Sample preparation method of titanium target material for EBSD detection

Abstract

The invention relates to a sample preparation method of a titanium target material for EBSD detection, and the sample preparation method comprises the following steps: (1) grinding a titanium target material sample to obtain a first sample; (2) carrying out mechanical polishing treatment on the first sample obtained in the step (1) to obtain a second sample; and (3) carrying out ion polishing treatment on the second sample obtained in the step (2) to obtain the EBSD detection sample. According to the sample preparation method provided by the invention, through combined operation of grinding treatment, mechanical polishing treatment and ion polishing treatment, the surface of the sample can be normal and free of scratches, and the EBSD calibration rate and the sample preparation efficiency are relatively high.

Description

Technical Field

[0001] The present invention relates to the technical field of target materials, and particularly relates to a method for preparing a titanium target for EBSD detection. Background Art

[0002] Sputtering targets are widely used in industries such as electronics and information, glass coating, and wear-resistant materials. Mainly through the magnetron sputtering process, under the action of an electric field, Ar ions are accelerated to bombard the target surface, so that target atoms are detached and deposited on the substrate to form a thin film.

[0003] Among them, the semiconductor industry has high requirements for the purity and performance of sputtering targets, and the internal microstructure of the target will seriously affect the performance of the thin film. In order to detect the internal microstructure and tissue uniformity of the target, the existing process usually uses electron backscatter diffraction (EBSD) technology to detect the target. The EBSD technology combines the high-resolution imaging ability of a scanning electron microscope (SEM) and the crystallographic analysis ability of X-ray diffraction (XRD). It can achieve diffraction analysis with a spatial resolution of sub-micrometers while retaining the conventional characteristics of the SEM, and is applicable to a variety of polycrystalline materials, including ceramics, semiconductors, superconductors, and ores. The EBSD technology can provide rich crystallographic information, such as orientation difference, orientation relationship, orientation distribution function (ODF), and interface crystal plane index, etc., providing strong support for in-depth research on the performance of materials.

[0004] As an important sputtering target, titanium targets are widely used in fields such as semiconductors, aerospace, and biomedicine. However, the crystal structure of titanium targets is complex, and the internal microstructure is easily affected by factors such as preparation processes and heat treatment conditions, resulting in uneven orientation distribution. This will not only affect the performance of the sputtered thin film but also increase the risk of material failure. At present, the sample preparation method for titanium targets is not yet perfect, and it is difficult to meet the requirements of the EBSD technology for the surface flatness, non-damage, and high conductivity of the sample, resulting in limited acquisition of orientation distribution information.

[0005] Therefore, developing a sample preparation method for titanium targets suitable for EBSD detection is of great significance for improving the quality and performance of titanium targets. Summary of the Invention

[0006] Aiming at the above problems, the purpose of the present invention is to provide a method for preparing a titanium target for EBSD detection. Compared with the existing technology, the sample preparation method provided by the present invention can make the sample surface smooth and free of scratches, resulting in a high calibration rate for EBSD detection, clear diffraction Kikuchi bands, and relatively high sample preparation efficiency.

[0007] To achieve the purpose of this invention, the present invention adopts the following technical solutions:

[0008] The present invention provides a method for preparing a titanium target for EBSD detection, and the sample preparation method includes the following steps:

[0009] (1) Grind the titanium target sample to obtain a first sample;

[0010] (2) Mechanically polish the first sample obtained in step (1) to obtain a second sample;

[0011] (3) Ion-polish the second sample obtained in step (2) to obtain an EBSD detection sample.

[0012] In the sample preparation method provided by the present invention, first, large defects on the sample surface are removed through grinding treatment to make the sample surface flatter; then, the scratches and minute defects remaining after grinding are further removed through mechanical polishing treatment to make the sample surface smoother; afterwards, through ion polishing treatment, microcracks and stress concentration regions on the surface can be removed, making the sample surface reach extremely high flatness and smoothness. Thus, it can be seen that the sample preparation method provided by the present invention can effectively reduce the surface defects of the sample and improve the surface quality of the sample and the calibration rate of EBSD through the combined operations of grinding treatment, mechanical polishing treatment, and ion polishing treatment.

[0013] Preferably, the titanium target sample is cut before the grinding treatment in step (1).

[0014] Preferably, the size of the titanium target sample after the cutting treatment is (10 - 20) cm × (10 - 20) cm × (5 - 15) cm. For example, it can be 10 cm × 10 cm × 5 cm, 15 cm × 15 cm × 10 cm, or 20 cm × 20 cm × 15 cm, but is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0015] Preferably, the grinding medium used in the grinding treatment in step (1) includes silicon dioxide sandpaper.

[0016] Preferably, the grinding treatment includes first grinding, second grinding, and third grinding carried out in sequence.

[0017] Preferably, the sandpaper mesh number used in the first grinding in step (1) is 240#.

[0018] Preferably, the sandpaper mesh number used in the second grinding is 600#.

[0019] Preferably, the sandpaper mesh number used in the third grinding is 1000#.

[0020] In the present invention, by preferably performing the first grinding, the second grinding, and the third grinding and controlling the mesh number of the abrasive papers used from coarse to fine, the scratches on the surface of the sample can be gradually reduced and minimized, enabling the subsequent mechanical polishing and ion polishing to proceed more smoothly, reducing the time required to remove scratches during the subsequent polishing process, and improving the polishing efficiency.

[0021] Preferably, the mechanical polishing treatment in step (2) includes the first mechanical polishing, the second mechanical polishing, and the third mechanical polishing carried out in sequence.

[0022] Preferably, the polishing liquid used in the first mechanical polishing in step (2) includes a diamond suspension.

[0023] Preferably, the particle size of the diamond in the diamond suspension is 1 - 5 μm. For example, it can be 1 μm, 2 μm, 3 μm, 4 μm, or 5 μm, but is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0024] Preferably, the time for the first mechanical polishing is 5 - 10 min. For example, it can be 5 min, 6 min, 7 min, 8 min, 9 min, or 10 min, but is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0025] Preferably, the polishing liquid used in the second mechanical polishing includes an alumina suspension.

[0026] Preferably, the particle size of the alumina in the alumina suspension is 0.1 - 0.5 μm. For example, it can be 0.1 μm, 0.2 μm, 0.3 μm, 0.4 μm, or 0.5 μm, but is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0027] Preferably, the time for the second mechanical polishing is 5 - 10 min. For example, it can be 5 min, 6 min, 7 min, 8 min, 9 min, or 10 min, but is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0028] Preferably, the polishing liquid used in the third mechanical polishing includes a silica suspension.

[0029] Preferably, the particle size of the silica in the silica suspension is 20 - 80 nm. For example, it can be 20 nm, 30 nm, 40 nm, 50 nm, 60 nm, 70 nm, or 80 nm, but is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0030] Preferably, the time of the third mechanical polishing is 5-10 minutes. For example, it can be 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes or 10 minutes, but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0031] In the present invention, by preferably controlling the mechanical polishing process to include the first mechanical polishing, the second mechanical polishing and the third mechanical polishing carried out in sequence, and preferably controlling the particle size and time of the polishing particles used in the mechanical polishing, the surface can be gradually refined, effectively reducing the depth and number of surface scratches, thereby reducing the surface stress. While achieving a good polishing effect, over-polishing is avoided.

[0032] Preferably, the ion polishing treatment in step (3) includes the first ion polishing, the second ion polishing, the third ion polishing and the fourth ion polishing carried out in sequence.

[0033] Preferably, the voltage of the first ion polishing in step (3) is 2-4 kV. For example, it can be 2 kV, 2.2 kV, 2.4 kV, 2.6 kV, 2.8 kV, 3 kV, 3.2 kV, 3.4 kV, 3.6 kV, 3.8 kV or 4 kV, but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0034] Preferably, the current of the first ion polishing is 0.2-0.4 mA. For example, it can be 0.2 mA, 0.22 mA, 0.24 mA, 0.26 mA, 0.28 mA, 0.3 mA, 0.32 mA, 0.34 mA, 0.36 mA, 0.38 mA or 0.4 mA, but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0035] Preferably, the time of the first ion polishing is 1-3 minutes. For example, it can be 1 minute, 1.2 minutes, 1.4 minutes, 1.6 minutes, 1.8 minutes, 2 minutes, 2.2 minutes, 2.4 minutes, 2.6 minutes, 2.8 minutes or 3 minutes, but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0036] Preferably, the voltage of the second ion polishing is 4-6 kV. For example, it can be 4 kV, 4.2 kV, 4.6 kV, 4.8 kV, 5 kV, 5.2 kV, 5.4 kV, 5.6 kV, 5.8 kV or 6 kV, but is not limited to the listed values. Other unlisted values within the numerical range are equally applicable.

[0037] Preferably, the current of the second ion polishing is 0.2 - 0.4 mA. For example, it can be 0.2 mA, 0.22 mA, 0.24 mA, 0.26 mA, 0.28 mA, 0.3 mA, 0.32 mA, 0.34 mA, 0.36 mA, 0.38 mA or 0.4 mA. However, it is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0038] Preferably, the time of the second ion polishing is 1 - 3 min. For example, it can be 1 min, 1.2 min, 1.4 min, 1.6 min, 1.8 min, 2 min, 2.2 min, 2.4 min, 2.6 min, 2.8 min or 3 min. However, it is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0039] Preferably, the voltage of the third ion polishing in step (3) is 6 - 8 kV. For example, it can be 6 kV, 6.2 kV, 6.4 kV, 6.6 kV, 6.8 kV, 7 kV, 7.2 kV, 7.4 kV, 7.6 kV, 7.8 kV or 8 kV. However, it is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0040] Preferably, the current of the third ion polishing is 0.2 - 0.4 mA. For example, it can be 0.2 mA, 0.22 mA, 0.24 mA, 0.26 mA, 0.28 mA, 0.3 mA, 0.32 mA, 0.34 mA, 0.36 mA, 0.38 mA or 0.4 mA. However, it is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0041] Preferably, the time of the third ion polishing is 20 - 40 min. For example, it can be 20 min, 22 min, 24 min, 26 min, 28 min, 30 min, 32 min, 34 min, 36 min, 38 min or 40 min. However, it is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0042] Preferably, the voltage of the fourth ion polishing is 4 - 6 kV. For example, it can be 4 kV, 4.2 kV, 4.6 kV, 4.8 kV, 5 kV, 5.2 kV, 5.4 kV, 5.6 kV, 5.8 kV or 6 kV. However, it is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0043] Preferably, the current of the fourth ion polishing is 0.2 - 0.4 mA. For example, it can be 0.2 mA, 0.22 mA, 0.24 mA, 0.26 mA, 0.28 mA, 0.3 mA, 0.32 mA, 0.34 mA, 0.36 mA, 0.38 mA or 0.4 mA. However, it is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0044] Preferably, the time of the fourth ion polishing is 1 - 3 min. For example, it can be 1 min, 1.2 min, 1.4 min, 1.6 min, 1.8 min, 2 min, 2.2 min, 2.4 min, 2.6 min, 2.8 min or 3 min. However, it is not limited to the listed values, and other unlisted values within the numerical range are equally applicable.

[0045] In the present invention, by preferably controlling the ion polishing treatment including the first ion polishing, the second ion polishing, the third ion polishing and the fourth ion polishing carried out in sequence, and preferably controlling the voltage, current and time of the ion polishing, the polishing effect can be gradually optimized, the energy and action intensity of the ion beam can be precisely controlled, the damage to the sample surface can be reduced, the flatness and smoothness of the sample surface can be significantly improved, and a high EBSD calibration rate can be achieved.

[0046] As a preferred technical solution of the present invention, the sample preparation method includes the following steps:

[0047] (1) Cut the titanium target sample to a size of (10 - 20) cm × (10 - 20) cm × (5 - 15) cm, and then perform grinding treatment with silicon dioxide sandpaper, that is, first perform the first grinding with 240# sandpaper, then perform the second grinding with 600# sandpaper, and then perform the third grinding with 1000# sandpaper to obtain the first sample;

[0048] (2) Perform mechanical polishing on the first sample obtained in step (1), that is, first perform the first mechanical polishing with a diamond suspension with a particle size of 1 - 5 μm for 5 - 10 min, then perform the second mechanical polishing with an alumina suspension with a particle size of 0.1 - 0.5 μm for 5 - 10 min, and then perform the third mechanical polishing with a silicon dioxide suspension with a particle size of 20 - 80 nm for 5 - 10 min to obtain the second sample;

[0049] (3) Ion-polish the second sample obtained in step (2), that is, first perform the first ion polishing under the conditions of a voltage of 2 - 4 kV, a current of 0.2 - 0.4 mA, and a time of 1 - 3 min, then perform the second ion polishing under the conditions of a voltage of 4 - 6 kV, a current of 0.2 - 0.4 mA, and a time of 1 - 3 min, then perform the third ion polishing under the conditions of a voltage of 6 - 8 kV, a current of 0.2 - 0.4 mA, and a time of 20 - 40 min, and finally perform the fourth ion polishing under the conditions of a voltage of 4 - 6 kV, a current of 0.2 - 0.4 mA, and a time of 1 - 3 min to obtain an EBSD detection sample.

[0050] Compared with the prior art, the present invention has the following beneficial effects:

[0051] (1) The sample preparation method provided by the present invention can make the sample surface flat and scratch-free through a combined operation of grinding treatment, mechanical polishing treatment, and ion polishing treatment, and has a high sample preparation efficiency, shortening the sample preparation cycle and being able to quickly obtain a sample meeting the EBSD detection requirements.

[0052] (2) The EBSD detection sample obtained by the present invention has a high calibration rate, making the diffraction Kikuchi bands obtained by EBSD detection clearly distinguishable, facilitating accurate crystal orientation analysis and microstructure characterization. The sample preparation method provided by the present invention can make the calibration rate of the EBSD detection sample reach more than 98% under optimal conditions. Specific embodiments

[0053] The technical solution of the present invention will be further described below through specific embodiments. Those skilled in the art should understand that the embodiments are only for helping to understand the present invention and should not be regarded as specific limitations on the present invention.

[0054] Example 1

[0055] This example provides a sample preparation method for a titanium target for EBSD detection, and the sample preparation method includes the following steps:

[0056] (1) Cut the titanium target sample to a size of 15 cm × 15 cm × 10 cm, and then perform grinding treatment with silicon dioxide sandpaper, that is, first perform the first grinding with 240# sandpaper, then perform the second grinding with 600# sandpaper, and then perform the third grinding with 1000# sandpaper to obtain a first sample;

[0057] (2) Perform mechanical polishing on the first sample obtained in step (1), that is, first perform the first mechanical polishing for 5 minutes using a diamond suspension with a particle size of 3 μm, then perform the second mechanical polishing for 5 minutes using an alumina suspension with a particle size of 0.3 μm, and then perform the third mechanical polishing for 5 minutes using a silica suspension with a particle size of 50 nm to obtain a second sample;

[0058] (3) Perform ion polishing on the second sample obtained in step (2), that is, first perform the first ion polishing under the conditions of a voltage of 3 kV, a current of 0.3 mA, and a time of 2 minutes, then perform the second ion polishing under the conditions of a voltage of 5 kV, a current of 0.3 mA, and a time of 2 minutes, then perform the third ion polishing under the conditions of a voltage of 7 kV, a current of 0.3 mA, and a time of 30 minutes, and finally perform the fourth ion polishing under the conditions of a voltage of 5 kV, a current of 0.3 mA, and a time of 2 minutes to obtain an EBSD detection sample.

[0059] Example 2

[0060] This example provides a method for preparing a titanium target for EBSD detection, and the sample preparation method includes the following steps:

[0061] (1) Cut the titanium target sample to a size of 10 cm × 10 cm × 5 cm, and then perform grinding treatment using silica sandpaper, that is, first perform the first grinding using 240# sandpaper, then perform the second grinding using 600# sandpaper, and then perform the third grinding using 1000# sandpaper to obtain a first sample;

[0062] (2) Perform mechanical polishing on the first sample obtained in step (1), that is, first perform the first mechanical polishing for 7 minutes using a diamond suspension with a particle size of 5 μm, then perform the second mechanical polishing for 7 minutes using an alumina suspension with a particle size of 0.5 μm, and then perform the third mechanical polishing for 7 minutes using a silica suspension with a particle size of 80 nm to obtain a second sample;

[0063] (3) Perform ion polishing on the second sample obtained in step (2), that is, first perform the first ion polishing under the conditions of a voltage of 2 kV, a current of 0.4 mA, and a time of 3 minutes, then perform the second ion polishing under the conditions of a voltage of 4 kV, a current of 0.4 mA, and a time of 1 minute, then perform the third ion polishing under the conditions of a voltage of 6 kV, a current of 0.4 mA, and a time of 40 minutes, and finally perform the fourth ion polishing under the conditions of a voltage of 4 kV, a current of 0.4 mA, and a time of 3 minutes to obtain an EBSD detection sample.

[0064] Example 3

[0065] This embodiment provides a sample preparation method for a titanium target used in EBSD detection. The sample preparation method includes the following steps:

[0066] (1) Cut the titanium target sample to a size of 20 cm × 20 cm × 15 cm, and then perform grinding treatment with silicon dioxide sandpaper. First, perform the first grinding with 240# sandpaper, then perform the second grinding with 600# sandpaper, and then perform the third grinding with 1000# sandpaper to obtain the first sample;

[0067] (2) Perform mechanical polishing on the first sample obtained in step (1). First, perform the first mechanical polishing for 10 min with a diamond suspension with a particle size of 1 μm, then perform the second mechanical polishing for 10 min with an alumina suspension with a particle size of 0.1 μm, and then perform the third mechanical polishing for 10 min with a silicon dioxide suspension with a particle size of 20 nm to obtain the second sample;

[0068] (3) Perform ion polishing on the second sample obtained in step (2). First, perform the first ion polishing under the conditions of a voltage of 4 kV, a current of 0.2 mA, and a time of 1 min, then perform the second ion polishing under the conditions of a voltage of 6 kV, a current of 0.2 mA, and a time of 3 min, then perform the third ion polishing under the conditions of a voltage of 8 kV, a current of 0.2 mA, and a time of 20 min, and finally perform the fourth ion polishing under the conditions of a voltage of 6 kV, a current of 0.2 mA, and a time of 1 min to obtain the EBSD detection sample.

[0069] Example 4

[0070] This embodiment provides a sample preparation method for a titanium target used in EBSD detection. The difference between this sample preparation method and that of Example 1 is only that the sandpapers for the second grinding and the third grinding are the same as those for the first grinding.

[0071] Example 5

[0072] This embodiment provides a sample preparation method for a titanium target used in EBSD detection. The difference between this sample preparation method and that of Example 1 is only that the polishing liquids used for the second mechanical polishing and the third mechanical polishing are the same as those for the first mechanical polishing.

[0073] Example 6

[0074] This embodiment provides a sample preparation method for a titanium target used in EBSD detection. The difference between this sample preparation method and that of Example 1 is only that the voltages, currents, and times used for the second ion polishing, the third ion polishing, and the fourth ion polishing are the same as those for the first ion polishing.

[0075] Example 7

[0076] This embodiment provides a sample preparation method for a titanium target for EBSD detection. The only difference between this sample preparation method and that of Embodiment 1 is that the voltage of the second ion polishing is 3 kV.

[0077] Embodiment 8

[0078] This embodiment provides a sample preparation method for a titanium target for EBSD detection. The only difference between this sample preparation method and that of Embodiment 1 is that the voltage of the second ion polishing is 7 kV.

[0079] Embodiment 9

[0080] This embodiment provides a sample preparation method for a titanium target for EBSD detection. The only difference between this sample preparation method and that of Embodiment 1 is that the voltage of the third ion polishing is 5 kV.

[0081] Embodiment 10

[0082] This embodiment provides a sample preparation method for a titanium target for EBSD detection. The only difference between this sample preparation method and that of Embodiment 1 is that the voltage of the third ion polishing is 9 kV.

[0083] Embodiment 11

[0084] This embodiment provides a sample preparation method for a titanium target for EBSD detection. The only difference between this sample preparation method and that of Embodiment 1 is that the voltage of the fourth ion polishing is 3 kV.

[0085] Embodiment 12

[0086] This embodiment provides a sample preparation method for a titanium target for EBSD detection. The only difference between this sample preparation method and that of Embodiment 1 is that the voltage of the fourth ion polishing is 7 kV.

[0087] Comparative Example 1

[0088] This comparative example provides a sample preparation method for a titanium target for EBSD detection. The only difference between this sample preparation method and that of Embodiment 1 is that no grinding treatment is performed, and the titanium target sample is directly subjected to the first mechanical polishing.

[0089] Comparative Example 2

[0090] This comparative example provides a sample preparation method for a titanium target for EBSD detection. The only difference between this sample preparation method and that of Embodiment 1 is that no mechanical polishing treatment is performed, and the first sample is directly subjected to the first ion polishing.

[0091] Comparative Example 3

[0092] This comparative example provides a method for preparing a titanium target for EBSD detection, which is only different from that of Example 1 in that ion polishing treatment is not performed, and the second sample is the EBSD detection sample.

[0093] The EBSD detection samples obtained from the above examples and comparative examples were subjected to EBSD detection, and the calibration rates obtained are shown in Table 1.

[0094] Table 1

[0095] Calibration rate / % Example 1 99 Example 2 98 Example 3 98 Example 4 85 Example 5 83 Example 6 89 Example 7 94 Example 8 92 Example 9 95 Example 10 88 Example 11 97 Example 12 96 Comparative Example 1 82 Comparative Example 2 79 Comparative Example 3 72

[0096] It can be seen from the data in Table 1 as follows:

[0097] (1) It can be seen from the data of Examples 1-3 that by using the sample preparation method provided by the present invention, under relatively optimal conditions, the calibration rate of the EBSD detection sample can reach more than 98%.

[0098] (2) By comprehensively comparing the data of Example 1 and Examples 4-6, it can be seen that the present invention can further improve the surface quality of the sample and the EBSD calibration rate by preferably performing the first to third grinding, preferably performing the first to third mechanical polishing, preferably performing the first to fourth ion polishing, and controlling different processing parameters.

[0099] (3) By comprehensively comparing the data of Example 1 and Examples 7-12, it can be seen that the present invention can further improve the surface quality of the sample and the EBSD calibration rate by preferably controlling the voltage of each step of ion polishing within a specific range.

[0100] (4) By comprehensively comparing the data of Example 1 and Comparative Examples 1-3, it can be seen that the sample preparation method provided by the present invention can make the surface of the sample flat and scratch-free through a combination of grinding treatment, mechanical polishing treatment and ion polishing treatment, so that the EBSD detection sample has a high calibration rate.

[0101] The applicant declares that the above description is only a specific implementation manner 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 thought of by those skilled in the art within the technical scope disclosed by the present invention fall within the protection scope and the disclosure scope of the present invention.

Claims

1. A sample preparation method for a titanium target used in EBSD detection, characterized in that, The sample preparation method includes the following steps: (1) Grind the titanium target sample to obtain a first sample; (2) Mechanically polish the first sample obtained in step (1) to obtain a second sample; (3) Ion-polish the second sample obtained in step (2) to obtain an EBSD detection sample.

2. The sample preparation method according to claim 1, wherein Before the grinding treatment in step (1), the titanium target sample is cut; Preferably, the size of the titanium target sample after the cutting treatment is (10-20) cm × (10-20) cm × (5-15) cm.

3. The sample preparation method according to claim 1 or 2, characterized in that The grinding medium used in the grinding treatment in step (1) includes silica sandpaper; Preferably, the grinding treatment includes first grinding, second grinding, and third grinding carried out in sequence.

4. The sample preparation method according to claim 3, wherein The grit size of the sandpaper used in the first grinding in step (1) is 240#; Preferably, the grit size of the sandpaper used in the second grinding is 600#; Preferably, the grit size of the sandpaper used in the third grinding is 1000#.

5. The sample preparation method according to any one of claims 1-4, characterized in that, The mechanical polishing treatment in step (2) includes first mechanical polishing, second mechanical polishing, and third mechanical polishing carried out in sequence.

6. The sample preparation method according to claim 5, characterized in that, The polishing liquid used in the first mechanical polishing in step (2) includes diamond suspension; Preferably, the particle size of the diamond in the diamond suspension is 1-5 μm; Preferably, the time of the first mechanical polishing is 5-10 min; Preferably, the polishing liquid used in the second mechanical polishing includes alumina suspension; Preferably, the particle size of the alumina in the alumina suspension is 0.1-0.5 μm; Preferably, the time of the second mechanical polishing is 5-10 min; Preferably, the polishing liquid used in the third mechanical polishing includes silica suspension; Preferably, the particle size of the silica in the silica suspension is 20-80 nm; Preferably, the time of the third mechanical polishing is 5-10 min.

7. The sample preparation method according to any one of claims 1-6, characterized in that, The ion polishing treatment in step (3) includes first ion polishing, second ion polishing, third ion polishing, and fourth ion polishing carried out in sequence.

8. The sample preparation method according to claim 7, characterized in that, The voltage of the first ion polishing in step (3) is 2-4 kV; Preferably, the current of the first ion polishing is 0.2-0.4 mA; Preferably, the time of the first ion polishing is 1-3 min; Preferably, the voltage of the second ion polishing is 4-6 kV; Preferably, the current of the second ion polishing is 0.2-0.4 mA; Preferably, the time of the second ion polishing is 1-3 min.

9. The sample preparation method according to claim 7 or 8, characterized in that The voltage of the third ion polishing in step (3) is 6-8 kV; Preferably, the current of the third ion polishing is 0.2-0.4 mA; Preferably, the time of the third ion polishing is 20-40 min; Preferably, the voltage of the fourth ion polishing is 4-6 kV; Preferably, the current of the fourth ion polishing is 0.2-0.4 mA; Preferably, the time of the fourth ion polishing is 1-3 min.

10. The sample preparation method according to any one of claims 1-9, characterized in that, The sample preparation method includes the following steps: (1) Cut the titanium target sample to a size of (10 - 20) cm × (10 - 20) cm × (5 - 15) cm, and then perform grinding treatment with silicon dioxide sandpaper, that is, first perform the first grinding with 240# sandpaper, then perform the second grinding with 600# sandpaper, and then perform the third grinding with 1000# sandpaper to obtain the first sample; (2) Perform mechanical polishing on the first sample obtained in step (1), that is, first perform the first mechanical polishing for 5 - 10 min with a diamond suspension with a particle size of 1 - 5 μm, then perform the second mechanical polishing for 5 - 10 min with an alumina suspension with a particle size of 0.1 - 0.5 μm, and then perform the third mechanical polishing for 5 - 10 min with a silicon dioxide suspension with a particle size of 20 - 80 nm to obtain the second sample; (3) Perform ion polishing on the second sample obtained in step (2), that is, first perform the first ion polishing under the conditions of a voltage of 2 - 4 kV, a current of 0.2 - 0.4 mA, and a time of 1 - 3 min, then perform the second ion polishing under the conditions of a voltage of 4 - 6 kV, a current of 0.2 - 0.4 mA, and a time of 1 - 3 min, then perform the third ion polishing under the conditions of a voltage of 6 - 8 kV, a current of 0.2 - 0.4 mA, and a time of 20 - 40 min, and finally perform the fourth ion polishing under the conditions of a voltage of 4 - 6 kV, a current of 0.2 - 0.4 mA, and a time of 1 - 3 min to obtain the EBSD detection sample.