Sample preparation method of aluminum target EBSD sample
EBSD samples of aluminum targets were prepared by wire cutting, mounting, mechanical grinding, polishing and chemical etching, which solved the problems of long preparation time and low calibration rate, and achieved rapid and efficient sample preparation and high calibration rate.
Patent Information
- Application Number
- CN202511304034.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-12
- Publication Date
- 2025-12-05
AI Technical Summary
Existing methods for preparing EBSD samples from aluminum targets are time-consuming and cumbersome, making it difficult to meet the demand for rapid, large-scale sample preparation, and the calibration rate is not high.
After wire cutting, the samples were mounted, mechanically ground and polished, then chemically etched using a chemical etching solution composed of hydrofluoric acid, phosphoric acid and water. Finally, the samples were washed and dried to obtain EBSD samples with high calibration rates.
It enables rapid preparation of EBSD samples with high calibration rates, is simple to operate, suitable for mass production, and achieves a calibration rate of over 95%, reducing the requirements for personnel and equipment.
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Figure CN121068655A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of magnetron sputtering, and particularly relates to a sample preparation method of an aluminum target EBSD sample. BACKGROUND
[0002] Magnetron sputtering technology is a core process for preparing thin film materials. Through plasma bombardment of the target surface, atoms are sputtered and deposited to form a film, which can be applied in the fields of semiconductors, display panels and photovoltaic cells. Aluminum target is widely used in the fields of electronics, optics and aerospace due to its excellent electrical conductivity, low resistivity, high reflectivity, thermal conductivity and corrosion resistance. Key indicators of target performance include purity, density, chemical composition uniformity, crystal structure, size and shape accuracy, thermal stability and corrosion resistance. Among them, the crystal structure of the target affects the sputtering rate of the target and the performance of the thin film. Electron backscattered diffraction (EBSD) is a technology for detecting the crystal structure and orientation of the target, which can measure the phase, grain size, grain orientation, orientation difference and orientation distribution function of the crystal. The reliability of the EBSD analysis result is related to the quality of the sample preparation.
[0003] Currently, the EBSD sample of aluminum or aluminum alloy is prepared by mechanical polishing + vibration polishing or mechanical polishing + electrolytic polishing. For example, a related technology discloses a preparation method of an aluminum alloy free machining state EBSD sample, which comprises the following steps: (1) sawing the sample using a grinding wheel saw; (2) mechanically grinding and polishing the cut sample using an automatic grinding and polishing machine; (3) electrolytically polishing the sample using 6% to 12% high-chloric acid alcohol; and (4) finally cleaning the sample using alcohol ultrasonic cleaning. By controlling multiple parameters such as the composition of the electrolytic etching solution, voltage, current and temperature, the polishing requirements of the sample surface are achieved. However, vibration polishing takes a long time, usually several hours, which is not suitable for rapid and large-scale sample preparation. Electrolytic polishing needs to find and optimize the electrolyte formula and parameters for specific materials, which is complicated to operate. Therefore, there is an urgent need to develop a sample preparation method for aluminum target EBSD sample, which is simple to operate, has a high calibration rate and can quickly prepare the sample. SUMMARY
[0004] Therefore, the purpose of the present application is to provide a sample preparation method of an aluminum target EBSD sample. The sample preparation method provided by the present application is simple to operate, can quickly prepare an EBSD sample, and has a high calibration rate.
[0005] The present application provides a sample preparation method of an aluminum target EBSD sample, which comprises the following steps:
[0006] The aluminum target is line-cut to obtain an aluminum target block;
[0007] After the sample is inlaid, the aluminum target block is subjected to mechanical grinding and polishing in sequence to obtain a ground and polished aluminum target block;
[0008] The ground and polished aluminum target block is subjected to chemical etching, washing and drying to obtain an EBSD sample to be detected.
[0009] Preferably, the volume ratio of the hydrofluoric acid, the phosphoric acid and the water is (0.5-1.5):(10-15):(44-59), the concentration of the hydrofluoric acid is 40wt%, and the concentration of the phosphoric acid is 85wt%.
[0010] Preferably, the volume ratio of the hydrofluoric acid, the phosphoric acid and the water is 1:(10-15):(44-49).
[0011] Preferably, the time of the chemical etching is 1-3min.
[0012] Preferably, the length of the aluminum target block is 10-20mm, the width is 10-20mm, and the height is 8-10mm.
[0013] Preferably, the temperature of the inlaying is 120-150℃, and the holding time is 5-15min.
[0014] Preferably, the mechanical grinding comprises first grinding and second grinding in sequence, the first grinding adopts sandpaper of 400-800#, and the second grinding adopts sandpaper of 1000-1400#.
[0015] Preferably, the time of the first grinding and the second grinding is independently 3-5min.
[0016] Preferably, the polishing comprises first polishing, second polishing and third polishing in sequence, the first polishing and the second polishing use diamond polishing liquid, and the third polishing uses alumina polishing liquid.
[0017] Preferably, the average particle size of the diamond in the diamond polishing liquid used for the first polishing is 8.8-9.2μm, and the time of the first polishing is 5-8min; the average particle size of the diamond in the diamond polishing liquid used for the second polishing is 2.9-3.1μm, and the time of the second polishing is 3-8min; the average particle size of the alumina in the alumina polishing liquid is 0.04-0.06μm, and the time of the third polishing is 5-8min.
[0018] Compared with the prior art, the present application has the following beneficial effects:
[0019] The application provides a sample preparation method of an aluminum target EBSD sample, comprising the following steps: linear cutting of an aluminum target to obtain an aluminum target block; after sample mounting of the aluminum target block, sequentially performing mechanical grinding and polishing to obtain a ground and polished aluminum target block; performing chemical etching, washing and drying on the ground and polished aluminum target block to obtain an EBSD sample to be detected; and the chemical etching liquid used in the chemical etching is composed of hydrofluoric acid, phosphoric acid and water.
[0020] After mechanical grinding and polishing of the aluminum target block, the polished surface of the aluminum target block is subjected to chemical etching treatment, the chemical etching liquid is composed of hydrofluoric acid, phosphoric acid and water, the hydrofluoric acid can dissolve aluminum oxide on the surface of the aluminum, the phosphoric acid can react with the aluminum and has weak oxidizing property, slightly passivates and reduces pitting, can quickly react and can also obtain a smooth surface and a proper resolution rate. The sample preparation method can obtain an EBSD sample with a calibration rate of more than 95%. The sample preparation method is simple to operate, can react at room temperature, does not need complex equipment, has low requirements on personnel, can quickly and massively prepare EBSD samples, and has a high calibration rate. BRIEF DESCRIPTION OF DRAWINGS
[0021] In order to more clearly illustrate the technical solutions in the embodiments of the application or the prior art, the following will briefly introduce the drawings needed in the embodiments. Obviously, the drawings in the following description are only some embodiments of the application, and other drawings can also be obtained by those skilled in the art without creative effort.
[0022] Figure 1 The test result graph of the aluminum target EBSD sample prepared for Example 1 is shown in the figure;
[0023] Figure 2 The test result graph of the aluminum target EBSD sample prepared for Example 2 is shown in the figure;
[0024] Figure 3 The test result graph of the aluminum target EBSD sample prepared for Example 3 is shown in the figure;
[0025] Figure 4 The test result graph of the aluminum target EBSD sample prepared for Comparative Example 1 is shown in the figure;
[0026] Figure 5 The test result graph of the aluminum target EBSD sample prepared for Comparative Example 2 is shown in the figure;
[0027] Figure 6 The test result graph of the aluminum target EBSD sample prepared for Comparative Example 3 is shown in the figure;
[0028] Figure 7 The test result graph of the aluminum target EBSD sample prepared for Comparative Example 4 is shown in the figure. DETAILED DESCRIPTION
[0029] The application provides a sample preparation method of an aluminum target EBSD sample, comprising the following steps:
[0030] The aluminum target is linearly cut to obtain an aluminum target block;
[0031] After the aluminum target block is inlaid, mechanical grinding and polishing are sequentially performed to obtain a ground and polished aluminum target block;
[0032] The ground and polished aluminum target block is subjected to chemical corrosion, washing and drying to obtain an EBSD sample to be detected; the chemical corrosion liquid used in the chemical corrosion is composed of hydrofluoric acid, phosphoric acid and water.
[0033] In the application, the materials and equipment used are commercially available goods in the field unless otherwise specified.
[0034] The aluminum target is linearly cut to obtain an aluminum target block.
[0035] In the application, the aluminum target has a mass content of aluminum of preferably >99%, and specifically can be 99.5% or 100%.
[0036] In the application, the aluminum target block has a length of preferably 10-20 mm, a width of preferably 10-20 mm, and a height of preferably 8-10 mm, and specifically can be an aluminum target block with a length of 20 mm, a width of 10 mm and a height of 8 mm, or an aluminum target block with a length of 18 mm, a width of 12 mm and a height of 9 mm, or an aluminum target block with a length of 20 mm, a width of 15 mm and a height of 8 mm; the aluminum target block is suitable for EBSD characterization.
[0037] After the aluminum target block is obtained, the aluminum target block is inlaid, and then mechanical grinding and polishing are sequentially performed to obtain a ground and polished aluminum target block.
[0038] In the application, the temperature of the inlaying is preferably 120-150 DEG C, and the holding time is preferably 5-15 min, and specifically can be 8 min or 10 min. The inlaying is preferably performed in a metallographic inlaying machine, and after the sample is placed in the metallographic inlaying machine, metallographic inlaying powder is added.
[0039] In the application, the mechanical grinding preferably comprises sequentially performing first grinding and second grinding, the first grinding preferably uses sandpaper with a grit of 400-800, and specifically can be 600# or 800#, and the grinding time is preferably 3-5 min, and specifically can be 3 min, 4 min or 5 min; the second grinding uses sandpaper with a grit of 1000-1400, and specifically can be 1000# or 1200#, and the grinding time is preferably 3-5 min, and specifically can be 3 min, 4 min or 5 min.
[0040] In the present application, the polishing comprises sequentially performing first polishing, second polishing and third polishing, the polishing liquid of the first polishing is preferably diamond polishing liquid, the average particle size of diamond in the diamond polishing liquid is preferably 8.8-9.2 μm, and specifically can be 9 μm, and the polishing time is preferably 5-8 min, and specifically can be 5 min, 6 min or 8 min; the polishing liquid of the second polishing is preferably diamond polishing liquid, the average particle size of diamond in the diamond polishing liquid is preferably 2.9-3.1 μm, and specifically can be 3 μm, and the polishing time is preferably 3-8 min, and specifically can be 3 min, 5 min, 6 min or 8 min; the polishing liquid of the third polishing is preferably alumina polishing liquid, the average particle size of alumina in the alumina polishing liquid is preferably 0.04-0.06 μm, and specifically can be 0.05 μm, and the polishing time is preferably 5-8 min, and specifically can be 5 min, 6 min or 8 min.
[0041] After obtaining the polished aluminum target block, the polished aluminum target block is subjected to chemical etching, washing and drying to obtain an EBSD sample to be detected.
[0042] In the present application, the water is preferably deionized water.
[0043] In the present application, the concentration of the hydrofluoric acid is preferably 40 wt%, and the concentration of the phosphoric acid is preferably 85 wt%; the volume ratio of the hydrofluoric acid, the phosphoric acid and the water is preferably (0.5-1.5):(10-15):(44-59), and more preferably 1:(10-15):(44-49), and specifically can be 1:10:49, 1:12:47 or 1:15:44. The chemical etching liquid in the present application has a smooth etched surface, and suitable analysis rate and large-angle grain boundary value.
[0044] In the present application, the time of the chemical etching is preferably 1-3 min, and specifically can be 60 s, 100 s or 160 s. During the chemical etching, the acid reacts with the metal surface, the grain boundary is etched out, the reaction of the phosphoric acid and the aluminum generates aluminum phosphate which is a thin film insoluble in water, and the hydrofluoric acid reacts with the aluminum oxide and the aluminum phosphate; compared with the single hydrofluoric acid, the addition of the phosphoric acid makes the etching reaction more moderate and uniform.
[0045] In the present application, the washing is preferably water flushing.
[0046] In the present application, the drying is preferably room temperature blowing, and specifically can be cold air blowing or compressed air blowing using a hair dryer.
[0047] The application provides a sample preparation method of an aluminum target EBSD sample, which comprises the following steps: sequentially subjecting an aluminum target block to mechanical grinding and polishing, and then performing chemical etching on the aluminum target block by using an etching solution composed of hydrofluoric acid, phosphoric acid and deionized water, and then performing washing and drying to obtain an EBSD sample to be detected.
[0048] In order to further illustrate the application, the sample preparation method of the aluminum target EBSD sample provided by the application is described in detail below in combination with the drawings and examples, but they should not be understood as limiting the protection scope of the application.
[0049] In the examples or comparative examples of the application, the hydrofluoric acid used is commercially available hydrofluoric acid with a concentration of 40 wt%, the phosphoric acid used is commercially available phosphoric acid with a concentration of 85 wt%, and the aluminum content in the aluminum target is 99.5%.
[0050] Example 1
[0051] The sample preparation method of the aluminum target EBSD sample comprises the following steps:
[0052] (1) An aluminum target with an aluminum content of more than 99% is cut by wire cutting to obtain an aluminum target block with a length of 20 mm, a width of 10 mm and a height of 8 mm.
[0053] (2) The aluminum target block obtained in step (1) is subjected to sample mounting at a temperature of 120 DEG C for 10 min, and then is subjected to mechanical grinding and polishing to obtain a ground and polished aluminum target block.
[0054] The mechanical grinding comprises first rough grinding by using 600# sandpaper and second rough grinding by using 1000# sandpaper, and the time is 5 min respectively.
[0055] The polishing comprises sequentially polishing for 5 min by using diamond polishing liquid with an average particle size of 9 μm, polishing for 5 min by using diamond polishing liquid with an average particle size of 3 μm and polishing for 5 min by using alumina polishing liquid with an average particle size of 0.05 μm.
[0056] (3) The ground and polished aluminum target block obtained in step (2) is subjected to chemical etching for 160 s, water washing and cold air blowing to obtain a sample to be detected (i.e. an aluminum target EBSD sample); the chemical etching uses a mixed solution of hydrofluoric acid, phosphoric acid and deionized water with a volume ratio of 1:10:49.
[0057] The aluminum target EBSD sample is subjected to analysis and testing, and the test result shows that the calibration rate of the aluminum target EBSD sample is 99.2%. Figure 1 The test result graph of the aluminum target EBSD sample prepared in Example 1.
[0058] Example 2
[0059] The sample preparation method of the aluminum target EBSD sample includes the following steps:
[0060] (1) The aluminum target with aluminum content >99% is wire cut to obtain an aluminum target block with a length of 18 mm, a width of 12 mm, and a height of 9 mm.
[0061] (2) The aluminum target block obtained in step (1) is inlaid at a temperature of 120°C for 8 min, and then is mechanically ground and polished to obtain a ground and polished aluminum target block.
[0062] The mechanical grinding includes first rough grinding with 800# sandpaper and second rough grinding with 1200# sandpaper, and the time is 3 min and 4 min, respectively;
[0063] The polishing includes polishing with diamond polishing liquid with an average particle size of 9 μm for 6 min, polishing with diamond polishing liquid with an average particle size of 3 μm for 6 min, and polishing with alumina polishing liquid with an average particle size of 0.05 μm for 6 min.
[0064] (3) The ground and polished aluminum target block obtained in step (2) is chemically etched for 100 s, washed with water, and dried with cold air to obtain a sample to be detected; the chemical etching liquid used is a mixed solution of hydrofluoric acid, phosphoric acid, and deionized water with a volume ratio of 1:12:47.
[0065] The aluminum target EBSD sample is analyzed and tested, and the test result shows that the calibration rate of the aluminum target EBSD sample is 99.5%. Figure 2 The test result graph of the aluminum target EBSD sample prepared in Example 2.
[0066] Example 3
[0067] The sample preparation method of the aluminum target EBSD sample includes the following steps:
[0068] (1) The aluminum target with aluminum content >99% is wire cut to obtain an aluminum target block with a length of 20 mm, a width of 15 mm, and a height of 8 mm.
[0069] (2) The aluminum target block obtained in step (1) is inlaid at a temperature of 120°C for 10 min, and then is mechanically ground and polished to obtain a ground and polished aluminum target block.
[0070] The mechanical grinding includes first rough grinding with 600# sandpaper and second rough grinding with 1200# sandpaper, and the time is 4 min and 4 min, respectively;
[0071] The polishing comprises polishing for 8 min using diamond polishing liquid with an average particle size of 9 μm, polishing for 8 min using diamond polishing liquid with an average particle size of 3 μm, and polishing for 8 min using alumina polishing liquid with an average particle size of 0.05 μm.
[0072] (3) The polished aluminum target block obtained in step (2) is subjected to chemical etching for 60 s, water washing, and cold air blowing to obtain a sample to be detected; the chemical etching liquid used in the chemical etching is a mixed solution of hydrofluoric acid, phosphoric acid, and deionized water with a volume ratio of 1:15:44.
[0073] The aluminum target EBSD sample prepared in Example 3 is subjected to analysis and testing, and the test result shows that the calibration rate of the aluminum target EBSD sample is 96.6%. Figure 3 The test result graph of the aluminum target EBSD sample prepared in Example 3.
[0074] Comparative Example 1
[0075] The difference from Example 1 is that the chemical etching liquid used in the chemical etching in step (3) is a mixed solution of hydrofluoric acid, phosphoric acid, and deionized water with a volume ratio of 1:8:51.
[0076] The aluminum target EBSD sample is subjected to analysis and testing, and the test result shows that the calibration rate of the aluminum target EBSD sample is 82.2%. The uneven corrosion of the sample leads to too large surface undulation, reduces the intensity and clarity of the backscattered electron signal, makes the diffraction pattern fuzzy, and the image unclear, and thus reduces the overall calibration rate. Figure 4 The test result graph of the aluminum target EBSD sample prepared in Comparative Example 1.
[0077] Comparative Example 2
[0078] The difference from Example 1 is that the chemical etching time in step (3) is 200 s.
[0079] The aluminum target EBSD sample is subjected to analysis and testing, and the test result shows that the calibration rate of the aluminum target EBSD sample is 90%. Corrosion pits appear on the surface of the sample, and there is no signal at the pits, thus reducing the calibration rate. Figure 5 The test result graph of the aluminum target EBSD sample prepared in Comparative Example 2.
[0080] Comparative Example 3
[0081] The difference from Example 1 is that the chemical etching liquid used in the chemical etching in step (3) is a mixed solution of hydrofluoric acid and deionized water with a volume ratio of 3:40, and the chemical etching time is 200 s.
[0082] The analysis test of the aluminum target EBSD sample shows that the calibration rate of the aluminum target EBSD sample is 92%. The corrosion time is long, the microstructure is damaged, the intracrystalline corrosion occurs, the surface is rough, and the calibration rate is reduced by using the mixed solution of hydrofluoric acid and deionized water. Figure 6 The test result graph of the aluminum target EBSD sample prepared for Comparative Example 4.
[0083] Comparative Example 4
[0084] The difference between Comparative Example 3 and Comparative Example 4 is that the chemical corrosion time is 100 s.
[0085] The analysis test of the aluminum target EBSD sample shows that the corrosion time is short, the scratch stress has not been removed, and many small-angle grain boundaries are produced. Figure 7 The test result graph of the aluminum target EBSD sample prepared for Comparative Example 4.
[0086] It can be found from the data of the examples and comparative examples that the sample preparation method of the aluminum target EBSD sample of the present application is simple to operate, does not need electrolysis, vibration or ion polishing equipment, can quickly prepare the EBSD sample of the aluminum target in a large quantity, the grain boundary profile of the aluminum target EBSD sample prepared by chemical corrosion is clear, the calibration rate is > 95%, the present application improves the detection efficiency of the aluminum target EBSD, reduces the cost, and keeps a good calibration rate, and provides a better solution.
[0087] Although the above examples have made a detailed description of the present application, it is only a part of the examples of the present application, but not all the examples, and other examples can be obtained by people according to the examples of the present application without creative labor, and these examples all belong to the protection scope of the present application.
Claims
1. A method for preparing EBSD samples of aluminum target material, characterized in that, Includes the following steps: The aluminum target material is wire-cut to obtain an aluminum target block; After the aluminum target block is mounted, it is mechanically ground and polished in sequence to obtain a polished aluminum target block; The polished aluminum target block is chemically etched, washed, and dried to obtain the EBSD sample to be tested; the chemical etching solution used in the chemical etching consists of hydrofluoric acid, phosphoric acid, and water.
2. The sample preparation method according to claim 1, characterized in that, The volume ratio of hydrofluoric acid, phosphoric acid, and water is (0.5–1.5):(10–15):(44–59), the concentration of hydrofluoric acid is 40 wt%, and the concentration of phosphoric acid is 85 wt%.
3. The sample preparation method according to claim 2, characterized in that, The volume ratio of hydrofluoric acid, phosphoric acid and water is 1:(10-15):(44-49).
4. The sample preparation method according to claim 1 or 2, characterized in that, The chemical corrosion time is 1 to 3 minutes.
5. The sample preparation method according to claim 1, characterized in that, The aluminum target block has a length of 10-20 mm, a width of 10-20 mm, and a height of 8-10 mm.
6. The sample preparation method according to claim 1, characterized in that, The temperature of the inlay is 120-150℃, and the holding time is 5-15 minutes.
7. The sample preparation method according to claim 1, characterized in that, The mechanical grinding includes a first grinding and a second grinding in sequence. The first grinding uses 400-800# sandpaper, and the second grinding uses 1000-1400# sandpaper.
8. The sample preparation method according to claim 7, characterized in that, The first and second grinding sessions each lasted 3 to 5 minutes.
9. The sample preparation method according to claim 1, characterized in that, The polishing process includes a first polishing, a second polishing, and a third polishing in sequence. The first and second polishings use diamond polishing slurry, and the third polishing uses alumina polishing slurry.
10. The sample preparation method according to claim 9, characterized in that, The diamond polishing slurry used for the first polishing has an average diamond particle size of 8.8–9.2 μm, and the first polishing time is 5–8 min; the diamond polishing slurry used for the second polishing has an average diamond particle size of 2.9–3.1 μm, and the second polishing time is 3–8 min; the alumina polishing slurry has an average alumina particle size of 0.04–0.06 μm, and the third polishing time is 5–8 min.