A method for preparing an ebsd sample of tantalum and tantalum alloy

Abstract

The application discloses a preparation method of tantalum and tantalum alloy EBSD samples, and belongs to the technical field of metal material metallographic analysis, and solves the problems of low efficiency and poor effect of the existing preparation method of tantalum and tantalum alloy EBSD samples. The method comprises the following steps: S1, processing tantalum and tantalum alloy EBSD samples; S2, adopting a method of combining mechanical polishing with manual polishing to polish the surfaces of the tantalum and tantalum alloy EBSD samples; S3, electrolytic polishing the samples after surface polishing; the electrolyte for electrolytic polishing is a mixed solution of sulfuric acid and methanol; and S4, cleaning the samples after electrolysis to obtain tantalum and tantalum alloy EBSD samples. The method can quickly prepare the tantalum and tantalum alloy EBSD samples with good quality.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of metal material organization texture characterization, and particularly relates to a preparation method of a tantalum and tantalum alloy EBSD sample. BACKGROUND

[0002] Tantalum and tantalum alloy are applied to electronic components, chemical industry, aerospace, etc. due to their good corrosion resistance, high temperature resistance, high ductility, high hardness and other characteristics. With the innovation and progress of research methods, and the continuous promotion of the research on the organization evolution of tantalum and tantalum alloy at high strain rate, the electron backscatter diffraction technology (EBSD) plays a more prominent role in the evolution of tantalum and tantalum alloy organization and texture. The traditional sample preparation method of the EBSD sample of tantalum and tantalum alloy has problems such as long cycle, poor effect, etc. in the grinding and polishing process, and it is difficult to prepare the sample and the efficiency is low.

[0003] Therefore, finding a fast, reliable, convenient and feasible preparation method of the EBSD sample of tantalum and tantalum alloy has great practical significance for improving the texture detection accuracy and efficiency of tantalum and tantalum alloy, and reducing the anisotropy characterization difficulty of tantalum and tantalum alloy material. SUMMARY

[0004] In view of the above analysis, the present application aims to provide a preparation method of a tantalum and tantalum alloy EBSD sample, which can solve the problems of low efficiency and poor effect of the existing preparation method of the tantalum and tantalum alloy EBSD sample.

[0005] The purpose of the present application is mainly realized by the following technical solutions:

[0006] The present application provides a preparation method of a tantalum and tantalum alloy EBSD sample, which comprises the following steps:

[0007] S1, processing a tantalum and tantalum alloy EBSD sample;

[0008] S2, using a method combining mechanical polishing and manual polishing to polish the surface of the tantalum and tantalum alloy EBSD sample;

[0009] S3, electrolytic polishing the sample after surface polishing; the electrolyte for electrolytic polishing is a mixed solution of sulfuric acid and methanol;

[0010] S4, cleaning the sample after electrolysis to obtain a tantalum and tantalum alloy EBSD sample.

[0011] Further, in S3, the volume ratio of each component in the mixed solution is 0.5-2:7 of sulfuric acid to methanol.

[0012] Further, in S3, during the electrolytic polishing process, the electrolytic voltage is 14-20 V, the electrolytic time is 15-45 s, and the current control is 0.8-1.3 A.

[0013] Further, in S1, the sample is a square sample, and the surface size of the sample is 5-10mm in length of one side.

[0014] Further, in S1, the sample is a cylindrical sample, and the diameter of the sample is not greater than 10mm.

[0015] Further, in S2, the mechanical polishing is processed by using a full-automatic polishing and grinding integrated machine.

[0016] Further, in S2, after the mechanical polishing, the sample is manually polished by using 3000-mesh sandpaper.

[0017] Further, in S4, after the electrolytic polishing is completed, the sample is quickly placed in alcohol to stabilize the surface oxidation, and the ultrasonic cleaning is used to remove the residual stains on the surface of the sample.

[0018] Further, in S4, after the cleaning, the sample surface is quickly dried by using a hair dryer, and after the drying, the anti-oxidation adhesive tape is used to protect the detection surface.

[0019] Further, in S3, the sulfuric acid is 93%-98.3% sulfuric acid in mass concentration.

[0020] Compared with the prior art, the present application can at least achieve one of the following beneficial effects:

[0021] 1) The preparation method of the tantalum and tantalum alloy EBSD sample of the present application adopts the method of mechanical polishing and manual polishing to polish the surface of the tantalum and tantalum alloy EBSD sample, and then adopts electrolytic polishing, so that the sample preparation period is short (for example, the sample preparation period is not greater than 5min), and the sample preparation efficiency and sample quality are significantly improved.

[0022] 2) The preparation method of the tantalum and tantalum alloy EBSD sample provided by the present application can quickly prepare the tantalum and tantalum alloy EBSD sample, improve the operability, obtain the EBSD sample with good quality and clear grain boundary profile, and has high one-time detection rate, high calibration rate, reliable orientation characterization result, and clear performance of part of the fine structure and characteristics, which has good effect on improving the EBSD detection efficiency, quality and reducing the cost of tantalum and tantalum alloy.

[0023] 3) The electrolyte of the present application adopts a mixed solution of sulfuric acid and methanol, does not need to use toxic substances, is harmless to human body, is environment-friendly, and ensures the personal safety of the operator.

[0024] Other features and advantages of the present application will be set forth in the following description of the application, and in part will become apparent to those skilled in the art from the description, or can be learned by practice of the application. The objects and other advantages of the present application can be achieved and obtained by specifically pointing out in the written description and the accompanying drawings of the specification. Attached Figure Description

[0025] The accompanying drawings are for illustrative purposes only and are not intended to limit the invention. Throughout the drawings, the same reference numerals denote the same parts.

[0026] Figure 1 The results are for the detection of the EBSD sample prepared in Example 1 of the present invention. Detailed Implementation

[0027] The preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings, which form part of the present invention and, together with the embodiments of the present invention, serve to illustrate the principles of the present invention.

[0028] Currently, traditional methods for preparing EBSD samples of tantalum and tantalum alloys suffer from problems such as long processing times and poor results during the polishing process, making sample preparation difficult and inefficient. Some methods employ electrolytic polishing, but the electrolytes used are often hydrofluoric acid, which is toxic and easily pollutes the environment. Therefore, finding a rapid, reliable, convenient, and feasible method for preparing EBSD samples of tantalum and tantalum alloys is of great practical significance for improving the accuracy and efficiency of texture detection of tantalum and tantalum alloys and reducing the difficulty of anisotropic characterization of tantalum and tantalum alloy materials.

[0029] This invention provides a method for preparing tantalum and tantalum alloy EBSD samples, comprising the following steps:

[0030] S1. Processing EBSD samples of tantalum and tantalum alloys;

[0031] S2. The EBSD samples of tantalum and tantalum alloys were polished by a combination of mechanical polishing and manual polishing.

[0032] S3. Electropolishing is performed on the sample after surface grinding; the electrolyte for electropolishing is a mixed solution of sulfuric acid and methanol;

[0033] S4. Clean the electrolyzed sample to obtain tantalum and tantalum alloy EBSD samples.

[0034] Compared with the prior art, the method for preparing tantalum and tantalum alloy EBSD samples of the present invention uses a combination of mechanical polishing and manual polishing to polish the surface of tantalum and tantalum alloy EBSD samples, followed by electrolytic polishing. This method has a short sample preparation cycle and significantly improves sample preparation efficiency and sample quality.

[0035] Specifically, in S3 above, the sulfuric acid used is sulfuric acid with a mass concentration of 93% to 98.3%.

[0036] Specifically, in the above S3, considering that the concentration of sulfuric acid is too large, the electrolysis rate is fast, and the electrolysis surface is easy to be uneven, and the concentration of sulfuric acid is low, the electrolysis rate is slow, and the electrolysis time is too long; therefore, the volume ratio of each component in the mixed solution of sulfuric acid and methanol is controlled as follows: sulfuric acid: methanol is 0.5-2:7; for example, 0.5:7, 1:7, 1.5:7, 2:7.

[0037] Specifically, in the above S3, the electrolytic polishing process is a process of immersing the sample electrolysis surface in the electrolyte under the action of an external electric field, the anode metal atoms lose electrons to form ions and separate from the metal surface, and the fresh surface is exposed. In order to achieve better electrolysis effect, the electrolyte, electrolysis voltage and current density need to be controlled, and the selection of related parameters is unreasonable, which will lead to the problems of difficult electrolysis, uneven surface, slow electrolysis rate, surface oxidation and the like. After in-depth research by the inventors, the electrolysis voltage is controlled to be 14-20V, the electrolysis time is controlled to be 15-45s, and the current is controlled to be 0.8-1.3A. After electrolytic polishing, clear organization can be seen by using the above process.

[0038] Specifically, in the above S3, in order to weaken the electrolysis process and prevent the electrolysis surface from ion aggregation, leading to uneven electrolysis or even surface oxidation, ultrasonic is used as an electrolyte diffusion promoting means for the electrolysis process. Considering that the ultrasonic frequency is too low, the forced diffusion ion ability is weak, and too high, the equipment implementation is difficult, and the equipment use cost is high; therefore, the ultrasonic frequency is controlled to be 15-30kHz.

[0039] Specifically, in the above S1, in order to ensure that the detection surface has good detection quality, the sample size needs to be controlled, and appropriate processing method is selected according to the shape and characteristics of the sample. Machining center and wire cutting are often used to process the sample to appropriate size; if the sample size is too small, the edge arc phenomenon is obvious during the sample preparation process, especially the electrolysis process, which leads to deviation between the detection result and the actual result; if the sample size is too large, the surface quality is uneven, which affects the overall preparation result. Therefore, for square samples, the recommended value of the surface size single side length is 5-10mm, and for cylindrical samples, the recommended value of the sample diameter is not more than 10mm, for example, the sample diameter is 5-10mm, and the sample height is 10-15mm.

[0040] Specifically, in the above S1, during the processing of the sample, the influence on the sample organization (such as overheating) should be avoided when the sample is cut, and preventive measures (such as water cooling) can be taken during processing, or the influence can be removed after processing.

[0041] Specifically, in the above S2, the main role of surface polishing is to remove the machining marks on the surface of the sample, which mainly includes machining surface tool marks and wire cutting surface oxidation. In order to improve the sample preparation efficiency, in the above S2, a method combining mechanical polishing and manual polishing is used. The mechanical polishing mainly removes the machining marks of the sample, and the manual polishing refines the surface scratches and removes the oxidation layer generated in the mechanical polishing process. In the mechanical polishing process, due to the high overall hardness of the sample, the effect of single sandpaper polishing is poor. In order to improve the polishing efficiency and quality, a full-automatic polishing machine is used to cooperate with 600-mesh sandpaper and high-hardness medium such as diamond spray or diamond grinding paste for mechanical polishing treatment. The sample is continuously cooled by cooling water during the polishing process. After mechanical polishing, the sample is polished by hand using 3000-mesh sandpaper to refine the scratches and remove the surface oxidation. It should be noted that the mechanical polishing process is fast and generates a lot of heat, which is easy to cause oxidation. Therefore, 3000-mesh sandpaper is used for manual polishing to remove the surface oxidation layer.

[0042] Specifically, in the above S2, if the speed of the full-automatic polishing machine is too large, it is not easy to ensure the flatness of the polished surface, and multi-surface problems are easy to occur. If the speed is too small, the grinding efficiency is low and the polished surface roughness is large. Therefore, the speed of the full-automatic polishing machine is controlled to be 200-600 r.

[0043] Specifically, in the above S4, the exposed surface of the sample after electrolysis is easy to oxidize in the air, and the residual electrolyte is easy to contaminate the sample surface. At the same time, the sample surface needs to be protected after sample preparation and before sample detection, and the sample storage environment needs to be controlled. Therefore, after completing the electrolytic polishing, the sample needs to be quickly placed in alcohol to stabilize the surface oxidation, and ultrasonic cleaning is used to remove the residual stains on the sample surface. During sample storage, anti-oxidation tape can be used to protect the detection surface, and the sample can be placed in a sample box with a desiccant for protection.

[0044] Specifically, in the above S4, the sample is placed in alcohol with the electrolysis surface standing on one side to prevent the electrolysis surface from directly contacting the bottom of the beaker or the electrolysis surface from being upward, which avoids the electrolysis surface from being polished or not being cleaned.

[0045] Specifically, in the above S4, the cleaning time is 30-120 s; after cleaning, the sample surface is quickly dried using a hair dryer, and then the detection surface is protected using anti-oxidation tape and waiting for detection.

[0046] Specifically, the above method for preparing a tantalum and tantalum alloy EBSD sample can complete the high-quality preparation of a single sample within 5 minutes (for example, 200-270 s).

[0047] Compared with the prior art, the preparation method of the tantalum and tantalum alloy EBSD sample provided by the present application can quickly prepare the tantalum and tantalum alloy EBSD sample, improve the ease of operation, and obtain the EBSD sample with good quality, clear grain boundary profile, high one-time detection rate, high calibration rate, reliable orientation characterization result, and clear expression of part of the fine microstructure and characteristics, thereby improving the EBSD detection efficiency, quality and reducing the cost of the tantalum and tantalum alloy.

[0048] The electrolyte of the present application adopts a mixed solution of sulfuric acid and methanol, does not need to use toxic substances, is harmless to the human body, is environmentally friendly, and ensures the personal safety of the operator.

[0049] Embodiment 1

[0050] The present embodiment provides a preparation method of a tantalum alloy EBSD sample, the tantalum alloy is FTa1 tantalum alloy, and the method comprises the following steps:

[0051] S1, processing a tantalum alloy EBSD sample;

[0052] S2, using a method combining mechanical polishing and manual polishing to polish the surface of the tantalum and tantalum alloy EBSD sample;

[0053] S3, electrolytic polishing the sample after surface polishing; the electrolyte for electrolytic polishing is a mixed solution of sulfuric acid and methanol; the sulfuric acid has a mass concentration of 95%; the volume ratio of each component in the mixed solution is: sulfuric acid:methanol is 1:7;

[0054] S4, cleaning the sample after electrolysis to obtain a tantalum and tantalum alloy EBSD sample.

[0055] Specifically, in the above S1, the sample size is processed to 6mm*7mm*8mm (length* width*height) by using a wire cutting method, the surface roughness of the processed sample is not higher than 0.8, the surface is free of excess burrs and burrs, and the roughness is uniform, and the 6mm*7mm surface is determined as the detection surface.

[0056] Specifically, in the above S2, 600-mesh sandpaper is installed on the polishing disc of the full-automatic grinding and polishing integrated machine, the surface of the sandpaper is completely immersed with tap water, a layer of diamond spray is uniformly sprayed on the sandpaper, the rotating speed of the full-automatic grinding and polishing integrated machine is set to 300r, the cooling water is turned on, the surface to be polished is attached to the surface of the sandpaper, and the surface is uniformly moved until the surface processing marks are removed and the grinding marks are uniform, and then the mechanical polishing is stopped. The sample surface is blown dry, 3000-mesh sandpaper is used, manual polishing is performed along the direction perpendicular to the grinding marks of the 600-mesh sandpaper, and when the grinding marks of the 3000-mesh sandpaper completely cover the original marks, the surface polishing is completed.

[0057] Specifically, in the above S3, 100 mL of electrolyte is configured, after the electrolyte is completely cooled, it is put into an electrolytic cell, a tantalum alloy sample is fixed on an electrolytic anode, a 1mm thick 304 stainless steel sheet is fixed on an electrolytic cathode, the surface of the sample is parallel to the surface of the cathode, a direct current power supply is used to form an electric field environment, the electrolysis voltage is controlled to be 16V, the current is controlled to be 0.8-1A, and the electrolysis time is 40s. After 40s, the sample is immediately taken out.

[0058] Specifically, in the above S3, ultrasonic is used as an electrolyte diffusion promoting means for the electrolysis process, and the ultrasonic frequency is controlled to be 20kHz.

[0059] Specifically, in the above S4, after the electrolytic polishing is completed, the sample is quickly put into alcohol to stabilize the surface oxidation, the sample is placed vertically on the electrolytic surface side when it is put into alcohol, and the ultrasonic cleaning is used to remove the residual stains on the surface of the sample, the cleaning time is 60s. After cleaning, the sample surface is quickly dried by using a hair dryer, and the sample surface is protected by using an anti-oxidation tape after drying, and then detection is waited.

[0060] Specifically, the preparation method of the tantalum alloy EBSD sample is used to complete the high-quality preparation of a single block sample in 270s.

[0061] Figure 1 The detection result of the EBSD sample of the embodiment is detected by using a TESCAN VGA3 tungsten filament scanning electron microscope, the magnification is 100 times, the step is 5μm, the detection area is 1200μm×1200μm, and the detection CI value is 0.80. It can be seen that the grain boundary profile is clear, the calibration rate is high, and the detection result is reliable.

[0062] Embodiment 2

[0063] The embodiment provides a preparation method of a tantalum alloy EBSD sample, the tantalum alloy is Ta2 tantalum alloy, the preparation method is basically the same as that in the above embodiment 1, and the difference lies in that:

[0064] In the above S1, the sample is a cylindrical sample, the sample diameter is 7mm, and the sample height is 10mm.

[0065] In the above S2, the rotation speed of the automatic grinding and polishing machine is set to 350r.

[0066] In the above S3, the electrolysis voltage is controlled to be 18V, the current is controlled to be 0.8-1A, and the electrolysis time is 30s.

[0067] Specifically, the preparation method of the tantalum alloy EBSD sample is used to complete the high-quality preparation of a single block sample in 260s.

[0068] The EBSD sample of the embodiment is detected by using a TESCAN VGA3 tungsten filament scanning electron microscope, and the sample orientation characterization is accurate, the grain boundary profile is clear, and the sample can be used for analysis of the crystal orientation of the Ta2 tantalum alloy.

[0069] The inventors made a large number of schemes during the research process, and some of the schemes with poor effects are taken as comparative examples for comparison.

[0070] Comparative Example 1

[0071] The present comparative example provides a preparation method of a tantalum alloy EBSD sample, the type of the tantalum alloy is the same as that in Example 1, and the preparation method is substantially the same as that in Example 1, and the difference lies in that:

[0072] In S3, the volume ratio of each component in the electrolyte is: sulfuric acid:methanol is 2:7; the electrolysis voltage is controlled to be 16V, the current is controlled to be 0.8-1A, and the electrolysis time is 40s; in S3, the mechanical polishing is not followed by manual polishing with 3000-mesh sandpaper.

[0073] The EBSD sample prepared in the present comparative example is observed under a microscope, and the sample surface is unevenly electrolyzed, sharp protrusions appear in local areas, and a small amount of areas have visible metallographic structures under the microscope. The electrolytic sample cannot meet the basic requirements of EBSD detection.

[0074] Comparative Example 2

[0075] The present comparative example provides a preparation method of a tantalum alloy EBSD sample, the type of the tantalum alloy is the same as that in Example 1, and the preparation method is substantially the same as that in Example 1, and the difference lies in that:

[0076] In S3, the volume ratio of each component in the electrolyte is: sulfuric acid:methanol is 1:7; the electrolysis voltage is controlled to be 25V, the current is controlled to be 0.9-1A, and the electrolysis time is 40s; in S3, the electrolysis voltage fails to meet the parameter requirements.

[0077] The EBSD sample prepared in the present comparative example is observed under a microscope, and the sample surface is bright, the grain boundary is clear, but the fluctuation is obvious and the surface is not flat, which is not conducive to obtaining accurate and reliable data.

[0078] Comparative Example 3

[0079] The present comparative example provides a preparation method of a tantalum alloy EBSD sample, the type of the tantalum alloy is the same as that in Example 1, and the preparation method is substantially the same as that in Example 1, and the difference lies in that:

[0080] In S3, the volume ratio of each component in the electrolyte is: sulfuric acid:methanol is 1:7; the electrolysis voltage is controlled to be 15V, the current is controlled to be 0.8-1A, and the electrolysis time is 10s; in S3, the electrolysis time fails to meet the parameter requirements.

[0081] The EBSD sample prepared by the present comparative example is bright at the edge of the sample surface under a light microscope, the grain boundary is clear, the center is dark and there are polishing marks, and the center region cannot complete EBSD detection data collection.

[0082] It is found by the comparative examples and the present comparative example that the preparation method of the tantalum and tantalum alloy EBSD sample of the present application can quickly prepare the tantalum and tantalum alloy EBSD sample, improve the ease of operation, obtain the EBSD sample with good quality, clear grain boundary profile, high one-time detection rate, high calibration rate, reliable orientation characterization result, and clearly show part of the fine structure and characteristics, and has a good effect on the EBSD detection efficiency, quality improvement, and cost reduction of the tantalum and tantalum alloy.

[0083] The above is only a preferred specific embodiment of the present application, but the protection scope of the present application is not limited thereto, any person skilled in the art can easily think of changes or replacements within the technical range disclosed by the present application, which should be covered within the protection scope of the present application.

Claims

1. A method of preparing a tantalum alloy EBSD sample, characterized by, The preparation method comprises the following steps: S1, processing a tantalum alloy EBSD sample; S2, surface polishing of the tantalum alloy EBSD sample by a method combining mechanical polishing and manual polishing; S3, electrolytic polishing of the sample after surface polishing; the electrolyte for electrolytic polishing is a mixed solution of sulfuric acid and methanol; S4, cleaning of the sample after electrolysis to obtain a tantalum alloy EBSD sample; In S3, the volume ratio of each component in the mixed solution is: sulfuric acid:methanol is 1:7; In S3, during the electrolytic polishing process, the electrolytic voltage is 16V, the electrolytic time is 40s, and the current control is 0.8~1A; In S1, the sample is a square sample, and the surface size of the sample is 5~10mm in length on one side; or the sample is a cylindrical sample, the sample diameter is 5~10mm, and the sample height is 10~15mm; In S2, mechanical polishing is carried out by using a full-automatic polishing and grinding integrated machine, 600-mesh sandpaper and diamond spraying or diamond grinding paste; the rotating speed of the full-automatic polishing and grinding integrated machine is controlled to be 200~600r; In S3, ultrasonic is used as an electrolyte diffusion promoting means for the electrolysis process, and the ultrasonic frequency is controlled to be 20kHz; In S4, in S4, the electrolysis surface is placed vertically when the sample is placed in alcohol, and the cleaning time is 30~120s; The preparation method of the tantalum alloy EBSD sample can complete the high-quality preparation of a single sample within 5min, and clear organization can be seen after electrolytic polishing.

2. The production method according to claim 1, characterized by, In S2, after mechanical polishing, the sample is manually polished using 3000-mesh sandpaper.

3. The preparation method according to claim 1, characterized in that, In S4, after completing electrolytic polishing, the sample is quickly placed in alcohol to stabilize the surface oxidation, and ultrasonic cleaning is used to remove residual stains on the surface of the sample.

4. The production method according to claim 3, characterized by, In S4, after cleaning, the sample surface is quickly blown dry using a hair dryer, and after drying, an anti-oxidation adhesive tape is used to protect the detection surface.

5. The production method according to any one of claims 1 to 4, characterized by, In S3, the sulfuric acid has a mass concentration of 93%~98.3%.

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