First, the MoSi target material is cut to a size of 10mm×10mm×2mm. Then, it is ultrasonically cleaned three times with alternating anhydrous ethanol and acetone, each time for 12 minutes. Then, it is ultrasonically cleaned with deionized water for 10 minutes. The ultrasonic power of each ultrasonic cleaning is 500W and the frequency is 40kHz. After that, it is quickly dried with nitrogen. The MoSi target sample was then subjected to a first polishing treatment to a surface roughness of 0.8 μm, including polishing with 400-grit, 800-grit, and 1200-grit silicon carbide sandpaper in sequence, with a polishing machine pressure of 10 N and a rotation speed of 50 r / min. After polishing, the sample was rinsed with anhydrous ethanol to remove polishing debris. The MoSi target sample was then subjected to a second polishing treatment to a surface roughness of 0.09 μm, including polishing with 2000-grit and 5000-grit silicon carbide sandpaper in sequence, with a polishing machine pressure of 5 N and a rotation speed of 100 r / min. The polishing time with 5000-grit silicon carbide sandpaper was 12 min to ensure no obvious scratches. The sample was then ultrasonically cleaned with anhydrous ethanol for 5 min and dried with nitrogen. Subsequently, mechanical polishing was performed using a polyurethane polishing pad until the surface was free of scratches and had a mirror-like finish. The mechanical polishing included polishing with 1μm diamond polishing fluid (10wt%) for 20 minutes at 50r / min, followed by polishing with 0.5μm diamond polishing fluid (10wt%) for 15 minutes, with anhydrous ethanol continuously added during the process. The MoSi target sample was then subjected to chemical mechanical polishing. The polishing solution used for chemical mechanical polishing consisted of 100 parts by weight of a base solution (water and ethylene glycol in a volume ratio of 4:1), 1 part by weight of a nitric acid solution (10 wt%), and 15 parts by weight of colloidal silica (particle size of 50-100 nm). The polishing solution was continuously added dropwise at a flow rate of 10 mL / min. The polishing disc rotation speed was 120 r / min, the sample pressure was 2 N, and the time was 30 min. Subsequently, the sample was ultrasonically cleaned with deionized water for 10 min, then ultrasonically cleaned with anhydrous ethanol for 10 min, and finally dried with nitrogen. Finally, the surface of the MoSi target material is quickly wiped with isopropanol to obtain the sample to be tested, which is then placed in a vacuum dryer with a vacuum degree of 0.8 Pa.

[0064] Example 4 This embodiment provides a sample preparation method for EBSD detection of MoSi target material. The sample preparation method is the same as that in Example 1, except that the polishing solution used in the chemical mechanical polishing contains 8 parts of colloidal silica.

[0065] Example 5 This embodiment provides a sample preparation method for EBSD detection of MoSi target material. The sample preparation method is the same as that in Example 1, except that the colloidal silica in the polishing solution used for chemical mechanical polishing is 18 parts.

[0066] Example 6 This embodiment provides a sample preparation method for EBSD detection of MoSi target material. The sample preparation method is the same as in Example 1, except that the ethylene glycol in the base solution of the polishing slurry used in the chemical mechanical polishing is replaced with an equal amount of water.

[0067] Example 7 This embodiment provides a sample preparation method for EBSD detection of MoSi target material. Except for the drop rate of the polishing liquid during the chemical mechanical polishing process being 3 mL / min, the sample preparation method is the same as in Example 1.

[0068] Example 8 This embodiment provides a sample preparation method for EBSD detection of MoSi target material. Except for the dripping acceleration rate of the polishing liquid during the chemical mechanical polishing process being 12 mL / min, the sample preparation method is the same as that in Example 1.

[0069] II. Comparative Example Comparative Example 1 This comparative example provides a sample preparation method for EBSD detection of MoSi target material. Except for the fact that the nitric acid solution (8wt%) in the polishing solution used in the chemical mechanical polishing is 0.3 parts, the sample preparation method is the same as in Example 1.

[0070] Comparative Example 2 This comparative example provides a sample preparation method for EBSD detection of MoSi target material. Except for the fact that the nitric acid solution (8wt%) in the polishing solution used in the chemical mechanical polishing is 1.2 parts, the sample preparation method is the same as in Example 1.

[0071] Comparative Example 3 This comparative example provides a sample preparation method for EBSD detection of MoSi target material. Except for the concentration of nitric acid solution in the polishing solution used for chemical mechanical polishing being 4wt%, the sample preparation method is the same as that in Example 1.

[0072] Comparative Example 4 This comparative example provides a sample preparation method for EBSD detection of MoSi target material. Except for the concentration of nitric acid solution in the polishing solution used for chemical mechanical polishing being 12wt%, the sample preparation method is the same as that in Example 1.

[0073] Comparative Example 5 This comparative example provides a sample preparation method for EBSD detection of MoSi target material. The sample preparation method is the same as in Example 1, except that the chemical mechanical polishing is replaced with chemical polishing.

[0074] III. Tests and Results The samples to be tested obtained by the sample preparation method of the MoSi target EBSD test provided in the above embodiments or comparative examples were subjected to EBSD test. The clarity of the diffraction Kikuchi band was observed and the sample calibration rate was analyzed. The results are shown in Table 1. The sample calibration rate is calculated using the following formula: Table 1 The data in Table 1 shows that: (1) As can be seen from Examples 1 to 3, the sample preparation method for EBSD detection of MoSi target material provided by the present invention produces MoSi target material samples with clear diffraction Kikuchi bands when used for EBSD detection, and the sample calibration rate is as high as 90% or more, which is of great significance for the study of EBSD of MoSi material.

[0075] (2) As can be seen from the combined examples 1 and 4 to 8, the present invention further preferably includes, by weight, 100 parts of base liquid and 10 to 15 parts of colloidal silica in the polishing liquid, preferably the base liquid includes solvent and lubricant, and further preferably the dripping acceleration rate of the polishing liquid during the chemical mechanical polishing process is 5 to 10 mL / min; that is, the composition and dripping acceleration rate of the chemical mechanical polishing are further preferred, which further improves the removal effect on the oxide layer on the surface of the MoSi target sample and the stress layer generated after mechanical polishing, further reduces its surface roughness, and further improves the clarity of the diffraction Kikuchi band and the sample calibration rate when the obtained MoSi target sample is used for EBSD detection.

[0076] (3) It can be seen from the comprehensive comparison of Example 1 and Comparative Examples 1 to 5 that, due to the small amount of nitric acid solution in the polishing solution used for chemical mechanical polishing in Comparative Example 1 and the low concentration of nitric acid solution in the polishing solution used for chemical mechanical polishing in Comparative Example 3, the oxide layer on the surface of the MoSi target material cannot be fully removed, resulting in unclear diffraction daphne bands and a decrease in the sample calibration rate; due to the large amount of nitric acid solution in the polishing solution used for chemical mechanical polishing in Comparative Example 2 and the high concentration of nitric acid solution in the polishing solution used for chemical mechanical polishing in Comparative Example 4, the surface of the MoSi target material is corroded, resulting in increased surface roughness, unclear diffraction daphne bands, and a decrease in the sample calibration rate; and due to the fact that only chemical polishing was performed in Comparative Example 5, the stress layer generated after mechanical polishing could not be fully removed, resulting in unclear diffraction daphne bands and a decrease in the sample calibration rate.

[0077] In summary, this invention employs a polishing method combining mechanical polishing and chemical mechanical polishing to efficiently remove the oxide layer from the surface of MoSi target samples while ensuring a smooth and flat surface without obvious scratches. This reduces surface roughness to the nanometer level, resulting in clear diffraction Kikuchi bands and high sample calibration rate when used for EBSD detection, thus improving detection accuracy. This invention is of great research significance for revealing information such as crystal orientation, interfacial crystal plane index, and phase composition.

[0078] 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 EBSD detection of MoSi target material, characterized in that, The sample preparation method includes the following steps: The MoSi target material is sequentially cut, ground, mechanically polished, and chemically mechanically polished to obtain the sample to be tested; The polishing slurry used in the chemical mechanical polishing treatment includes a base liquid, an acid liquid, and colloidal silica. The polishing slurry includes 0.5 to 1 part of acid liquid per 100 parts by weight of the base liquid, and the concentration of the acid liquid is 5 to 10 wt%.

2. The sample preparation method according to claim 1, characterized in that, The polishing solution comprises 100 parts base liquid, 0.5 to 1 part acid solution and 10 to 15 parts colloidal silica.

3. The sample preparation method according to claim 2, characterized in that, The base fluid includes solvents and lubricants; Preferably, the volume ratio of solvent to lubricant in the base fluid is (2~4):1; Preferably, the lubricant comprises ethylene glycol and / or polyethylene glycol.

4. The sample preparation method according to claim 2 or 3, characterized in that, The acid solution includes nitric acid solution and / or phosphoric acid solution; Preferably, the particle size of the colloidal silica is 50~100 nm; Preferably, the hardness of the colloidal silica is less than the hardness of the MoSi target material.

5. The sample preparation method according to any one of claims 1 to 4, characterized in that, The rotation speed of the polishing disc during the chemical mechanical polishing process is 80~120 r / min; Preferably, the pressure on the MoSi target sample during the chemical mechanical polishing process is 1~2N; Preferably, the chemical mechanical polishing time is 20-30 minutes; Preferably, the polishing liquid is continuously added during the chemical mechanical polishing process, and the dropping rate is 5~10 mL / min.

6. The sample preparation method according to any one of claims 1 to 5, characterized in that, The polishing process includes a first polishing process and a second polishing process performed sequentially. Preferably, the surface roughness of the MoSi target sample after the first polishing treatment is ≤1μm; Preferably, the surface roughness of the MoSi target sample after the second polishing treatment is ≤0.1μm.

7. The sample preparation method according to claim 6, characterized in that, The first polishing process includes polishing with 400-grit, 800-grit, and 1200-grit sandpaper in sequence; Preferably, the grinding machine pressure during the first grinding process is 5~10N; Preferably, the rotation speed of the grinding machine during the first grinding process is 50~100 r / min.

8. The sample preparation method according to claim 6 or 7, characterized in that, The second polishing process includes polishing with 2000-grit and 5000-grit sandpaper in sequence; Preferably, the grinding machine pressure during the second grinding process is 3~5N; Preferably, the rotation speed of the grinding machine during the second grinding process is 50~100 r / min; Preferably, the second polishing process involves polishing with 5000-grit sandpaper for ≥10 minutes.

9. The sample preparation method according to any one of claims 1 to 8, characterized in that, The mechanical polishing is performed using a wool polishing disc and / or a polyurethane polishing disc. Preferably, the polishing disc rotates at a speed of 100-150 r / min during the mechanical polishing process; Preferably, the pressure on the MoSi target sample during the mechanical polishing process is 2~3N; Preferably, the polishing slurry used for mechanical polishing includes 1μm diamond polishing slurry and / or 0.5μm diamond polishing slurry; Preferably, the concentration of the polishing slurry for mechanical polishing is 5-10 wt%.

10. The sample preparation method according to any one of claims 1 to 9, characterized in that, The sample preparation method also includes cleaning after the chemical mechanical polishing; Preferably, the cleaning includes plasma cleaning; Preferably, the power of the plasma cleaning is 100~200W; Preferably, the plasma cleaning time is 30-60 seconds; Preferably, the sample preparation method further includes an anti-oxidation treatment after the cleaning.

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