Method for preparing 3D printed titanium alloy ebsd sample and application

Abstract

This invention relates to a method for preparing and applying 3D-printed titanium alloy EBSD samples, and pertains to the field of metallographic testing technology. The preparation method utilizes a polishing technique with controllable interface transformation to create a "abrasive-free, controllable interface transformation" polishing environment, fundamentally solving the oxidation-embedding coupling problem inherent in the preparation of titanium alloy EBSD samples.

Description

Technical Field

[0001] This invention relates to the field of metallographic testing technology, and to the preparation method and application of 3D printed titanium alloy EBSD samples. Background Technology

[0002] With the increasing demands for performance of complex components in fields such as nuclear power and aerospace, 3D-printed titanium alloys (e.g., TC4), represented by laser powder bed fusion technology, are gaining popularity due to their high degree of freedom in forming and excellent performance. EBSD technology is a key means to analyze their non-equilibrium solidification structure and reveal the process-structure-property relationship.

[0003] However, the preparation of 3D-printed titanium alloy EBSD samples faces severe challenges. Conventional vibratory polishing methods, borrowed from steel materials, perform extremely poorly when applied to titanium alloys. The fundamental reason lies in the extremely reactive chemical properties of titanium. During vibratory polishing, once the fresh surface of the sample is exposed, it reacts instantly with oxygen in the air, forming a dense, hard, and chemically stable TiO2 oxide film. This oxide film undergoes periodic rupture under continuous vibration loads, and the soft metal matrix exposed at the rupture points is easily pressed into and embedded by hard abrasive particles (such as Al2O3 and SiO2) in the polishing slurry, forming surface contamination that is difficult to remove. Ultimately, this results in the presence of both residual deformation layers and abrasive contamination on the sample surface, such as... Figure 1 As shown, the Kikuchi pattern in EBSD is blurry or even impossible to generate.

[0004] To address this issue, some researchers have proposed adding components such as urea, hydrogen peroxide, and fumed silica to synergistically remove material. However, this approach relies on the mechanical cutting action of solid abrasives, which cannot solve the inherent "abrasive embedding" problem in vibratory polishing of titanium alloys. Furthermore, the stability of its complex multi-component system is difficult to guarantee during long-term vibratory polishing, making it unsuitable for 3D-printed titanium alloys with more reactive chemical properties. Therefore, a new method for preparing titanium alloy EBSD samples that can fundamentally avoid abrasive contamination and effectively remove the surface deformation layer is urgently needed. Summary of the Invention

[0005] To address the aforementioned problems, this invention provides a method for preparing 3D-printed titanium alloy EBSD samples. This method constructs a polishing environment that is "abrasive-free and has controllable interface transformation" through a polishing method with controllable interface transformation, fundamentally solving the oxidation-embedding coupling problem in the preparation process of titanium alloy EBSD samples.

[0006] This invention provides a method for preparing 3D printed titanium alloy EBSD samples, comprising the following steps: Sample pretreatment and mechanical polishing: The sample is cut to obtain the sample, and the test surface of the sample is ground and polished to make the test surface mirror-like; the test surface is mechanically polished using a polishing agent; Interface conversion polishing: The mechanically polished sample is placed in an interface conversion polishing solution, with the liquid level higher than the detection surface of the sample to form a liquid phase isolation. Vibration polishing is then performed, followed by washing and drying to obtain a 3D printed titanium alloy EBSD sample. The interface conversion polishing solution is composed of water and hydrogen peroxide solution, with a volume ratio of water to hydrogen peroxide solution of 4:1 and a mass percentage concentration of 30% for the hydrogen peroxide solution.

[0007] Addressing the challenges of preparing titanium alloy EBSD samples in existing technologies, the inventors tackled two key problems: "too rapid oxidation and too slow removal" of titanium alloys. They discovered that completely preventing surface oxidation of titanium alloys is thermodynamically nearly impossible, and that the solid abrasives in traditional polishing slurries are the root cause of "embedded contamination." Therefore, this invention adopts a reverse approach: instead of preventing oxidation, it regulates the oxidation products to make them easier to remove, completely eliminating solid abrasives. Specifically, by adding an appropriate amount of hydrogen peroxide to the vibratory polishing slurry, an interfacial conversion polishing slurry is formed. This allows a substance (such as hydrated titanium oxide) to form a complex with titanium ions on the titanium alloy surface in a liquid phase environment. This oxide film is "softer" and more easily removed by liquid shear force compared to the dense TiO2 formed in natural air. The concentration of hydrogen peroxide needs to be strictly controlled; otherwise, it may accelerate harmful oxidation. Simultaneously, before vibratory polishing, the thickness of the mechanically deformed layer on the sample surface must be minimized through fine mechanical polishing. Ideally, vibratory polishing should only be responsible for removing the last few tens of nanometers of oxide film and extremely minor damage. The entire preparation process must be completed in one go, without lingering for too long in between, to avoid the formation of a new dense oxide film on the titanium alloy in the air.

[0008] In one embodiment, in the interface conversion polishing step, the vibration frequency of the vibration polishing is 100-200Hz, and the vibration polishing time is calculated based on the interface conversion-thinning synergistic process model. The interface transformation-thinning synergistic process model is shown below: ; Wherein, t is the vibration polishing time; h0 is the maximum thickness of the residual deformation layer on the sample surface after mechanical polishing; C is the mass percentage concentration of the hydrogen peroxide solution; T is the ambient temperature during vibration polishing, ranging from 293K to 303K; e is the natural logarithm, with a value of 2.718; Eα is the apparent activation energy of the interfacial transformation reaction of titanium in the interfacial transformation polishing solution system, with a value of 2.5×10⁴ J / mol; R is the ideal gas constant, with a value of 8.314 J / (mol·K); K is the process correction coefficient, which is 2.0×10⁻³ when the vibration frequency of the vibration polishing is ≥150Hz, and 1.0×10⁻³ when the vibration frequency of the vibration polishing is <150Hz.

[0009] In one embodiment, the sample pretreatment and mechanical polishing steps include grinding and polishing the test surface by using wet sandpaper to grind the test surface until it is flat, and polishing the test surface by using diamond spray.

[0010] In one embodiment, the wet sandpaper has a mesh size of at least one of 400 mesh and 1200 mesh; The diamond spray has a particle size of at least one of 5μm, 1.5μm, and 0.5μm.

[0011] In one embodiment, in the sample pretreatment and mechanical polishing step, the polishing agent includes an alumina suspension and a hydrogen peroxide solution, wherein the volume ratio of the alumina suspension to the hydrogen peroxide solution is 4:1.

[0012] In one embodiment, the hydrogen peroxide solution has a mass percentage concentration of 30% in the sample pretreatment and mechanical polishing steps.

[0013] In one embodiment, in the sample pretreatment and mechanical polishing step, the detection surface is mechanically polished until the oxide film attached to the detection surface is removed, and the polishing speed of the mechanical polishing is 300-400 r / min.

[0014] In one embodiment, the mechanical polishing time is ≥5 min.

[0015] In one embodiment, during the interface conversion polishing step, the liquid level is 1-3 mm higher than the detection surface of the sample; the load for the vibration polishing is 200 g.

[0016] In one embodiment, the preparation method includes the following steps: Step 1: Sample pretreatment and fine mechanical polishing: The sample is wire-cut into pieces with a length of 10-20 mm, a width of 10-20 mm, and a thickness of 2-3 mm. These pieces are then cold-mounted into Φ40×20 mm blocks (the size can be determined according to the abrasive tool used). The mounted samples are then polished with 400-grit and 1200-grit wet sandpaper until a smooth and fine surface is achieved. Polishing is then performed using 5μm, 1.5μm, and 0.5μm diamond sprays until a smooth and clean mirror surface is achieved.

[0017] Add 10 ml of hydrogen peroxide to 40 ml of alumina suspension, and perform fine mechanical polishing on a clean, dedicated short-pile polishing cloth. During this stage, the polishing speed should be reduced to 300-400 r / min, and the polishing time should be greater than 5 min.

[0018] Step 2: Preparation of the interface conversion polishing slurry: An interface conversion polishing slurry for vibratory polishing is prepared, comprising deionized water and a conversion accelerator, and containing no solid abrasive particles. Specifically, a hydrogen peroxide aqueous solution is prepared. Step 1: Mix 400ml of distilled water with 100ml of 30% hydrogen peroxide (superior grade) and stir well.

[0019] Step 2: Pour the hydrogen peroxide solution prepared in Step 1 into the vibratory polishing disc (the amount added can be adjusted according to the size of the polishing disc, ensuring that the height of the hydrogen peroxide solution in the polishing disc is 1~3mm above the height of the embedded sample (to ensure that the sample surface to be polished is completely immersed in the diluent and does not come into contact with air, thus achieving an oxygen-free environment). Step 3: Interface transformation vibration polishing based on process model: Place the sample treated in step one onto the sample holder of the vibratory polisher. Add the interfacial conversion polishing slurry prepared in step two to the polishing disc, ensuring the slurry level is 1-3 mm above the sample surface to be polished, forming a liquid phase isolation layer. Then, load a 200g weight and vibrate at a frequency of 100-200Hz.

[0020] To achieve precise control and repeatability of the process, this invention establishes the following interface transformation-thinning synergistic process model based on extensive experimental data to determine the optimal vibration polishing time parameters: ; Wherein, t is the vibration polishing time (unit: h); h0 is the maximum thickness of the residual deformation layer on the sample surface after mechanical polishing (unit: nm), which can be measured by equipment such as a white light interferometer; C is the mass percentage concentration of hydrogen peroxide solution (%); T is the ambient temperature during the vibration polishing process (unit: K), with a value ranging from 293K to 303K; e is the natural logarithm, with a value of 2.718; Eα is the apparent activation energy of the interfacial transformation reaction of titanium in the interfacial transformation polishing solution system (unit: J / mol), with an empirical value of 2.5×10⁴ J / mol based on experimental fitting; R is the ideal gas constant, with a value of 8.314 J / (mol·K); K is the process correction coefficient, with a value of 2.0×10⁻³ when the vibration frequency of the vibration polishing is ≥150Hz, and a value of 1.0×10⁻³ when the vibration frequency of the vibration polishing is <150Hz. After polishing, remove the sample and rinse it with running water for 2 minutes. Place it in a beaker, add anhydrous ethanol, and clean it with ultrasound for 5 minutes. After drying, remove the sample from the mounting mold and perform EBSD detection and analysis as soon as possible.

[0021] The present invention also provides 3D printed titanium alloy EBSD samples obtained by the preparation method described above.

[0022] The present invention also provides an EBSD detection and analysis method, which uses the 3D printed titanium alloy EBSD sample obtained by the preparation method or the 3D printed titanium alloy EBSD sample to perform detection and analysis.

[0023] The present invention also provides the application of the preparation method or the 3D printed titanium alloy EBSD sample in EBSD detection and analysis methods.

[0024] Compared with the prior art, the present invention has the following beneficial effects: 1. Innovative Principle (Interface Transformation Mechanism): This invention proposes for the first time a polishing mechanism of "interface transformation-thinning synergy" and establishes a corresponding process model. Unlike traditional polishing that attempts to completely suppress surface reactions ("complete suppression of surface reactions" is thermodynamically infeasible for titanium alloys), this invention constructs a controllable liquid-phase reaction environment using low-concentration H2O2, causing a loose, easily removable hydrated oxide intermediate layer on the titanium alloy surface. This "controllable interface transformation" replaces "natural air oxidation," thereby achieving layer-by-layer, efficient thinning of the deformed layer.

[0025] 2. Avoiding abrasive contamination: The polishing slurry of this invention contains no solid abrasive particles, which fundamentally eliminates the "embedded contamination" problem of abrasive embedding into the sample surface in traditional vibration polishing, ensuring the purity of the EBSD analysis surface, so that the BC diagram can truly reflect the microstructure such as grain boundaries and phase boundaries without interference from false information.

[0026] 3. Quantifiable and Portable Process: The process model proposed in this invention quantifies and correlates polishing time with key parameters such as initial deformed layer thickness, H2O2 concentration, and ambient temperature. This eliminates reliance on the operator's personal experience, allowing different personnel and laboratories to quickly determine the optimal polishing process through simple measurements and calculations, demonstrating strong reproducibility and versatility.

[0027] 4. High calibration rate and high quality: The 3D printed TC4 titanium alloy EBSD sample prepared by the method of this invention can achieve a stable calibration rate of over 98%. The resulting IPF image has clear grain orientation and a complete grain map without fragments, which fully meets the needs of high-end materials science research. Attached Figure Description

[0028] Figure 1 The morphology (SEM image) of the TC4 titanium alloy EBSD sample after conventional vibration polishing shows the defective and abrasive contamination. Figure 2 The BC+IPF+GB surface distribution diagram of the 3D printed TC4 titanium alloy sample in Example 1 (calibration rate 98%). Figure 3 The BC+IPF+GB surface distribution diagram of the 3D printed TC4 titanium alloy sample in Comparative Example 1 (calibration rate is 0). Figure 4 The BC+IPF+GB surface distribution diagram of the 3D printed TC4 titanium alloy sample in Comparative Example 2 is shown (calibration rate 78.9%). Detailed Implementation

[0029] To facilitate understanding of the present invention, a more complete description will be given below with reference to the accompanying drawings. Preferred embodiments of the invention are shown in the drawings. However, the invention can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a thorough and complete understanding of the disclosure of the invention.

[0030] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0031] Unless otherwise specified, all reagents, materials, and equipment used in this embodiment are commercially available; unless otherwise specified, all test methods are conventional test methods in this field.

[0032] Example 1: 3D printed TC4 titanium alloy sample I. Sample Preparation The sample is wire-cut into pieces with a length of 10-20 mm, a width of 10-20 mm, and a thickness of 2-3 mm. These pieces are then cold-mounted into Φ40×20 mm blocks (the size can be determined according to the abrasive used). The mounted samples are then polished with 400-grit and 1200-grit wet sandpaper until a smooth and fine surface is achieved. Polishing is then performed by using 5μm, 1.5μm, and 0.5μm diamond sprays to polish the test surface to a smooth and clean mirror finish.

[0033] Add 10 ml of hydrogen peroxide to 40 ml of alumina suspension, and perform fine mechanical polishing with running water on a clean, dedicated short-pile polishing cloth. During this stage, the polishing speed should be reduced to 300-400 r / min, and the polishing time should be greater than 5 min, until the oxide film adhering to the test surface is removed.

[0034] II. Preparation of Interface Conversion Polishing Slurry Preparation of hydrogen peroxide aqueous solution Step 1: Mix 400ml of distilled water with 100ml of 30% hydrogen peroxide (analytical grade) and stir until homogeneous. This yields an interface conversion polishing slurry with an H2O2 volume concentration of approximately 4.76%. This polishing slurry does not contain any solid abrasives.

[0035] Step 2: Pour the hydrogen peroxide aqueous solution prepared in Step 1 into the vibratory polishing disc (the amount added can be adjusted according to the size of the polishing disc, ensuring that the height of the hydrogen peroxide aqueous solution in the polishing disc is 1-3mm above the height of the embedded sample, so that the sample surface to be polished is completely immersed in the diluent and does not come into contact with air, thus achieving an oxygen-free environment). III. Interface Transformation Vibration Polishing Based on Process Model The thickness of the residual deformation layer on the sample surface after step one, h0 = 500 nm, was measured using a white light interferometer. Ambient temperature... T =298K. The frequency of the vibratory polishing machine is set to 150Hz. From the table, the process correction factor K = 2.0 × 10⁻⁶. 3 Substitute the following interface transformation-thinning collaborative process model to determine the optimal vibration polishing time parameters: ; t is the vibration polishing time (in h); h0 is the maximum thickness of the residual deformation layer on the sample surface after mechanical polishing (in nm); C is the mass percentage concentration of hydrogen peroxide solution (%); T is the ambient temperature during vibration polishing (in K), ranging from 293K to 303K; e is the natural logarithm, with a value of 2.718; Eα is the apparent activation energy of the interfacial transformation reaction of titanium in the interfacial transformation polishing solution system (in J / mol), with a value of 2.5 × 10⁴ J / mol; R is the ideal gas constant, with a value of 8.314 J / (mol·K); K is the process correction coefficient, which is 2.0 × 10⁻³ when the vibration frequency of the vibration polishing is ≥150Hz, and 1.0 × 10⁻³ when the vibration frequency of the vibration polishing is <150Hz.

[0036] The polishing time was calculated using the aforementioned interface transformation-thinning synergistic process model. t =4.8h.

[0037] Pour the prepared polishing solution into the polishing pan, ensuring the solution level is 1.5 mm above the sample. Place the sample in the pan, add a 200 g weight, and start vibration polishing. After polishing for the calculated time of 4.8 hours, remove the sample, rinse with running water, ultrasonically clean with anhydrous ethanol for 5 minutes, and then dry. Perform EBSD analysis on a SEM. The results are as follows: Figure 2 As shown, the BC diagram is clean and uncontaminated, the IPF diagram shows clear grain orientation, and the GB diagram shows complete grain boundaries, with a calibration rate of 98.5%.

[0038] Comparative Example 1: 3D printed TC4 titanium alloy sample The main difference compared to Example 1 is that H2O2 is not added.

[0039] I. Sample Preparation The sample is wire-cut into pieces with a length of 10-20 mm, a width of 10-20 mm, and a thickness of 2-3 mm. These pieces are then cold-mounted into Φ40×20 mm blocks (the size can be determined according to the abrasive tool used). The mounted samples are then polished with 400-grit and 1200-grit wet sandpaper until a smooth and fine surface is achieved. Polishing is then performed using 5μm, 1.5μm, and 0.5μm diamond sprays until a smooth and clean mirror surface is achieved.

[0040] II. Vibratory Polishing Step 1: Mix 100ml of distilled water and 20ml of alumina suspension until well combined.

[0041] Step 2: Pour the alumina suspension prepared in Step 1 into the vibratory polishing disc. Place the prepared 3D-printed TC4 sample into the prepared vibratory polishing disc and load a 200g weight. The vibration frequency is 100-200Hz. Place a 400g sample and polish for 4.8 hours using the same parameters as in Example 1. Remove the sample and rinse with running water for 5 minutes, simultaneously rinsing the alumina suspension dilution in the polishing disc. Then, add ultrapure water, ensuring the water level in the polishing disc is 1-3mm higher than the sample height. Vibrate and polish again for 40 minutes. After vibratory polishing, remove the sample and rinse with running water for 2 minutes. Place it in a beaker, add anhydrous ethanol, and ultrasonically clean for 5 minutes. Remove and dry the sample. Gently pry it out of the embedded epoxy resin and perform EBSD analysis using SEM. The calibration rate is zero, the deformed layer was not removed, the polished surface was contaminated by the suspension, and no diffraction pattern was observed. See [see attached image]. Figure 3 .

[0042] Comparative Example 2: 3D printed TC4 titanium alloy sample The main difference compared to Example 1 is that it contains alumina abrasive particles.

[0043] I. Sample Preparation The sample is wire-cut into pieces with a length of 10-20 mm, a width of 10-20 mm, and a thickness of 2-3 mm. These pieces are then cold-mounted into Φ40×20 mm blocks (the size can be determined according to the abrasive tool used). The mounted samples are then polished with 400-grit and 1200-grit wet sandpaper until a smooth and fine surface is achieved. Polishing is then performed using 5μm, 1.5μm, and 0.5μm diamond sprays until a smooth and clean mirror surface is achieved.

[0044] Add 10 ml of hydrogen peroxide to 40 ml of alumina suspension, and perform fine mechanical polishing with running water on a clean, dedicated short-pile polishing cloth. During this stage, the polishing speed should be reduced to 300-400 r / min, and the polishing time should be greater than 5 min.

[0045] II. Vibratory Polishing Preparation of hydrogen peroxide aqueous solution Step 1: Mix 400ml of distilled water, 20ml of alumina suspension, and 100ml of 30% hydrogen peroxide (superior grade) until homogeneous.

[0046] Step 2: Pour the hydrogen peroxide-alumina solution prepared in Step 1 into the vibratory polishing disc (the amount added can be adjusted according to the size of the polishing disc, ensuring that the height of the hydrogen peroxide aqueous solution in the polishing disc is 1~3mm above the height of the embedded sample, so that the sample surface to be polished is completely immersed in the diluent and does not come into contact with air, thus achieving an oxygen-free environment).

[0047] The prepared 3DD-printed TC4 sample was placed in a prepared vibratory polishing disc and a 200g weight was added. The vibration frequency was 100-200Hz, and the same parameters as in Example 1 were used for polishing for 4.8 hours. After removing the sample, it was quickly rinsed with running water for 2 minutes, placed in a beaker with anhydrous ethanol, and ultrasonically cleaned for 10 minutes. After drying, the sample was removed from the mounting mold and subjected to EBSD detection and analysis using SEM. The calibration rate was 78.9%. The deformed layer was not completely removed, and the polished surface was contaminated by the suspension, resulting in an unclear distribution map. The results are shown in [see attached image]. Figure 4 .

[0048] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0049] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims.

Claims

1. A method for preparing 3D-printed titanium alloy EBSD samples, characterized in that, Includes the following steps: Sample pretreatment and mechanical polishing: The sample is cut to obtain the sample, and the test surface of the sample is ground and polished to make the test surface a mirror surface. The test surface is mechanically polished using a polishing agent; Interface conversion polishing: The mechanically polished sample is placed in an interface conversion polishing solution, with the liquid level higher than the detection surface of the sample to form a liquid phase isolation. Vibration polishing is then performed, followed by washing and drying to obtain a 3D printed titanium alloy EBSD sample. The interface conversion polishing solution is composed of water and hydrogen peroxide solution, with a volume ratio of water to hydrogen peroxide solution of 4:1 and a mass percentage concentration of 30% for the hydrogen peroxide solution.

2. The preparation method according to claim 1, characterized in that, In the interface conversion polishing step, the vibration frequency of the vibration polishing is 100-200Hz, and the vibration polishing time is calculated based on the interface conversion-thinning synergistic process model. The interface transformation-thinning synergistic process model is shown below: ; Wherein, t is the vibration polishing time; h0 is the maximum thickness of the residual deformation layer on the sample surface after mechanical polishing; C is the mass percentage concentration of the hydrogen peroxide solution; T is the ambient temperature during vibration polishing, ranging from 293K to 303K; e is the natural logarithm, with a value of 2.718; Eα is the apparent activation energy of the interfacial transformation reaction of titanium in the interfacial transformation polishing solution system, with a value of 2.5×10⁴ J / mol; R is the ideal gas constant, with a value of 8.314 J / (mol·K); K is the process correction coefficient, which is 2.0×10⁻³ when the vibration frequency of the vibration polishing is ≥150Hz, and 1.0×10⁻³ when the vibration frequency of the vibration polishing is <150Hz.

3. The preparation method according to claim 1, characterized in that, In the sample pretreatment and mechanical polishing steps, the grinding and polishing include: grinding the test surface to a smooth surface with wet sandpaper, and polishing the test surface with diamond spray.

4. The preparation method according to claim 3, characterized in that, The wet sandpaper has a mesh size including at least one of 400 mesh and 1200 mesh; The diamond spray has a particle size of at least one of 5μm, 1.5μm, and 0.5μm.

5. The preparation method according to claim 1, characterized in that, In the sample pretreatment and mechanical polishing steps, the polishing agent includes an alumina suspension and a hydrogen peroxide solution, with a volume ratio of 4:1 between the alumina suspension and the hydrogen peroxide solution.

6. The preparation method according to claim 1, characterized in that, In the sample pretreatment and mechanical polishing steps, the detection surface is mechanically polished until the oxide film attached to the detection surface is removed, and the polishing speed of the mechanical polishing is 300-400 r / min.

7. The preparation method according to claim 1, characterized in that, In the interface conversion polishing step, the liquid level is 1-3 mm higher than the detection surface of the sample; the load for the vibration polishing is 200 g.

8. A 3D printed titanium alloy EBSD sample obtained by the preparation method according to any one of claims 1-7.

9. A method for detecting and analyzing EBSD, characterized in that, The 3D printed titanium alloy EBSD sample obtained by any one of the preparation methods of claims 1-7 or the 3D printed titanium alloy EBSD sample of claim 8 was tested and analyzed.

10. The application of the preparation method according to any one of claims 1-7 or the 3D printed titanium alloy EBSD sample according to claim 8 in the EBSD detection and analysis method.

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