CN103128657A - Clamp used for electron back scattering diffraction sample vibration polishing and use method thereof - Google Patents
Clamp used for electron back scattering diffraction sample vibration polishing and use method thereof Download PDFInfo
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- CN103128657A CN103128657A CN2011103796438A CN201110379643A CN103128657A CN 103128657 A CN103128657 A CN 103128657A CN 2011103796438 A CN2011103796438 A CN 2011103796438A CN 201110379643 A CN201110379643 A CN 201110379643A CN 103128657 A CN103128657 A CN 103128657A
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Abstract
The invention relates to a clamp used for electron back scattering diffraction sample vibration polishing. The clamp comprises a sample and is characterized in that the sample is arranged on the bottom portion of a second cylinder, a first cylinder and a weight stack are sequentially arranged above the second cylinder, a first stud is arranged in the horizontal direction of the sample, and the first stud stretches into the inner side of the second cylinder from a through hole of the side wall of the second cylinder. A second stud is arranged in a vertical direction of the upper end of the sample, and the second stud stretches into the inner portion of the second cylinder from through holes of the second cylinder, the first cylinder and the weight stack. Simultaneously, the invention further provides a use method used for the clamp for electron back scattering diffraction sample vibration polishing. The clamp can effectively solve the problems that due to the fact that an electron back scattering diffraction sample is small in size, the sample in difficult to prepare, and due to small weight of the sample, vibration polishing effect is not good, and solve the machining problem of the sample surface which has a certain relationship with specific crystal orientation.
Description
Technical field
The present invention relates to a kind of fixture and using method thereof, relate to particularly a kind of fixture and using method thereof for EBSD sample vibrations polishing.
Background technology
EBSD (EBSD, be Electron BackScattered Diffraction), namely get on the crystal samples of inclination by a branch of fixing electron beam, thereby form diffraction pattern on fluorescent screen, this diffracting diagram understands the crystal structure of sample.Be mainly used in the crystallography information of quick obtaining crystalline material, can carry out texture and the analysis of intercrystalline misorientation to material, crystallite dimension and distribution of shapes analysis, crystal boundary, subgrain and twin analysis, the analysis of strain and recrystallization, and the identification of phases and phase content calculating etc., solve the problem of material in the processes such as crystallization, film preparation, semiconductor devices, deformation, recrystallization, phase transformation, fracture, corrosion.
Along with the development of Electron Back-scatter Diffraction Analysis Technique, the requirement of experiment of analyzing about EBSD in daily research and production work is also more and more.Because the EBSD analysis is very high for the requirement of sample, so the preparation of EBSD analytical sample just becomes an important research direction.EBSD is analyzed restriction for sample mainly from two aspects: the one, and need to carry out to sample the inclination of certain angle when analyzing due to EBSD, so also just require the specimen size can not be too large; The 2nd, the EBSD analysis is higher for the thickness requirement of the strain remnant layer of specimen surface, will the mass formation of diffraction pattern be seriously influenced in case the strain remnant layer is thicker, even may cause producing style.
There is following difficulty in above-mentioned requirement for restriction for sample when making the preparation sample:
At first, small sample size itself has improved the difficulty of sample preparation.Little must causing of specimen size makes sample be difficult for controlling in polishing and polishing stage, thereby increase the difficulty of polishing and polishing, sample can occur even control the situation that incessantly causes sample to fly out, this can threaten and very easily damage sample sample preparation personnel's personal safety;
Secondly, the surface stress that EBSD is analyzed for sample requires very high, therefore ordinary circumstance mainly takes the way of multiple polishing to reduce surface stress, namely first carry out just throwing under high rotating speed, rough polishing particle polishing liquid, then carry out essence and throw under the slow-speed of revolution, fine polishing particle polishing liquid.Even need 3～4 heavy repeatedly polishings for some special sample, so just greatly reduced the efficient of sample preparation, can't satisfy the needs of research and production; Another way is to adopt the vibrations polishing technology to remove the stressor layers of specimen surface.The principle of vibrations polishing is utilize the sample vibrations and conduct oneself with dignity and reduce the technology of surface strain layer, is mainly used in the polishing of softer material.But EBSD analytical sample itself causes itself weight can't reach the weight requirement of vibrations polishing to the requirement of specimen size.And existing specimen holder can't satisfy the flexible counterweight requirement of different polishing samples, can only single counterweight, namely require to carry out optimum counterweight according to sample.
Again, the depth of parallelism of original method for making sample before to the sample polishing requires very high.The sample upper and lower surface must be parallel before preparation to require sample, because it can't adjust the depth of parallelism of sample upper and lower surface in sample making course.In addition, if need to observe the orientation of sample particular plane, can't reach in traditional sample making course.
For the preparation and fabrication of sample, the present domestic following patent documentation that mainly exists:
Application number: 200520126668.7, utility model title: Multifunction sample polishing holder for spectral analysing sample.Its principal character is at the fixing adjusted kink of the front end of handle, establish four symmetrical spill embedding mouths on the opening's edge of regulating kink, be equipped with adjustment screw on the arc-like sheet between adjacent spill embedding mouth, by spill embedding mouth and adjustment screw, non-magnetic material and sample different, variable thickness fixed.Yet the fixture that provides by this utility model, and can't guarantee the fixing of particular orientation sample namely can't prepare the specimen surface that possesses certain relation with particular crystal orientation, and counterweight flexibly.
Application number: 200620047017.3, utility model title: a kind of sample polishing clamp.The fixture that this utility model provides is placed sample by two cavitys are set, and stretches into the body cavity with the sample that is fixedly clamped by trip bolt from the base side section, and magnetic is set in order to adsorb sample in body cavity.Yet this kind fixture can't carry out the preparation of non magnetic sample, and counterweight flexibly, and can't prepare the specimen surface that possesses certain relation with particular crystal orientation.
Summary of the invention
For solving the purpose of above-mentioned existence, the object of the present invention is to provide a kind of fixture for EBSD sample vibrations polishing, be used for effectively solving the sample that the EBSD sample causes because size is less prepares difficult problem, the vibrations polishing effect that causes because sample weight is less is bad problem and possess the processing problems of the specimen surface of certain relation with particular crystal orientation.Simultaneously, the present invention also provides the described using method that shakes the fixture of polishing for the EBSD sample.
For achieving the above object, the present invention takes following technical scheme:
A kind of fixture for EBSD sample vibrations polishing, described fixture is used for the clamping sample, it is characterized in that:
Described sample is arranged at bottom the second cylinder,
Be disposed with the first cylinder and weight stack above described the second cylinder,
Be provided with the first double-screw bolt in described sample horizontal direction, described the first double-screw bolt stretches into the second cylinder interior from the through hole of the second cylindrical sidewall,
Be provided with the second double-screw bolt in described sample upper end vertical direction, it is inner that described the second double-screw bolt stretches into the second cylinder from the through hole of the second cylinder, the first cylinder and weight stack.
According to a kind of fixture for EBSD sample vibrations polishing provided by the invention, what adopt is, the quantity of described the first double-screw bolt is 4, and the quantity of described the second double-screw bolt is 4, described 4 the first double-screw bolts are the cross setting, the setting that is square of described 4 the second double-screw bolts.
According to a kind of fixture for EBSD sample vibrations polishing provided by the invention, employing be, described the second double-screw bolt is provided with nut at weight stack one end, described through hole is tapped through hole.
According to a kind of fixture for EBSD sample vibrations polishing provided by the invention, employing be, the described first cylindrical diameter is 25～35mm, the described second cylindrical diameter is 15～25mm.
According to a kind of fixture for EBSD sample vibrations polishing provided by the invention, employing be that described the second cylinder is hollow cylinder, and bottom opening.
According to a kind of fixture for EBSD sample vibrations polishing provided by the invention, what adopt is, described the first double-screw bolt, the second double-screw bolt, the first cylinder and the second cylinder select one or more low density metals to make, and described low density metals comprises aluminium, titanium, magnesium.
According to a kind of fixture for EBSD sample vibrations polishing provided by the invention, employing be, described weight stack is processed by several metal mixed, described metal comprises aluminium, iron and molybdenum.
In addition, the present invention also provides a kind of using method that shakes the fixture of polishing for the EBSD sample, and technical scheme is as follows:
With the sample horizontal positioned, the placed face down with needs processing is characterized in that, also comprises the steps:
(a), clip vertical is positioned over the top of sample;
(b), adjust the first double-screw bolt, the first double-screw bolt is fixed sample from the side;
(c), adjust the second double-screw bolt, the second double-screw bolt is fixed sample from the top;
(d), sample is polished and polishing;
(e), adjust the whole total amount of sample and fixture by weight stack;
(f), sample is shaken polishing;
(g), make required sample.
According to the using method of a kind of fixture for EBSD sample vibrations polishing provided by the invention, employing be when sample is irregular small sample, also to comprise the steps:
(1), adjust the second double-screw bolt described in described step (c), the second double-screw bolt and sample upper surface are fitted;
(2), adjust the first double-screw bolt according to described step, the first double-screw bolt is fixed sample from the side;
(3), according to described step, sample is polished and polishing, make the sample lower surface concordant with the first cylinder lower surface;
(4), after treatment sample in step (three) is taken out, be inverted sample and according to the fixing sample of step () and step (two);
(5), according to described step (d), the sample in step is polished and polishing, make the sample lower surface concordant with upper surface;
(6), according to described step (e) and step (f), the sample that obtains after processing through step (five) is processed processing;
(7), make required sample.
According to a kind of fixture for EBSD sample vibrations polishing provided by the invention, employing be when sample is the particular orientation sample, also to comprise the steps:
(A), determine the angle of the specimen surface that makes in described step (g) and crystal orientation by X-ray diffractometer;
(B), the second double-screw bolt described in set-up procedure (c), make that in step (f), prepared sample forms determined angle in step (A);
(C), repeating step (three) is to step (six), makes required sample.
Provided by the present invention a kind ofly be for the fixture of EBSD sample vibrations polishing and the beneficial effect of using method thereof:
(1), by the first cylinder and the second cylinder being set, the size of expansion sample, thereby reduction sample preparation difficulty, raising sample preparation efficient;
(2), coordinating by weight stack and fixture, can adjust flexibly the overall weight of sample and fixture, be applied to the requirement of polished surface weight when satisfying different metal and specimen surface situation for the vibrations polishing, thereby improve vibrations polishing specimen surface quality, increase work efficiency;
(3), by the first double-screw bolt and the second double-screw bolt are set, thereby guarantee can guarantee the stable of sample man-hour and be easy to clamping adding, therefore the irregular small sample that is difficult for cutting can be processed into the parallel small sample of upper and lower surface;
(4), by the first double-screw bolt and the second double-screw bolt are set, thereby guarantee can guarantee the stable of sample man-hour and be easy to clamping adding, therefore can prepare the sample (being the particular orientation sample) that is orientated to certain angle with crystal.
Description of drawings
Fig. 1 is a kind of structural representation that shakes the fixture of polishing for the EBSD sample provided by the present invention.
Fig. 2 is the top view of Fig. 1.
Fig. 3 uses a kind of structural representation that shakes the fixture of polishing for the EBSD sample provided by the present invention when being the irregular small sample of processing.
Fig. 4 is with the structural representation after the lower surface processing of the irregular small sample in Fig. 3.
Fig. 5 is the structural representation after the irregular small sample in Fig. 4 is inverted.
Fig. 6 is with the structural representation after the lower surface processing of the irregular small sample in Fig. 5.
Fig. 7 is the structural representation of preparation particular orientation sample.
In figure, the 1, first cylinder 2, the first double-screw bolt 3, weight stack 4, sample 5, nut 6, the second cylinder 7, the second double-screw bolt 8, through hole.
The specific embodiment
Below in conjunction with accompanying drawing, a kind of fixture and using method thereof for EBSD sample vibrations polishing provided by the invention is further explained explanation.
At first, the structure of described a kind of fixture for EBSD sample vibrations polishing is as follows:
as shown in Figure 1, sample 4 is arranged at the second cylinder 6 bottoms, the second cylinder 6 is hollow cylinder and lower ending opening, described the second cylinder 6 upper ends are disposed with the first cylinder 1 and weight stack 3, be provided with the first double-screw bolt 2 in described sample 4 horizontal directions, described the first double-screw bolt 2 stretches into the second cylinder 6 inboards from the through hole 8 of the second cylinder 6 sidewalls, be provided with the second double-screw bolt 7 in described sample 4 upper end vertical direction, described the second double-screw bolt 7 is from the second cylinder 6, the through hole 8 of the first cylinder 1 and weight stack 3 stretches into the second cylinder 6 inside, described the second double-screw bolt 7 is provided with nut 5 at weight stack 3 one ends, be used for fixed weight sheet 3.
Wherein, described through hole 8 is tapped through hole; The diameter of described the first cylinder 1 is 25～35mm, and the diameter of described the second cylinder 6 is 15～25mm; Described the first double-screw bolt 2, the second double-screw bolt 7, the first cylinder 1 and the second cylinder 6 select one or more in low density metals to make, and described low density metals comprises aluminium, titanium, magnesium, and wherein, density is defined as low-density lower than Fe7.86.Its material can be single metal, can be also two or more, i.e. alloy; Described weight stack 3 is processed by several metal mixed, described metal comprises aluminium, iron and molybdenum, wherein, the purpose of using light and heavy metals to mix is in the situation that do not change the variation that the weight stack size can realize weight stack weight, change the weight of weight stack by the variation of different densities weight sheet, to realize that not polishing in specie is for the requirement of weight flexible and changeablely.The effect of described the first double-screw bolt 2 is fixedly sample 4, thereby makes sample 4 and fixture together move; The effect of described the second double-screw bolt 7 is to prevent sample play Shang Xia 4, is used for simultaneously loading weight stack 3, and can coordinates with the first cylinder 1 the processing processing of completing different angles planes sample.
As shown in Figure 2, the number of the first double-screw bolt 2 is 4, is cross symmetric arrays setting in twos; The number of the second double-screw bolt 7 is 4, and being square is symmetrical arranged.
Secondly, the using method of described a kind of fixture for EBSD sample vibrations polishing is as follows:
One, the preparation of common sample
As shown in Figure 1, in figure, sample 4 is common sample, and the operating procedure of fixture is as follows:
(a), with sample 4 horizontal positioned, with the analysis that the needs processing polished placement that faces down, clip vertical is positioned over the top of sample 4, adjust the first double-screw bolt 2 and the second double-screw bolt 7, the space that makes the first double-screw bolt 2 and the second double-screw bolt 7 form is enough to hold sample 4;
(b), adjust the first double-screw bolts 2 by through hole 8, make the first double-screw bolt 2 from the side that sample 4 is fixing;
(c), adjust the second double-screw bolts 7 by through hole 8, make the second double-screw bolt 7 from the top, that sample 4 is fixing;
(d), sample 4 is polished and polishing;
(e), adjust the whole total amount of samples 4 and fixture by weight stack 3, make it satisfy the requirement of vibrations polishing;
(f), sample 4 is shaken polishing, make it reach the specimen surface state that meets EBSD analysis requirement;
(g), make required sample.
Two, the preparation of irregular small sample
As shown in Figure 3, in figure, sample 4 is irregular small sample, and the operating procedure of fixture is as follows:
(1), with sample 4 horizontal positioned, with the analysis that the needs processing polished placement that faces down, clip vertical is positioned over the top of sample 4, adjust the first double-screw bolt 2 and the second double-screw bolt 7, the space that makes the first double-screw bolt 2 and the second double-screw bolt 7 form is enough to hold sample 4;
(2), adjust the first double-screw bolts 2 by through hole 8, make the first double-screw bolt 2 from the side that sample 4 is fixing;
(3), adjust the second double-screw bolts 7 by through hole 8, make the second double-screw bolt 7 from the top, that sample 4 is fixing, at this moment, in the second double-screw bolt 7 position what same planes, but fit respectively at the upper surface of sample 4, as shown in Figure 3;
(4), the sample 4 in step (three) is polished and polishing, make sample 4 lower surfaces concordant with the lower surface of the second cylinder 6, as shown in Figure 4;
(5), after treatment sample 4 in step (four) is taken out, be inverted sample 4 and according to the fixing sample 4 of step (two) and step (three), as shown in Figure 5.
(6), the sample 4 in step (five) is polished and polishing, make sample 4 lower surface upper surfaces concordant, as shown in Figure 6;
(7), adjust the whole total amount of samples 4 and fixture by weight stack 3, make it satisfy the requirement of vibrations polishing;
(8), sample 4 described in step (six) is shaken polishing, make it reach the specimen surface state that meets EBSD analysis requirement;
(9), make required sample.
Three, the preparation of particular orientation sample
(A), determine the angle of the specimen surface that makes in described step (g) and crystal orientation by X-ray diffractometer;
(B), the second double-screw bolt described in set-up procedure (c), make that in step (g), prepared sample forms determined angle in step (A), as shown in Figure 7;
(C), repeat (four) in the preparation process of irregular small sample to (eight), thereby make required sample.
A kind of fixture for EBSD sample vibrations polishing that following table provides for the application of the invention is processed the sample that makes and the comparison that utilizes the sample after prior art processing is processed.
| Preparation time | The sample surfaces quality | The back scattering diffraction style | |
| The present invention | 30 minutes | Good | Clear |
| Comparative example | 1-2 working day | Relatively poor | Fuzzyyer |
The problem that the sample preparation difficult problem that adopts a kind of fixture for EBSD sample vibrations polishing provided by the present invention can effectively solve the back scattering diffraction sample to cause because size is less, the vibrations polishing effect that the shortage in weight problem causes are bad and the problem of specific orientation sample preparation.
Claims (10)
1. one kind is used for the fixture that the EBSD sample shakes polishing, and described fixture is used for clamping sample (4), it is characterized in that:
Described sample (4) is arranged at bottom the second cylinder (6),
Described the second cylinder (6) top is disposed with the first cylinder (1) and weight stack (3),
Be provided with the first double-screw bolt (2) in described sample (4) horizontal direction, described the first double-screw bolt (2) stretches into the second cylinder (6) inboard from the through hole (8) of the second cylinder (6) sidewall,
Be provided with the second double-screw bolt (7) in described sample (4) upper end vertical direction, described the second double-screw bolt (7) stretches into the second cylinder (6) inside from the through hole (8) of the second cylinder (6), the first cylinder (1) and weight stack (3).
2. a kind of fixture for EBSD sample vibrations polishing according to claim 1, it is characterized in that: the quantity of described the first double-screw bolt (2) is 4, the quantity of described the second double-screw bolt (7) is 4, described 4 the first double-screw bolts (2) are the cross setting, described 4 the second double-screw bolts (7) setting that is square.
3. a kind of fixture for EBSD sample vibrations polishing according to claim 1, it is characterized in that: described the second double-screw bolt (7) is provided with nut (5) at weight stack (3) one ends, and described through hole (8) is tapped through hole.
4. a kind of fixture for EBSD sample vibrations polishing according to claim 1, it is characterized in that: the diameter of described the first cylinder (1) is 25～35mm, the diameter of described the second cylinder (6) is 15～25mm.
5. according to claim 1 or 4 described a kind of fixtures for EBSD sample vibrations polishing, it is characterized in that: described the second cylinder (6) is hollow cylinder, and bottom opening.
6. a kind of fixture for EBSD sample vibrations polishing according to claim 1, it is characterized in that: described the first double-screw bolt (2), the second double-screw bolt (7), the first cylinder (1) and the second cylinder (6) select one or more low density metals to make, and described low density metals comprises aluminium, titanium, magnesium.
7. a kind of fixture for EBSD sample vibrations polishing according to claim 1, it is characterized in that: described weight stack (3) is processed by several metal mixed, and described metal comprises aluminium, iron and molybdenum.
8. the using method of the fixture for EBSD sample vibrations polishing as claimed in claim 1, with sample (4) horizontal positioned, the placed face down with needs processing is characterized in that, also comprises the steps:
(a), clip vertical is positioned over the top of sample (4);
(b), adjust the first double-screw bolt (2), make the first double-screw bolt (2) from the side that sample (4) is fixing;
(c), adjust the second double-screw bolt (7), make the second double-screw bolt (7) from the top, that sample (4) is fixing;
(d), sample (4) is polished and polishing;
(e), adjust the whole total amount of sample (4) and fixture by weight stack (3);
(f), sample (4) is shaken polishing;
(g), make required sample.
9. a kind of using method that shakes the fixture of polishing for the EBSD sample according to claim 8, is characterized in that, when sample (4) is irregular small sample, also comprises the steps:
(1), adjust the second double-screw bolt (7) described in described step (c), the second double-screw bolt (7) and sample (4) upper surface are fitted;
(2), adjust the first double-screw bolt (2) according to described step (b), make the first double-screw bolt (2) from the side that sample (4) is fixing;
(3), according to described step (d), sample (4) is polished and polishing, make sample (4) lower surface concordant with the first cylinder (1) lower surface;
(4), after treatment sample (4) in step (three) is taken out, be inverted sample (4) and according to the fixing sample (4) of step () and step (two);
(5), according to described step (d), the sample (4) in step (four) is polished and polishing, make sample (4) lower surface concordant with upper surface;
(6), according to described step (e) and step (f), the sample (4) that obtains after processing through step (five) is processed processing;
(7), make required sample.
10. according to claim 8 or 9 described a kind of usings method that shake the fixture of polishing for the EBSD sample, is characterized in that, when sample (4) is the particular orientation sample, also comprises the steps:
(A), determine the angle of the specimen surface that makes in described step (g) and crystal orientation by X-ray diffractometer;
(B), the second double-screw bolt (7) described in set-up procedure (c), make that in step (g), prepared sample forms determined angle in step (A);
(C), repeating step (three) is to step (six), makes required sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103796438A CN103128657A (en) | 2011-11-24 | 2011-11-24 | Clamp used for electron back scattering diffraction sample vibration polishing and use method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103796438A CN103128657A (en) | 2011-11-24 | 2011-11-24 | Clamp used for electron back scattering diffraction sample vibration polishing and use method thereof |
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| CN103128657A true CN103128657A (en) | 2013-06-05 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103926263A (en) * | 2014-04-09 | 2014-07-16 | 北京工业大学 | Method for researching alloy baseband recrystallization and cubic texture forming mechanisms through quasi in-situ electron back scattered diffraction (EBSD) technology |
| CN104209844A (en) * | 2014-08-08 | 2014-12-17 | 安徽昱工耐磨材料科技有限公司 | Cutting machine |
| CN106813966A (en) * | 2015-12-01 | 2017-06-09 | 上海梅山钢铁股份有限公司 | A kind of EBSD analysis preparation method of low-carbon (LC) steel sample |
| CN107907406A (en) * | 2017-12-26 | 2018-04-13 | 郑州大学 | A kind of multilayer round platform delamination fixture based on electrochemical polish |
| CN108007862A (en) * | 2016-10-31 | 2018-05-08 | 中国石油化工股份有限公司 | Sheet metal specimens fixture for direct reading spectrometry |
| CN110712129A (en) * | 2019-11-13 | 2020-01-21 | 核工业理化工程研究院 | Auxiliary clamp for mechanical vibration polishing sample |
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| CN103926263A (en) * | 2014-04-09 | 2014-07-16 | 北京工业大学 | Method for researching alloy baseband recrystallization and cubic texture forming mechanisms through quasi in-situ electron back scattered diffraction (EBSD) technology |
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| CN106813966A (en) * | 2015-12-01 | 2017-06-09 | 上海梅山钢铁股份有限公司 | A kind of EBSD analysis preparation method of low-carbon (LC) steel sample |
| CN108007862A (en) * | 2016-10-31 | 2018-05-08 | 中国石油化工股份有限公司 | Sheet metal specimens fixture for direct reading spectrometry |
| CN107907406A (en) * | 2017-12-26 | 2018-04-13 | 郑州大学 | A kind of multilayer round platform delamination fixture based on electrochemical polish |
| CN110712129A (en) * | 2019-11-13 | 2020-01-21 | 核工业理化工程研究院 | Auxiliary clamp for mechanical vibration polishing sample |
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