CN105300761B - The preparation method of the double membrane samples that gush of TEM electrolysis of small sized metallic material - Google Patents
The preparation method of the double membrane samples that gush of TEM electrolysis of small sized metallic material Download PDFInfo
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- CN105300761B CN105300761B CN201510671024.4A CN201510671024A CN105300761B CN 105300761 B CN105300761 B CN 105300761B CN 201510671024 A CN201510671024 A CN 201510671024A CN 105300761 B CN105300761 B CN 105300761B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000005868 electrolysis reaction Methods 0.000 title claims abstract description 23
- 239000012528 membrane Substances 0.000 title claims abstract description 14
- 239000007769 metal material Substances 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 21
- 229910000851 Alloy steel Inorganic materials 0.000 claims abstract description 10
- 229910001209 Low-carbon steel Inorganic materials 0.000 claims abstract description 9
- 244000137852 Petrea volubilis Species 0.000 claims abstract description 9
- 238000012360 testing method Methods 0.000 claims abstract description 9
- 238000007796 conventional method Methods 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 9
- 239000000956 alloy Substances 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- 239000010959 steel Substances 0.000 claims description 9
- 229910045601 alloy Inorganic materials 0.000 claims description 7
- 229910000976 Electrical steel Inorganic materials 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 238000004026 adhesive bonding Methods 0.000 claims description 3
- 238000002788 crimping Methods 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 2
- 238000005498 polishing Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 7
- 239000003638 chemical reducing agent Substances 0.000 abstract description 5
- 238000006722 reduction reaction Methods 0.000 abstract description 5
- 239000000523 sample Substances 0.000 description 46
- 239000007921 spray Substances 0.000 description 15
- 239000010408 film Substances 0.000 description 14
- 230000005540 biological transmission Effects 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 7
- 229910001004 magnetic alloy Inorganic materials 0.000 description 7
- 238000000992 sputter etching Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000010977 jade Substances 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- BMTLETAJHZZUPD-UHFFFAOYSA-N chloric acid;ethanol Chemical compound CCO.OCl(=O)=O BMTLETAJHZZUPD-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 238000007430 reference method Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a kind of preparation method of the double membrane samples that gush of the TEM of small sized metallic material electrolysis, this method comprises the following steps：1) low-carbon and low-alloy steel material surface is polished with 400~No. 1200 sand paper, then with HF and H2O2Mixed solution carry out chemical reduction, overall diameter is 3mm, diameter of bore is slightly less than the disk on the narrow side of test button and polishes through being washed into perforating press, and pad is prepared；2) test button of the size less than 2.5mm is milled into thickness to paste on pad to 50~80 μm, ensures the covering whole endoporus of pad, then carried out twin-jet electropolishing according to a conventional method and be thinned, you can the double membrane samples that gush of TEM electrolysis are prepared.The inventive method has advantages below：1) the sample preparation time is short, structure observation effect is good；2) it is pollution-free to sample in sample thinning process；3) pad makes simple, does not influence the electric conductivity of sample, and polishing effect is good.
Description
Technical field
The invention belongs to transmission electron microscope (TEM) sample preparation technology field, and in particular to a kind of small sized metallic material
The preparation method of the double membrane samples that gush of TEM electrolysis.
Background technology
With the development of modern science and technology and industrial level, higher requirement it is also proposed to the performance of steel, and steel
Many performances of iron are all decided by nanometer or Geng little range scales inner tissue substructure, such as sub boundary and interfacial structure, dislocation
Etc. various crystal defects, separate out distributed mutually and state etc. so that transmission electron microscope analysis turns into micro-structural point in ferrous materials research
The main method of analysis.But be commonly encountered when in real work because ferrous materials size (width or diameter) is too small, it can not prepare
Into qualified transmission electron microscope film sample.In below 2mm, some failures zero the steel cord diameter produced such as recent years
For part size also below 2.5mm, the preparation to film sample adds difficulty.
For metal material, the preparation method of transmission electron microscope film sample is：Pass through mechanical lapping or chemical reduction to 60
~80 μm, then be electrolysed double sprays and be thinned and ion milling, obtain below 300nm thin area.In real work, generally use
The double spray thining methods of electrolysis, its thinned speed is fast, is usually no more than 1 minute, and the thin area of sample is big；Because belonging to of this method
Corrosion thinning is learned, is had differences so speed is thinned in heterogeneity or sub-structure so that crystal boundary, sub boundary, phase in tissue
Boundary is relatively thin, and carbide etc. second compares thickness, is speculated so as to add tissue, and observing effect is good；But shortcoming be sample diameter or
Width dimensions cannot be below 2.5mm, because setting Φ 3mm circular pits in twin-jet electropolishing instrument specimen holder, internal aperture is
2.4mm.The advantages of ion milling is to be limited by sample size smaller, can partly make up the shortcomings that double sprays of electrolysis are thinned, but it subtracts
Thin speed is very slow, it usually needs 4~8 hours, because not perforating warning function, such as perforation was not found in time, the time
Slightly long Jian Haobao areas can be disposed by ion beam again；And the tissue of sample is speculated poor, is unfavorable for small angle in metal material
Spend the observation analysis of substructure tissue.Ion milling is relatively applied to the preparation of inorganic non-metallic (such as ceramics) sample.So for
Width less than 2.5mm metal material or diameter be less than 2.5mm wire rod, want quickly to obtain preferable film sample, it is necessary to
It is a kind of to be suitable for being electrolysed the thinned film sample preparation method of double sprays.
Through being retrieved in relevant bibliographic data base, finding the document stronger with research contents correlation of the present invention altogether has 4：
Hao Jingli；Bring up Xinhua；Meng Yang；The side of double spray detailed information silk longitudinal sections transmission electron microscope film sample is electrolysed Deng Capital Iron ＆ Steel General Co
Method application numbers:CN201310218516.9. (referred to as " document 1 "), Xie Xuezhi；Double sprays electricity of Zhou Zhilan bearing steel metallic films
Solution polishing technology of preparing .1983:29-32+63. (referred to as " document 2 "), Ye Yun；Li Qiao tinkling of pieces of jade Nanocrystalline Two-phase RE permanent magnetic alloys
The preparation .1999 of transmission electron microscope film sample:181-183. (referred to as " document 3 "), Ye Yun；Li Qiao tinkling of pieces of jade electrobrightenings and ion
Thinning method, which is combined, prepares Nanocrystalline Two-phase RE permanent magnetic alloy TEM sample .2002:840~841. (referred to as " document 4 ").Pass through
Looked into pertinent literature is read, analysis, obtained a result as follows：
In above-mentioned pertinent literature, document 1 discloses a kind of double spray detailed information silk longitudinal section transmission electron microscope film samples of electrolysis
The method of product：Sample is cut, ground, is clamped, line, the double sprays of electrolysis is adjusted and cleans, sample is prepared and finished；Utilize electricity
Xie Shuan, which sprays method and diameter 3.0mm aperture samples folder, realizes the successful preparation of diameter 1.0mm filament samples longitudinal section film, this
Kind method for making sample reduces the use of part sample making apparatus, reduces cost, improves sample preparation efficiency and success rate.But the document
In disclosed technical scheme, specimen holder comparison is complicated, and the physical property such as the electric conductivity of clamp material, corrosion resistance may
Influence polishing effect.Because the influence factor of twin-jet electropolishing polishing is a lot, electrolyte component, temperature, voltage x current value and sample
Material itself and its physical state are all interrelated.
Document 2 describes the method that bearing steel metallic film is prepared using twin-jet electropolishing polishing.To experimental provision, sample preparation
The selection of journey, electrolytic polishing process is inquired into, and the observation of diffraction image has been carried out to the martensite substructure in bearing steel
With light field, details in a play not acted out on stage, but told through dialogues, the analysis of SEAD.Using metallic film made from the method for twin-jet electropolishing polishing, due to center
Perforation nearby has sizable transmission area, and surrounding leaves thick edge, has rigidity well, is cut into a diameter of 3mm
Disk after, it is not necessary to wire netting support, electron microscopic observation can be directly placed into, thus visual field selection not by wire netting grid
Limitation.But in technical scheme disclosed in the document, specimen size is needed for Φ 3mm, and 2.5mm gold is less than for diameter or width
Belong to material, can not equally be detected.
Document 3 has inquired into Nanocrystalline Two-phase RE permanent magnetic alloy in PTFE fixture disk polishing processes and in Ion Milling Technique In The Microstructure Study
In electron microscope film sample preparation, explore preferably for transmission electron microscope observing analysis Nanocrystalline Two-phase rare earth permanent magnet close
The double sprays of the preparation method of gold thin film sample, i.e. electrolysis plus Ion Milling Technique In The Microstructure Study.Electrolysis is thrown used by document 4 describes document 3
Light and ion thinning method combine that to prepare the experimental method of Nanocrystalline Two-phase RE permanent magnetic alloy TEM sample be feasible, this method
It is not only effective to preparing Nanocrystalline Two-phase RE permanent magnetic alloy, to solving analyzed material when its width is less than 3mm, also should
It is one of reference method of highly effective preparation TEM sample., may due to impact of the twin-jet electropolishing liquid to analysis sample surfaces
It can cause chipping because of Nanocrystalline Two-phase RE permanent magnetic alloy sample fragility, cause to make Nanocrystalline Two-phase rare earth permanent magnet and close
Golden TEM products failure.Therefore, when be electrolysed double sprays, make twin-jet electropolishing flow velocity as on the low side as possible, be just advantageous to keep
Nanocrystalline Two-phase RE permanent magnetic alloy sample surfaces are not impacted and fragmentation by electrolyte.In the scheme of document 3 and document 4, electrolysis
It is double spray for ion milling before it is pre- be thinned, it is still available when Sample Width is between 2.5mm~3mm, but when sample is wide
Not directly double sprays when spending for 2.5mm or less than 2.5mm.Because twin-jet electropolishing instrument can be automatic after certain luminous flux is reached
It is stopped.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of double membrane samples that gush of TEM electrolysis of small sized metallic material
Preparation method, with to diameter less than 2.5mm wire rod and width less than 2.5mm metal material carry out sample preparation, meet electrolysis
Requirement of double spray methods to transmission electron microscope film sample.
In order to solve the above technical problems, the technical scheme that the present invention designs comprises the following steps：
1) pad is prepared：
Low-carbon and low-alloy steel material surface is polished with 400~No. 1200 sand paper, then with HF and H2O2Mixed solution carry out
Chemical reduction, until be thinned to 50~80 μm, with perforating press be washed into overall diameter be 3mm, diameter of bore be less than the narrow side of test button
Disk, then the crimping of disk is polished with 800~No. 1200 sand paper, that is, low-carbon and low-alloy pad is prepared；It is described low
The weight percent content of the carbon of carbon and low-alloy Steel material is less than 0.3%, and the weight percent content of alloy is less than 5%.
2) small sized metallic sample is milled into thickness to paste on pad to 50~80 μm, ensures that covering pad is entirely interior
Hole, i.e., specimen size is successfully extended to a diameter of 3mm, then carries out twin-jet electropolishing according to a conventional method and be thinned, you can be prepared into
To the double membrane samples that gush of TEM electrolysis；The size of the small sized metallic sample is less than 2.5mm.
Further, in the step 1), low-carbon and low-alloy material is silicon steel material or thin steel sheet for automobile material.
Further, in the step 1), the thickness of low-carbon and low-alloy material is 0.2~0.35mm.
Further, in the step 2), test button and pad of the size less than 2.5mm by low melt point paraffin or
502 gluing stick together.
The method that the present invention prepares the double membrane samples that gush of TEM electrolysis of metal material of the size less than 2.5mm, has following
Advantage：
1) small sample is extended to after Φ 3mm by the present invention meets that sample requirement is thinned in the double sprays of electrolysis, substantially reduces
Sample preparation time, structure observation effect are good；
2) in sample thinning process, sample pad, which plays, to be in the light and supporting role, can be thinned on a small quantity, relative to copper ring
Material, the low-carbon and low-alloy Steel material as pad is pollution-free to sample, and the low-carbon and low-alloy such as silicon steel material is big product
Kind, can be tested more than sample carry out twice laid；
3) single hole sample pad prepared by the inventive method makes simple, does not influence the electric conductivity of sample, and polishing effect is good
It is good.
Embodiment
Technical scheme designed by the present invention comprises the following steps：
1) pad is prepared：
Low-carbon and low-alloy steel material surface is polished with 400~No. 1200 sand paper, then with HF and H2O2Mixed solution carry out
Chemical reduction, until be thinned to 50~80 μm, with perforating press be washed into overall diameter be 3mm, diameter of bore be less than the narrow side of test button
Disk, then caused crimping in preparation process is polished with 800~No. 1200 sand paper, that is, low-carbon and low-alloy pad is prepared
Piece；The weight percent content of the carbon of the low-carbon and low-alloy Steel material is less than 0.3%, and the weight percent content of alloy is less than
5%.
2) test button of the size less than 2.5mm is milled into pasting on pad when thickness is 50~80 μm, ensures to cover
The whole endoporus of lid gasket, i.e., be successfully extended to a diameter of 3mm by specimen size, and then (electrolyte is 10% high according to a conventional method
Chloric acid ethanol solution or 10% perchloric acid glacial acetic acid solution) carry out twin-jet electropolishing and be thinned, you can it is prepared that TEM electrolysis are double to gush
Membrane sample.
In the embodiment of the present invention, single hole sample pad is prepared using the thick silicon steel plates of 0.3mm, prepared by pad
Method is：Chemical reduction is carried out by silicon steel plate surface rubbing, then with HF and H2O2 solution with No. 800 sand paper, until being thinned to
70 μm, it is disks of the 3mm with endoporus to be washed into overall diameter with perforating press, then with No. 1000 sand paper by caused volume in preparation process
While polishing, that is, obtain pad.Disk diameter of bore should be less than the narrow side of test button, it is generally the case that disk endoporus aperture more with
The narrow hem width degree of metallographictest approaches, and sample preparation effect and Detection results will be better.
Then, by size less than 2.5mm test button be milled into 60 μm by 502 it is gluing be attached on pad, ensure to cover
The whole endoporus of lid gasket, i.e., be successfully extended to Φ 3mm by specimen size, then carries out twin-jet electropolishing according to a conventional method and is thinned.
The thin area of sample prepared by this method is big, speculates, when being detected, it was observed that sub-structure such as sub boundary,
Twin, dislocation, nanoscale separate out equal pattern and become apparent from.
Claims (4)
- A kind of 1. preparation method of the double membrane samples that gush of TEM electrolysis of small sized metallic material, it is characterised in that：This method includes Following steps：1) pad is prepared：Low-carbon and low-alloy steel material surface is polished with 400~No. 1200 sand paper, then with HF and H2O2Mixed solution carry out chemistry Be thinned, until be thinned to 50~80 μm, with perforating press be washed into overall diameter be 3mm, diameter of bore be less than the circle on the narrow side of test button Piece, then caused crimping in preparation process is polished with 800~No. 1200 sand paper, that is, low-carbon and low-alloy pad is prepared； The weight percent content of the carbon of the low-carbon and low-alloy Steel material is less than 0.3%, and the weight percent content of alloy is less than 5%；2) small sized metallic sample is milled into thickness to paste on pad to 50~80 μm, ensures the covering whole endoporus of pad, Specimen size is successfully extended to a diameter of 3mm, twin-jet electropolishing is then carried out according to a conventional method and is thinned, you can be prepared The double membrane samples that gush of TEM electrolysis；The size of the small sized metallic sample is less than 2.5mm.
- 2. the preparation method of the double membrane samples that gush of TEM electrolysis of small sized metallic material according to claim 1, its feature It is：In the step 1), low-carbon and low-alloy Steel material is silicon steel material or thin steel sheet for automobile material.
- 3. the preparation method of the double membrane samples that gush of TEM electrolysis of small sized metallic material according to claim 1 or 2, its It is characterised by：In the step 1), the thickness of low-carbon and low-alloy Steel material is 0.2~0.35mm.
- 4. the preparation method of the double membrane samples that gush of TEM electrolysis of small sized metallic material according to claim 1 or 2, its It is characterised by：In the step 2), small sized metallic sample sticks together with pad by the way that low melt point paraffin or 502 are gluing.
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| CN109298000A (en) * | 2018-11-19 | 2019-02-01 | 重庆大学 | A kind of transmission electron microscope sample preparation method based on template auxiliary |
| CN109682848A (en) * | 2018-12-29 | 2019-04-26 | 国合通用测试评价认证股份公司 | A kind of preparation method of the transmissive film sample of Mg-RE-Zn system magnesium alloy |
| CN111982643B (en) * | 2020-07-10 | 2022-07-12 | 安徽工程大学 | Preparation method of transmission electron microscope sample of metal material surface deformation layer |
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| JP2001289752A (en) * | 2000-04-07 | 2001-10-19 | Nippon Steel Corp | Magnetic material sample preparation method for transmission electron microscope observation |
| JP3711018B2 (en) * | 2000-12-06 | 2005-10-26 | エスアイアイ・ナノテクノロジー株式会社 | TEM sample thinning method |
| CN101509848B (en) * | 2009-03-23 | 2011-07-20 | 大连交通大学 | Method for producing Transmission electron microscopy sample with surface layer high residual stress example cross section |
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