CN117451758A - Sample preparation method of titanium alloy foil EBSD sample - Google Patents
Sample preparation method of titanium alloy foil EBSD sample Download PDFInfo
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- CN117451758A CN117451758A CN202311489204.1A CN202311489204A CN117451758A CN 117451758 A CN117451758 A CN 117451758A CN 202311489204 A CN202311489204 A CN 202311489204A CN 117451758 A CN117451758 A CN 117451758A
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 39
- 238000001887 electron backscatter diffraction Methods 0.000 title claims abstract description 28
- 239000011888 foil Substances 0.000 title claims abstract description 16
- 238000005464 sample preparation method Methods 0.000 title claims abstract description 13
- 238000005498 polishing Methods 0.000 claims abstract description 93
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000005520 cutting process Methods 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000011347 resin Substances 0.000 claims abstract description 10
- 229920005989 resin Polymers 0.000 claims abstract description 10
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 8
- 239000010959 steel Substances 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 238000010892 electric spark Methods 0.000 claims abstract description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 7
- 244000137852 Petrea volubilis Species 0.000 claims description 4
- 239000002390 adhesive tape Substances 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 87
- 238000004458 analytical method Methods 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a sample preparation method of a titanium alloy foil EBSD sample, which specifically comprises the following steps: step 1: cutting and fixing a sample, namely clamping a titanium foil sample to be cut by adopting two straight steel plates, and cutting the titanium foil sample into a shape according to a preset size by wire electric discharge cutting; cutting a titanium alloy plate with the same size as the cut titanium foil sample by electric spark; alternately pasting the cut titanium foil sample and the titanium alloy plate to obtain a sample to be polished; embedding a sample to be polished into a cylindrical resin by using a thermal embedding machine; step 2: automatically polishing, and mechanically polishing the inlaid sample to be polished for three times: step 3: and (3) vibration polishing, namely placing the mechanically polished sample into a vibration polishing clamp, adding two balancing weights, vibration polishing for 3-5 h, and then ultrasonically cleaning the sample with ethanol for 10-20 min. The technical scheme of the invention solves the problems of defects in grinding and polishing of ultrathin titanium foil and complicated process in the prior art.
Description
Technical Field
The invention relates to the technical field of precise ultrathin strip surface treatment, in particular to a sample preparation method of a titanium alloy foil EBSD sample.
Background
With the progress of modern scientific technology, the demands of related industries such as micro-forming and the like on the development of precise ultrathin belts are also urgent. In recent years, the application amount of titanium and titanium alloy strip foil is also increasing, such as precision instruments with important applications, such as aerospace, etc., fillers with high requirements on corrosion resistance in chemical industry, materials for components in electronic industry, etc. As the internal structure of the titanium foil is greatly deformed in the thinning rolling process, the mechanical property of the titanium foil is finally affected. Therefore, research on the microstructure change of the material has important significance for exploring the comprehensive performance of the titanium foil.
At present, the electrolytic polishing technology is a simple and easy surface processing technology, and the obtained sample has low surface roughness and high brightness and is commonly used for sample preparation of metallographic phase, scanning and electron back scattering diffraction technology. The electrolytic polishing technology has been widely applied in the fields of metal finish machining, metallographic sample preparation and the need of controlling surface quality and finish, and applied in the fields of chemical industry, light industry, machine manufacturing, strong laser system, food processing equipment, decoration industry, biomedicine and the like.
EBSD is an analysis technology of electron back scattering pattern crystal micro-region orientation and crystal structure assembled on a scanning electron microscope, and is an important means for characterization analysis of microstructure and micro-texture of materials. The requirements on the surface of the sample in the test are high, and the sample is required to be smooth, flat, free of scratches and free of residual stress. Because the thickness of the titanium foil is too thin, excessive sample grinding and polishing can cause defects of the material, traditional sample preparation modes such as embedding, clamping, hand pinching and the like cannot be realized for extremely thin strips, and for electrolytic polishing, the thickness is too small, the surface to be detected is enabled to be in a cambered surface shape after electrolytic polishing, so that the surface is uneven, on one hand, the standard rate of a sample to be detected is reduced, and on the other hand, the area to be detected for the EBSD is too small, and information such as real microstructure, texture and the like cannot be truly reflected. In addition, the polishing solution is generally strong acid, the proportion of the electrolyte is high, and the processes such as current selection, electrolysis time and the like also need a great deal of time to explore.
The scanning electron microscope equipped with the EBSD probe can carry out crystal structure analysis on the titanium alloy in submicron scale, such as crystal orientation, grain boundary characteristic analysis, real grain size measurement, fracture mechanism, failure mechanism research, strain evaluation and the like, and has wide application on the research of the microstructure of the titanium alloy. At present, the polishing process for the medium-thickness titanium plate is mature, and certain difficulties exist in the sample preparation mode of the titanium alloy thin plate with the thickness of less than 1 mm. At present, the microstructure research of the ultrathin titanium alloy plate is also indispensable, so that the sample preparation mode of the ultrathin titanium alloy plate has wide application prospect.
Disclosure of Invention
According to the technical problems that the prior art is provided for polishing the ultrathin titanium foil sample and the process is complicated, the sample preparation method of the titanium alloy foil EBSD sample is provided.
The invention adopts the following technical means:
a sample preparation method of a titanium alloy foil EBSD sample specifically comprises the following steps:
step 1: sample interception and immobilization
Clamping a titanium foil sample to be intercepted by adopting two straight steel plates, and cutting the titanium foil sample according to a preset size by wire electric discharge cutting; cutting a titanium alloy plate with the same size as the cut titanium foil sample by electric spark; alternately pasting the cut titanium foil sample and the titanium alloy plate to obtain a sample to be polished; embedding a sample to be polished into a cylindrical resin by using a thermal embedding machine;
step 2: automatic polishing and polishing
And (3) mechanically polishing the inlaid sample to be polished for three times:
step 3: vibration polishing
Placing the mechanically polished sample into a vibration polishing clamp, adding two balancing weights, mixing the OP-S polishing solution and hydrogen peroxide for vibration polishing to obtain the polishing solution, performing vibration polishing for 3-5 h, and then ultrasonically cleaning the sample with ethanol for 10-20 min.
Further, in the step 1, two flat steel plates with the thickness of 2mm are adopted to clamp a titanium foil sample to be intercepted; the square titanium foil sample is 8mm long, 6mm wide and 0.10-0.15 mm thick; the thickness of the titanium alloy plate is 2-5mm; cutting conductive double faced adhesive tape with the same size as the cut titanium foil sample, and alternately pasting the cut titanium foil sample and the titanium alloy plate; samples to be polished were mounted into a 25mm diameter cylindrical resin using a model citoporess-30 thermal mounting machine.
Further, in the step 2, the embedded sample to be polished is mechanically polished for three times by adopting a Tegramin-25 automatic Style polisher: the single-point pressure of the first pass is 80N, the rotation speed of the polishing disc is 300rpm, the rotation speed of the sample clamp is 150rpm, the abrasive paper is 180# and the polishing time is 4 minutes; setting the single-point pressure of the second pass as 100N, setting the rotation speed of a polishing disc as 300rpm, setting the number of sand paper as 320#, and setting the polishing time as 3 minutes; the third pressure was increased to 120N, the polishing disc rotation speed was 150rpm, the sample holder rotation speed was 150rpm, the polishing disc was Diapro, and the polishing time was 5 minutes.
Further, in the step 3, the type of the adopted vibration polishing equipment is Vibromet2; the polishing solution is obtained by mixing OP-S polishing solution and hydrogen peroxide according to the volume ratio of 4:1.
Compared with the prior art, the invention has the following advantages:
the sample preparation method of the titanium alloy foil EBSD sample can prepare samples of precise ultrathin foil and can achieve the surface requirements of EBSD test by surface treatment; the whole sample preparation process does not need to use acid chemicals, and is safer and more environment-friendly; the method has the advantages that electrolytic polishing is not needed, the cost is low, the process is simpler, the prepared sample for EBSD analysis of the titanium foil has very high resolution, the resolution is up to about 98%, and the EBSD analysis requirement is completely met.
Based on the reasons, the method can be widely popularized in the field of precision ultrathin belt surface treatment.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to the drawings without inventive effort to a person skilled in the art.
FIG. 1 is a schematic view of the structure of a sample to be polished according to the present invention.
FIG. 2 is an IPF and BC plot of the sample prepared in example 1 calibrated with EBSD.
FIG. 3 is an IPF and BC plot of the sample prepared in example 2 calibrated with EBSD.
FIG. 4 is an IPF and BC plot of the sample prepared in example 3 calibrated with EBSD.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a sample preparation method of a titanium alloy foil EBSD sample, which specifically comprises the following steps:
step 1: sample interception and immobilization
Clamping a titanium foil sample to be intercepted by adopting two straight steel plates, and cutting the titanium foil sample according to a preset size by wire electric discharge cutting; cutting a titanium alloy plate with the same size as the cut titanium foil sample by electric spark; alternately pasting the cut titanium foil sample and the titanium alloy plate to obtain a sample to be polished; embedding a sample to be polished into a cylindrical resin by using a thermal embedding machine;
step 2: automatic polishing and polishing
And (3) mechanically polishing the inlaid sample to be polished for three times:
step 3: vibration polishing
Placing the mechanically polished sample into a vibration polishing clamp, adding two balancing weights, mixing the OP-S polishing solution and hydrogen peroxide for vibration polishing to obtain the polishing solution, performing vibration polishing for 3-5 h, and then ultrasonically cleaning the sample with ethanol for 10-20 min.
Further, in the step 1, two flat steel plates with the thickness of 2mm are adopted to clamp a titanium foil sample to be intercepted; the square titanium foil sample is 8mm long, 6mm wide and 0.10-0.15 mm thick; the thickness of the titanium alloy plate is 2-5mm; cutting conductive double faced adhesive tape with the same size as the cut titanium foil sample, and alternately pasting the cut titanium foil sample and the titanium alloy plate; samples to be polished were mounted into a 25mm diameter cylindrical resin using a model citoporess-30 thermal mounting machine.
Further, in the step 2, the embedded sample to be polished is mechanically polished for three times by adopting a Tegramin-25 automatic Style polisher: the single-point pressure of the first pass is 80N, the rotation speed of the polishing disc is 300rpm, the rotation speed of the sample clamp is 150rpm, the abrasive paper is 180# and the polishing time is 4 minutes; setting the single-point pressure of the second pass as 100N, setting the rotation speed of a polishing disc as 300rpm, setting the number of sand paper as 320#, and setting the polishing time as 3 minutes; the third pressure was increased to 120N, the polishing disc rotation speed was 150rpm, the sample holder rotation speed was 150rpm, the polishing disc was Diapro, and the polishing time was 5 minutes.
Further, in the step 3, the type of the adopted vibration polishing equipment is Vibromet2; the polishing solution is obtained by mixing OP-S polishing solution and hydrogen peroxide according to the volume ratio of 4:1.
According to the sample preparation method of the titanium alloy foil EBSD sample, acid chemicals are not required to be used in the whole sample preparation process, so that the method is safer and more environment-friendly; the method has the advantages that electrolytic polishing is not needed, the cost is low, the process is simpler, the prepared sample for EBSD analysis of the titanium foil has very high resolution, the resolution is up to about 98%, and the EBSD analysis requirement is completely met.
Example 1
The embodiment provides a sample preparation method of a titanium alloy foil EBSD sample, which specifically comprises the following steps:
step 1: sample interception and immobilization
Clamping a titanium foil sample to be intercepted by two flat steel plates with the thickness of 2mm, cutting a square titanium foil sample with the length of 8mm, the width of 6mm and the thickness of 0.15mm according to a preset size by wire electric discharge cutting; cutting a titanium alloy plate with the thickness of 2mm, which is the same as the size of the cut titanium foil sample, by electric spark; cutting conductive double faced adhesive tape with the same size as the cut titanium foil sample, alternately pasting the cut titanium foil sample and the titanium alloy plate to obtain a sample to be polished, wherein 1 is the titanium alloy plate with the thickness of 2mm, and 2 is the titanium foil sample with the thickness of 0.15mm as shown in figure 1; embedding a sample to be polished into cylindrical resin with the diameter of 25mm and the height of 12mm by using a model CitoPress-30 thermal embedding machine;
step 2: automatic polishing and polishing
And (3) mechanically polishing the inlaid sample to be polished for three times: and (3) mechanically polishing the inlaid sample to be polished for three times by adopting a Tegramin-25 automatic Style polishing machine: the single-point pressure of the first pass is 80N, the rotation speed of the polishing disc is 300rpm, the rotation speed of the sample clamp is 150rpm, the abrasive paper is 180# and the polishing time is 4 minutes; setting the single-point pressure of the second pass as 100N, setting the rotation speed of a polishing disc as 300rpm, setting the number of sand paper as 320#, and setting the polishing time as 3 minutes; the third pressure is increased to 120N, the rotation speed of the polishing disc is 150rpm, the rotation speed of the sample clamp is 150rpm, the polishing disc is Diapro, and the polishing time is 5 minutes;
step 3: vibration polishing
And (2) placing the mechanically polished sample into a vibration polishing clamp by adopting vibration polishing equipment with the model of Vibromet2, adding two balancing weights, mixing the polishing solution used in vibration polishing with OP-S polishing solution and hydrogen peroxide, performing vibration polishing for 3 hours, then ultrasonically cleaning the sample with ethanol for 20 minutes, and calibrating the sample by using a scanning electron microscope with an EBSD probe, wherein the calibration rate is 98 percent as shown in figure 2.
Example 2
The difference between this example and example 1 is that in step 1, the thickness of the titanium foil sample is 0.10mm and the thickness of the titanium alloy plate is 3mm; embedding a sample to be polished into a cylindrical resin with the diameter of 25mm and the height of 15mm by using a thermal embedding machine;
in the step 3, vibration polishing is carried out for 4 hours, then the sample is ultrasonically cleaned for 30 minutes by ethanol, a smooth and bright polished surface is obtained, and after the scanning electron microscope with the EBSD probe is calibrated, as shown in fig. 3, the calibration rate is 96%.
Example 3
The difference between this example and example 1 is that the thickness of the titanium foil sample is 0.14mm and the thickness of the titanium alloy plate is 2mm; embedding a sample to be polished into a cylindrical resin with the diameter of 25mm and the height of 16mm by using a thermal embedding machine;
in the step 3, vibration polishing is carried out for 3.5 hours, then the sample is ultrasonically cleaned for 25 minutes by ethanol, a smooth and bright polished surface is obtained, and the calibration rate is 95% after the scanning electron microscope with the EBSD probe is calibrated as shown in figure 4.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (4)
1. The sample preparation method of the titanium alloy foil EBSD sample is characterized by comprising the following steps of:
step 1: sample interception and immobilization
Clamping a titanium foil sample to be intercepted by adopting two straight steel plates, and cutting the titanium foil sample according to a preset size by wire electric discharge cutting; cutting a titanium alloy plate with the same size as the cut titanium foil sample by electric spark; alternately pasting the cut titanium foil sample and the titanium alloy plate to obtain a sample to be polished; embedding a sample to be polished into a cylindrical resin by using a thermal embedding machine;
step 2: automatic polishing and polishing
And (3) mechanically polishing the inlaid sample to be polished for three times:
step 3: vibration polishing
Placing the mechanically polished sample into a vibration polishing clamp, adding two balancing weights, mixing the OP-S polishing solution and hydrogen peroxide for vibration polishing to obtain the polishing solution, performing vibration polishing for 3-5 h, and then ultrasonically cleaning the sample with ethanol for 10-20 min.
2. The sample preparation method of the titanium alloy foil EBSD sample according to claim 1, wherein in the step 1, two flat steel plates with the thickness of 2mm are adopted to clamp the titanium foil sample to be intercepted; the square titanium foil sample is 8mm long, 6mm wide and 0.10-0.15 mm thick; the thickness of the titanium alloy plate is 2-5mm; cutting conductive double faced adhesive tape with the same size as the cut titanium foil sample, and alternately pasting the cut titanium foil sample and the titanium alloy plate; samples to be polished were mounted into a 25mm diameter cylindrical resin using a model citoporess-30 thermal mounting machine.
3. The sample preparation method of the titanium alloy foil EBSD sample according to claim 1, wherein in the step 2, a Tegramin-25 automatic Style polisher is adopted to mechanically polish the inlaid sample to be polished three times: the single-point pressure of the first pass is 80N, the rotation speed of the polishing disc is 300rpm, the rotation speed of the sample clamp is 150rpm, the abrasive paper is 180# and the polishing time is 4 minutes; setting the single-point pressure of the second pass as 100N, setting the rotation speed of a polishing disc as 300rpm, setting the number of sand paper as 320#, and setting the polishing time as 3 minutes; the third pressure was increased to 120N, the polishing disc rotation speed was 150rpm, the sample holder rotation speed was 150rpm, the polishing disc was Diapro, and the polishing time was 5 minutes.
4. The method for preparing the titanium alloy foil EBSD test sample according to claim 1, wherein in the step 3, the type of the vibration polishing equipment is Vibromet2; the polishing solution is obtained by mixing OP-S polishing solution and hydrogen peroxide according to the volume ratio of 4:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311489204.1A CN117451758A (en) | 2023-11-09 | 2023-11-09 | Sample preparation method of titanium alloy foil EBSD sample |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311489204.1A CN117451758A (en) | 2023-11-09 | 2023-11-09 | Sample preparation method of titanium alloy foil EBSD sample |
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| Publication Number | Publication Date |
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| CN117451758A true CN117451758A (en) | 2024-01-26 |
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| CN202311489204.1A Pending CN117451758A (en) | 2023-11-09 | 2023-11-09 | Sample preparation method of titanium alloy foil EBSD sample |
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