CN209741302U - device for preparing miniature EBSD sample by mechanical electrolytic polishing - Google Patents
device for preparing miniature EBSD sample by mechanical electrolytic polishing Download PDFInfo
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- CN209741302U CN209741302U CN201822058904.6U CN201822058904U CN209741302U CN 209741302 U CN209741302 U CN 209741302U CN 201822058904 U CN201822058904 U CN 201822058904U CN 209741302 U CN209741302 U CN 209741302U
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- 238000001887 electron backscatter diffraction Methods 0.000 title claims abstract description 37
- 238000005498 polishing Methods 0.000 title abstract description 26
- 238000005070 sampling Methods 0.000 claims abstract description 15
- 230000000903 blocking effect Effects 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 abstract description 18
- 238000007517 polishing process Methods 0.000 abstract description 6
- 238000000227 grinding Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 8
- 239000000956 alloy Substances 0.000 description 6
- 229910045601 alloy Inorganic materials 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
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- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N Heavy water Chemical compound [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000002984 plastic foam Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 239000003507 refrigerant Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005464 sample preparation method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 235000007516 Chrysanthemum Nutrition 0.000 description 1
- 244000189548 Chrysanthemum x morifolium Species 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
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- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
The utility model aims at providing a device for preparing a micro EBSD sample by mechanical electrolytic polishing, which comprises a sampling platform and clamping tweezers, wherein the sampling platform consists of two symmetrical clamps and two arc columns; a groove hole is formed in the height direction of the clamp; the arc column can be clamped in the groove hole, and the height of the arc column is smaller than that of the clamp; the arc column is fastened on the clamps through bolts, one surfaces of the two clamps with the groove holes are oppositely arranged and fastened together through the bolts, and a gap is reserved between the two clamps; the tail of the clamping tweezers is provided with a lofting platform for placing and fixing a miniature sample. The device solves the problems of difficult grinding and polishing of the miniature sample and the problem of sample fastening of the miniature sample in the electrolytic polishing process. The device has improved the preparation efficiency of miniature EBSD sample, and the system appearance effect is excellent, and the sample resolution reaches more than 90%, and application scope is wide, is fit for popularizing and applying.
Description
Technical Field
The utility model belongs to the technical field of the metal material analysis, a device that is used for machinery to add the miniature EBSD sample of electrolytic polishing preparation is provided very much.
Background
Since the advent of EBSD technology from the 20 th century and the 80 th era, EBSD technology has gradually been applied to metallic materials, ceramic materials, compounds, and the like. The EBSD technology can obtain the information of the material such as crystal grains, substructures, precipitated phases, microstructure, poor crystal grain orientation and the like, has great significance for the performance research and the like of the material, and is widely applied to the micro research of materials with different structures.
because electron back diffraction only occurs in the range of dozens of nanometers on the surface layer of the material, the preparation requirement on the EBSD sample is strict, namely the sample surface is flat, has no stress, has no serious corrosion pits and the like, and because the stress exists on the sample surface and the crystal lattice can be distorted, an EBSD system can not obtain an accurate chrysanthemum cell pattern, so that the resolution is reduced; if severe etch pits occur, the range of electron back diffraction is exceeded, and the resolution of the sample is liable to be lowered. Therefore, the EBSD test requires a high sample preparation requirement. Secondly, the preparation of the micro EBSD sample has higher requirements, the difficulties are grinding and mechanical polishing of the micro sample and fastening of the micro sample in the electrolytic polishing process, and meanwhile, the optimal electrolytic polishing process of the micro EBSD sample is difficult to find.
At present, the technology for preparing the micro EBSD sample is less, the general method for preparing the EBSD sample mainly comprises mechanical polishing and electrolytic polishing, and the micro EBSD sample is difficult to prepare for the conventional mechanical polishing and electrolytic polishing. For example, for a micro sample, mechanical polishing is not easy to operate, and the sample is very small, so the requirements on the aspect of electropolishing the sample are more strict, that is, the micro EBSD sample is difficult to prepare, and the prepared sample is often poor in effect. The invention patent with the application number of 201710695101.9 provides a preparation method of a multiphase alloy EBSD analysis test sample, which has the advantages of high sample preparation cost, long sample preparation time and low sample preparation efficiency, and a sample can be prepared only on an ion thinning instrument.
the method of preparing miniature EBSD sample through machinery + electrolytic polishing mode is a simple, easy to operate, low cost, the efficient method of preparation miniature EBSD sample of system appearance, the utility model provides a device that is used for machinery + electrolytic polishing preparation miniature EBSD sample.
SUMMERY OF THE UTILITY MODEL
the utility model aims at providing a device that is used for miniature EBSD sample of mechanical electrolytic polishing preparation. The device mainly solves the problems of difficult grinding and polishing of the miniature sample and the problem of sample fastening of the miniature sample in the electrolytic polishing process. The device has wide application range, and is suitable for preparing small-size micro samples and large-size samples.
The utility model discloses technical scheme as follows:
An apparatus for preparing a micro EBSD sample by mechanical electropolishing, the apparatus comprising a sampling platform and holding tweezers, wherein:
The sampling platform consists of two symmetrical clamps 4 and two arc columns 5; a groove hole 6 is arranged in the height direction of the clamp 4; the arc column 5 can be clamped in the groove hole 6, and the height of the arc column is less than that of the clamp 4; the arc column 5 is fastened on the clamps 4 through bolts 7, one surfaces of the two clamps 4 with the groove holes 6 are oppositely arranged and fastened together through the bolts 7, and a gap 8 is reserved between the two clamps 4;
The tail of the clamping tweezers is provided with a lofting platform for placing and fixing a miniature sample.
As a preferred technical scheme:
and a bolt 7 is arranged at the position, close to the groove hole 6, of the clamp 4, and the bolt 7 is arranged in parallel to the horizontal direction and used for fastening the sample inlaying sample 1 placed on the circular arc column 5.
the width of the gap 8 is greater than the length of the micro-scale sample.
the clamping forceps comprise a left part and a right part:
in the left part: the first forceps handle 11 and the first forceps head 12 are integrally of a linear structure, a lofting platform 13 is arranged at the tail of the first forceps head 12, an object blocking plate 14 is arranged on the lofting platform 13, and the object blocking plate 14 is arranged perpendicular to the width direction of the first forceps head 12;
In the right part: the second forceps handle 21 and the second forceps head 22 are integrally of a fold line-shaped structure, and when the tail ends of the first forceps handle 11 and the second forceps handle 21 are close to each other, the second forceps head 22 with the same width as the first forceps head 12 can be placed on the lofting platform 13 and is parallel to the first forceps head 12.
The clamping forceps are further provided with a clamp 10 for fastening the left and right parts of the clamping forceps together.
the device is applicable to the preparation of miniature EBSD sample, the sample concrete preparation step is as follows:
Inserting a sample:
cutting a metal material into a miniature sample 2, inlaying the miniature sample 2 to the center of an inlaying sample on an inlaying machine to finally form an inlaying sample 1, and avoiding inlaying the sample too tightly;
Opening a V-shaped groove:
Two V-shaped grooves 3 (shown in figure 1) are symmetrically formed in the sample embedding sample 1 in the direction perpendicular to the micro sample 2, and the micro sample 2 is positioned on the connecting line of the tips of the two V-shaped grooves 3;
Thirdly, mechanically polishing the sample-embedded sample 1;
adhering a protective layer (such as transparent adhesive to the surface) on the surface of the micro sample 2 to prevent the micro sample 2 from being scratched when the embedded sample 1 is knocked open; then placing the embedded sample 1 in a sampling platform;
fastening the sample 1 in the sampling platform, applying downward force to the center of the sample 1 to break the sample along the connecting line direction of the tips of the V-shaped grooves 3, taking out the micro sample 2, and removing the protective layer on the micro sample;
Sixthly, placing the micro sample 2 on an ultrasonic instrument, and ultrasonically vibrating and cleaning the micro sample by using alcohol;
Seventhly, placing the micro sample 2 in an acidic electrolytic polishing solution for electrolytic polishing:
Firstly, voltage is taken as a main part, and then current is taken as a main part: setting the current of a power supply to be 0.8A and the voltage to be maximum and 60V, then cooling the electrolytic polishing solution to 70 ℃ below zero by using a refrigerant (preferably liquid ammonia), connecting the power supply, wherein the power supply is mainly used for voltage and 0.1A, the current is gradually increased along with the temperature rise, the voltage is unchanged, the power supply is mainly used for current when the current reaches 0.8A, the current is kept unchanged at 0.8A, the voltage starts to be reduced, the power supply is turned off when the voltage is reduced to 50V, and taking out the micro sample 2; in the electrolytic polishing process, plastic foam is used for surrounding the electrolyte for heat preservation;
and flushing the miniature sample 2 with water, flushing with alcohol and blow-drying to finally obtain the miniature EBSD sample of the metal material.
wherein, the micro sample 2 is rectangular, square, round, diamond or pentagonal (preferably rectangular), and for the rectangular or square sample, the size range is as follows: the length is 0.5-10mm, the width is 0.3-10mm, and the thickness is 0.5-3mm (generally, when cutting a sample, if the sample width is small, the sample length needs to be longer). The thickness of the insert sample 1 is 2 to 3 times the thickness of the micro-scale sample 2.
the device has solved the system appearance process complicacy of miniature sample, sample resolution low grade problem, has improved the preparation efficiency of miniature sample by a wide margin. The device has wide application range, can be used for large and small samples, is particularly suitable for preparing miniature EBSD samples, improves the preparation efficiency of the miniature EBSD samples, has excellent sample preparation effect and ensures that the sample resolution rate reaches more than 90 percent. The device has comparatively huge economic value and social value of predictability.
drawings
FIG. 1 is a schematic view of a V-shaped groove of a sample inlaid with a micro sample;
FIG. 2 is a schematic structural view of a sampling platform;
FIG. 3 is a schematic view of a holding forceps;
FIG. 4 is a schematic view of an electropolishing apparatus;
FIG. 5 is a schematic view of a specific electropolishing process;
FIG. 6 is a schematic view of a tube and a sampling method.
Reference numerals: 1. the sample inserting device comprises a sample inserting sample, 2, a miniature sample, 3, a V-shaped groove, 4, a clamp, 5, an arc column, 6, a groove hole, 7, a bolt, 8, a gap, 10, a clamp, 11, a first forceps handle, 12, a first forceps head, 13, a lofting platform, 14, a blocking plate, 21, a second forceps handle, 22 and a second forceps head.
Detailed Description
Example 1
the Zr-4 alloy has the nominal composition of Zr-1.5Sn-0.2Fe-0.1Cr, has very low thermal neutron absorption cross section, high hardness, ductility and excellent corrosion resistance, and is mainly used as a fuel cladding material in a pressurized water reactor, a boiling water reactor and a heavy water reactor.
Since the Zr-4 pipe is cylindrical, in order to observe the real grain orientation on the surface of the pipe, the information such as structure of the pipe, etc., the surface of the pipe must be tested by the EBSD technology, so that the pipe needs to be cut into a very small size (the pipe sampling is shown in fig. 6) to truly represent the external surface or the internal surface of the pipe, and the size of the sample cut at this time is as follows: length 6mm, width 0.5mm, and thickness tube thickness. The sample preparation method comprises the following steps:
Inserting a sample:
Cutting a miniature sample 2 on a Zr-4 pipe by using a wire cutting machine, putting resin with the thickness about twice that of the miniature sample 2 into an inlaying machine to be inlaid together with the miniature sample, inlaying the miniature sample 2 into the center of the inlaying sample to finally form an inlaid sample 1, and not inlaying the sample too tightly;
opening a V-shaped groove:
symmetrically forming two V-shaped grooves 3 similar to the impact test on the embedded sample 1 by using a grinder in a direction perpendicular to the micro sample 2, wherein the micro sample 2 is positioned on a connecting line of the tips of the two V-shaped grooves 3, and the connecting line is perpendicular to the length direction of the micro sample 2 (shown in figure 1);
③ polishing the sample 1: grinding with 150#, 320#, 800#, 2000# sandpaper; mechanically polishing the ground sample on a polishing machine by using a nano-particle SiO2 polishing solution;
fourthly, pasting transparent adhesive on the surface of the micro sample 2, and placing the sample 1 in the sampling platform;
Fastening the sample 1 in the sampling platform, applying a downward force to the center of the sample 1 to break the sample 1 along the connecting line of the tips of the V-shaped grooves 3, taking out the micro sample 2, and removing the transparent adhesive on the micro sample;
Sixthly, placing the micro sample 2 on an ultrasonic instrument, and ultrasonically vibrating and cleaning the micro sample by using alcohol;
Seventhly, placing the micro sample 2 in an acidic electrolytic polishing solution for electrolytic polishing:
Firstly, voltage is taken as a main part, and then current is taken as a main part: setting the current of a power supply to be 0.8A and the voltage to be maximum and 60V, then cooling the electrolytic polishing solution to 70 ℃ below zero by using a refrigerant (preferably liquid ammonia), connecting the power supply, wherein the power supply is mainly used for voltage and 0.1A, the current is gradually increased along with the temperature rise, the voltage is unchanged, the power supply is mainly used for current when the current reaches 0.8A, the current is kept unchanged at 0.8A, the voltage starts to be reduced, the power supply is turned off when the voltage is reduced to 50V, and taking out the micro sample 2; in the electrolytic polishing process, plastic foam is used for surrounding the electrolyte for heat preservation;
And eighthly, washing the micro sample 2 with water, washing with alcohol and drying to obtain the micro EBSD sample of the Zr-4 pipe.
The sampling platform structure:
As shown in FIG. 2, the sampling platform used in the embodiment is composed of two symmetrical clamps 4 and two arc columns 5; a groove hole 6 is formed in the height direction of the clamp 4, and the diameter of the section of the groove hole 6 is larger than that of the sample 1; the arc column 5 can be clamped in the groove hole 6, the height of the arc column is smaller than that of the clamp 4, and the arc column 5 is used for supporting the sample 1; the arc column 5 is fastened on the clamp 4 through a bolt 7, and the two symmetrical clamps 4 are fastened together through the bolt 7.
and a bolt 7 is arranged at the position, close to the groove hole 6, of the clamp 4, the bolt 7 is arranged in parallel to the horizontal direction and is used for fastening the sample inlaying sample 1 placed on the circular arc column 5 so as to prevent the sample inlaying sample 1 from moving to scratch the miniature sample 2 in the smashing process.
When the sample embedding device is used, the arc columns 5 are clamped in the groove holes 6, then the surfaces, provided with the groove holes 6, of the two clamps 4 are arranged oppositely, a gap 8 is reserved between the clamps 4, the sample embedding sample 1 is placed on the two oppositely arranged arc columns 5, and the connecting line of the tips of the V-shaped grooves 3 on the sample embedding sample 1 is located in the gap 8 between the clamps 4; the bolts 7 between the two clamps 4 are tightened to clamp the mounted sample 1.
the structure of the clamping forceps is as follows:
as shown in FIG. 3, the holding forceps used in the embodiment is composed of a left part and a right part:
In the left part: the first forceps handle 11 and the first forceps head 12 are integrally of a linear structure, a lofting platform 13 is arranged at the tail of the first forceps head 12, an object blocking plate 14 is arranged on the lofting platform 13, and the object blocking plate 14 is arranged perpendicular to the width direction of the first forceps head 12;
in the right part: the second forceps handle 21 and the second forceps head 22 are integrally of a fold-line structure, when the tail ends of the first forceps handle 11 and the second forceps handle 21 are close to each other, the second forceps head 22 with the same width as the first forceps head 12 can be arranged on the lofting platform 13 and is parallel to the first forceps head 12, so that effective holding of a sample is guaranteed;
After the micro sample 2 is placed on the lofting platform 13, the left and right parts of the clamping tweezers are fastened together by the clamp 10.
example 2
the thickness direction (thickness of 0.3mm) of the Zr-2 alloy strip was then subjected to EBSD sample preparation by the method described in example 1.
The Zr-2 alloy has good corrosion resistance, moderate mechanical property, lower atomic thermal neutron absorption cross section (zirconium is 0.18 target en) at the high temperature and the high pressure of 300-400 ℃ in water vapor, and good compatibility with nuclear fuel, so the Zr-2 alloy can be used as a reactor core structural material (a fuel cladding, a pressure pipe, a bracket and a pore pipe) of a water-cooled nuclear reactor, and is mainly used as the Zr-2 alloy.
Since the Zr-2 strip is a thin sheet having a thickness of 0.3mm, the surface of the strip in the thickness direction must be tested by the EBSD technique in order to observe information such as the thickness surface grain orientation and texture of the strip. A difficulty in preparing samples of surface EBSD in the thickness direction of the strip is that the strip thickness is only 0.3 mm. The size of the sample cut at this time is as follows: the length is 6mm, the width is 0.5mm, and the thickness is 0.3 mm. The sample preparation method is basically the same as that in example 1.
the utility model is not the best known technology.
the above embodiments are only for illustrating the technical concept and features of the present invention, and the purpose of the embodiments is to enable people skilled in the art to understand the contents of the present invention and to implement the present invention, which cannot limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered by the protection scope of the present invention.
Claims (5)
1. an apparatus for preparing a micro EBSD sample by mechanical electropolishing, the apparatus comprising a sampling platform and holding tweezers, wherein:
the sampling platform consists of two symmetrical clamps (4) and two arc columns (5); a groove hole (6) is arranged in the height direction of the clamp (4); the arc column (5) can be clamped in the groove hole (6), and the height of the arc column is smaller than that of the clamp (4); the arc column (5) is fastened on the clamps (4) through bolts (7), one surfaces of the two clamps (4) with the groove holes (6) are oppositely arranged and fastened together through the bolts (7), and a gap (8) is reserved between the two clamps (4);
the tail of the clamping tweezers is provided with a lofting platform for placing and fixing a miniature sample.
2. The apparatus for preparing a micro EBSD specimen by mechanical electropolishing as claimed in claim 1, wherein: and a bolt (7) is arranged at the position, close to the groove hole (6), of the clamp (4), and the bolt (7) is arranged in parallel to the horizontal direction and used for fastening and placing the sample inlaying sample (1) on the arc column (5).
3. the apparatus for preparing a micro EBSD specimen by mechanical electropolishing as claimed in claim 1, wherein: the width of the gap (8) is larger than the length of the micro sample.
4. the apparatus for preparing a micro EBSD specimen by mechanical electropolishing as claimed in claim 1, wherein: the clamping forceps comprise a left part and a right part:
in the left part: the first forceps handle (11) and the first forceps head (12) are integrally of a linear structure, a lofting platform (13) is arranged at the tail of the first forceps head (12), an object blocking plate (14) is arranged on the lofting platform (13), and the object blocking plate (14) is arranged perpendicular to the width direction of the first forceps head (12);
in the right part: the second forceps handle (21) and the second forceps head (22) are integrally of fold-line structures, when the tail ends of the first forceps handle (11) and the second forceps handle (21) are close to each other, the second forceps head (22) with the same width as the first forceps head (12) can be placed on the lofting platform (13) and is parallel to the first forceps head (12).
5. The apparatus for preparing micro EBSD specimens by mechanical electropolishing as claimed in claim 4, wherein: the clamping tweezers are further provided with a clamp (10) for fastening the left part and the right part of the clamping tweezers together.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201822058904.6U CN209741302U (en) | 2018-12-10 | 2018-12-10 | device for preparing miniature EBSD sample by mechanical electrolytic polishing |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201822058904.6U CN209741302U (en) | 2018-12-10 | 2018-12-10 | device for preparing miniature EBSD sample by mechanical electrolytic polishing |
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| CN209741302U true CN209741302U (en) | 2019-12-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111595876A (en) * | 2020-06-02 | 2020-08-28 | 全球能源互联网研究院有限公司 | Electrolytic clamp and method for preparing EBSD sample of metal sheet |
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2018
- 2018-12-10 CN CN201822058904.6U patent/CN209741302U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111595876A (en) * | 2020-06-02 | 2020-08-28 | 全球能源互联网研究院有限公司 | Electrolytic clamp and method for preparing EBSD sample of metal sheet |
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