CN105004588A - Alloy-galvanized layer scanning electron microscope sectioned sample precision making method - Google Patents
Alloy-galvanized layer scanning electron microscope sectioned sample precision making method Download PDFInfo
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Abstract
The invention discloses an alloy-galvanized layer scanning electron microscope sectioned sample precision making method and belongs to the technical field of alloy-galvanized layer section scanning electron microscope analysis. The method comprises cutting an observation sample and an edge-preserving sample, carrying out ultrasonic cleaning on the observation sample and the edge-preserving sample by acetone, coating the observation sample and the edge-preserving sample with 502 glue, carrying out sequential superposition bonding, wherein the edge-preserving sample is used as an outer layer and the observation sample is used as an inner layer, and carrying out cold insertion, grinding and polishing, etching and carbon spraying treatment on the bonded sample. The method retains a loose structure, defects, holes and cracks at the outermost surface of the alloy-galvanized layer and prevents novel defects and false appearance produced in sample preparation.
Description
Technical field
The invention belongs to Alloy Plating zinc layers cross-sectional scans electrical microscope analysis field, particularly the accurate method for making sample of a kind of alloying zinc coat scanning electron microscope cross-section samples.
Background technology
GA plate zinc-iron alloy is higher than hot galvanized layer corrosion stability, and alloying Several Thiourea Derivatives on Zinc Plate Surface loosens and tiny holes substantially increases coating performance, and a small amount of zinc in surface and open structure decrease hot melt district during welding, decrease the damage of welding to coating.Alloying zinc coat may contain Γ phase, Γ 1 phase, δ phase, ζ phase and η pure zinc layer.It is used that surface porosity structure also serves certain protection in the packaging of product and the friction of transportation and collision process.The adhesion properties such as zinc coat efflorescence and stripping and surface porosity phase structure have very large relation.So the phase structure characteristic on alloying zinc coat outermost top layer plays very important effect to whole alloying zinc coat performance judgment.In sample preparation, the zinc-plated outermost loose phase structure of complete reservation is priority and difficulty.Distinguish the preparation method that the defect produced in the original defect of alloying zinc coat and preparation process needs coating precision in addition.At present, alloying zinc coat preparation method of sample generally takes superposition to inlay or centre adds conducting resinl, and Baoshan Iron & Steel Co., Ltd Zhang Li to raise etc. and takes conducting resinl to paste in the article and proprietary alloy heat-transmission galvanized coatings analytical approach (CN 1525167A) delivered to inlay sample preparation.In the method, the outermost δ phase of alloying zinc coat, ζ phase and η pure zinc layer open structure or space are difficult to real reservation first.So a kind of complete real reservation alloying zinc coat phase structure of exploitation, outermost open structure, defect, space and crackle are extremely important.
Summary of the invention
The object of the present invention is to provide the accurate method for making sample of a kind of alloying zinc coat scanning electron microscope cross-section samples, to solve in sample making course can not complete real reservation alloying zinc coat phase structure, outermost open structure, defect, space and crack problem.
Concrete technology step of the present invention and parameter as follows:
1, cut sample: bulk specimen is cut into 30mm-60mm square on plate shearing machine, according to cold embedding die size, cut observation sample with precision gas cutting machine; Cut and do outermost layer with the hot rolled plate observing sample same size and protect limit sample, sample ensures coating not damaged in cutting and preservation process, without bending;
2, washed samples: will observe sample and Bao Bian sample acetone Ultrasonic Cleaning, ensures that surface and surface void are totally without oil stain.
3, sample is pasted: observation sample and Bao Bian sample are placed in the cold pointing machine of vacuum, repeatedly vacuumize three times, vacuum tightness is greater than 4Ba, first on the sample sticking veneer of guarantor limit, be coated with 502 glue, on observation sample, be coated with 502 glue again, superpose stickup successively, outer for protecting limit sample, internal layer is for observing sample, with hand press several under, more repeatedly vacuumize three times, vacuum tightness is greater than 4Ba, the empty 20-30 minute of fidelity, sample just pastes completely; Under the effect of pressing and when repeatedly vacuumizing, 502 glue can be impregnated in the open structure of vacuum state, cavity, crackle and defect and solidify, thus play the complete real structure of protective coating, also to ensure in sample preparation not round edge.
4, coldly to inlay: the sample pasted carries out cold inlaying, cold gross thickness of observing sample and Bao Bian sample when inlaying is no more than cold half of inlaying sample thickness.
5, grinding and polishing: use 220#, 500#, 1000# and 2000# sand paper to add water on abrasive disk grinding successively, last alcohol washes, polishing disk carries out polishing with alcohol; Sample is observed and rotating disk angle is 30-45 degree, lap speed 800-1000 rev/min in grinding and polishing process; Polishing cloth is first spread thick layer canvas, and add flannelette, other polished steel samples of flannelette flatten fine hair, and polishing time is 2-4 minute.
6, etch: be that under the nitric acid alcohol wipe 10-15 of 0.3-0.5%, often descend the wiping time to be 1 second, the solution in wiping process on absorbent cotton can not be too much by mass percent, avoid making sample become immersion type etch; Tiltedly dry up along sample direction with cold wind.
7, carbon is sprayed: the process of spray carbon is carried out to polished sample; Inlaying agent because cold and 502 glue are all non-conductive, should carbon be sprayed to obtain better image effect.
The invention has the advantages that: not only alloying zinc coat outmost surface open structure, defect, hole and crackle are remained, can also avoid producing new defect and illusion in sample making course.
Accompanying drawing explanation
Fig. 1 is the complete pattern in DX53D+Z alloying zinc coat cross section.
Fig. 2 is the outer open structure pattern in DX53D+Z alloying zinc coat cross section.
Fig. 3 is the original cavity of DX53D+Z alloying zinc coat.
Fig. 4 is that in DX53D+Z alloying zinc coat preparation process, coating comes off.
Fig. 5 is the thick ζ phase morphology of DX53D+Z alloying zinc coat outermost layer.
Fig. 6 is DX54D+Z alloying zinc coat crackle.
Fig. 7 is the tiny δ phase of DX54D+Z alloying zinc coat outermost layer.
Embodiment
Embodiment 1:
Choose two kinds of alloyed hot-dip plates, be numbered 1# and 2#, the preparation of alloyed zinc layer cross section scanning electron microscope delicate specimens:
1, length of side 25mm, thickness is 0.6mm alloying galvanizing plate, cuts each two samples of 15mm × 15mm, then to cut same size thickness be that the hot rolled plate of 2mm does outermost layer and protects limit sample.
2, washed samples: will observe sample and Bao Bian sample acetone Ultrasonic Cleaning, ensures that surface and surface void are totally without oil stain.
3,502 glue filling sample spaces and stickup sample: all samples are placed in the cold pointing machine of vacuum and repeatedly vacuumize three times; first on protection sample sticking veneer, be coated with 502 glue; again observation sample is coated with 502 glue; superpose stickup successively, finally another protection sample paste on, with hand press several under; repeatedly vacuumize three times again; vacuum tightness is 4Ba, and to have taken out after vacuum fidelity for the last time empty 30 minutes, sample just pastes completely.
4, coldly to inlay: the sample pasted carries out cold inlaying, coldly observe sample whole thickness about 6.5mm when inlaying, be no more than the half of whole sample thickness.
5, grinding and polishing: use 220#, 500#, 1000# and 2000# sand paper to add water on abrasive disk grinding successively, last alcohol washes, polishing disk carries out polishing with alcohol; Grinding and polishing process observation sample layer and rotating disk add miter angle, lap speed 1000 revs/min; Polishing disk rotating speed is 800 revs/min.Polishing time is 3 minutes.
6, etch: be the nitric acid alcohol wipe 12 times of 0.3% by mass percent, the time is 12 seconds; Tiltedly dry up along sample direction with cold wind.
7, carbon is sprayed: the process of spray carbon is carried out to polished sample.
Use scanning electron microscopic observation sample:
Sample tungsten filament scanning electron microscopic observation, 1# alloying zinc coat cross section phase structure as Figure 1-Figure 5.Fig. 1 is the complete shape appearance figure of 1# alloying zinc coat cross section low power; Fig. 2 shows alloying zinc coat cross section outermost layer thick ζ phase open structure and retains very complete, and uneven Г phase, δ phase and the ζ phase of alloying zinc coat is all complete clear, and this sample is without Г 1 phase; Fig. 3 is original cavity in zinc coat, is filled with 502 glue in cavity, and empty place is thinner zinc layers because surface has, so plating leakage is herein because surface does not have hesive problem.Zinc liquid itself may cause containing snotter or cadmia, and coating comes off in the diagram on the contrary, and the place that comes off is empty, does not have 502 glue; Illustrate that defect is not original herein, but produce in sample preparation.Zinc layers outermost layer list props up thick ζ phase and also retains very complete in Figure 5.If such phase structure is many, easily come off in production and transportation, call in zinc liquid and form generation scratch in bits or transportation.As Figure 6-Figure 7, Fig. 6 is 2# alloying zinc coat original crack pattern to 2# alloying zinc coat cross section phase structure, and crackle is along phase crystal boundary, from coarse to fine, is not orthogonal to specimen surface.Fig. 7 shows zinc coat outermost layer tiny δ phase and retains complete too.
Claims (2)
1. the accurate method for making sample of alloying zinc coat scanning electron microscope cross-section samples, is characterized in that, concrete technology step and parameter as follows:
1) cut sample: bulk specimen is cut into 30mm-60mm square on plate shearing machine, according to cold embedding die size, cut observation sample with precision gas cutting machine; Cut and do outermost layer with the hot rolled plate observing sample same size and protect limit sample, sample ensures coating not damaged in cutting and preservation process, without bending;
2) washed samples: sample and Bao Bian sample acetone Ultrasonic Cleaning will be observed;
3) sample is pasted: observation sample and Bao Bian sample are placed in the cold pointing machine of vacuum, repeatedly vacuumize three times, vacuum tightness is greater than 4Ba, first on the sample sticking veneer of guarantor limit, be coated with 502 glue, then be coated with 502 glue on observation sample, superpose stickup successively, outer for protecting limit sample, internal layer is for observing sample; With hand press several under, more repeatedly vacuumize three times, vacuum tightness is greater than 4Ba, the empty 20-30 minute of fidelity, and sample just pastes completely;
4) coldly to inlay: the sample pasted carries out cold inlaying, cold gross thickness of observing sample and Bao Bian sample when inlaying is no more than cold half of inlaying sample thickness;
5) grinding and polishing: use 220#, 500#, 1000# and 2000# sand paper to add water on abrasive disk grinding successively, last alcohol washes, polishing disk carries out polishing with alcohol;
6) etch: be that under the nitric acid alcohol wipe 10-15 of 0.3-0.5%, often descend the wiping time to be 1 second, the solution in wiping process on absorbent cotton can not be too much by mass percent, avoid making sample become immersion type etch; Tiltedly dry up along sample direction with cold wind;
7) carbon is sprayed: the process of spray carbon is carried out to polished sample.
2. method according to claim 1, is characterized in that, step 5) grinding and polishing process in observe sample and rotating disk angle is 30-45 degree, lap speed 800-1000 rev/min; Polishing cloth is first spread thick layer canvas, and add flannelette, other polished steel samples of flannelette flatten fine hair, and polishing time is 2-4 minute.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105259002A (en) * | 2015-11-16 | 2016-01-20 | 武汉科技大学 | Preparation method of high-magnetic-induction grain-oriented silicon steel EBSD samples |
| CN105300777A (en) * | 2015-11-13 | 2016-02-03 | 广西玉柴机器股份有限公司 | Metallographic specimen and hardness specimen embedding method |
| CN108362233A (en) * | 2018-01-29 | 2018-08-03 | 中国第汽车股份有限公司 | A kind of detection method of micro hole roughness |
| CN109448878A (en) * | 2018-11-13 | 2019-03-08 | 中国核动力研究设计院 | The vacuum mosaic technology of sample after a kind of irradiation |
| CN109633209A (en) * | 2019-01-31 | 2019-04-16 | 长江存储科技有限责任公司 | Test sample and preparation method thereof |
| CN110057994A (en) * | 2019-05-05 | 2019-07-26 | 南通市产品质量监督检验所 | A kind of metallographic method identification steel product electrogalvanizing and hot galvanizing test method |
| CN113701702A (en) * | 2021-08-11 | 2021-11-26 | 山东钢铁集团日照有限公司 | Pre-forming sample preparation method for evaluating corrugation degree of floating-coating-free automobile panel |
| CN115876819A (en) * | 2023-03-03 | 2023-03-31 | 中国电建集团山东电力建设第一工程有限公司 | Cold inlaying method for preparing porous metallographic specimen for SEM by adding carbon fibers |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105300777A (en) * | 2015-11-13 | 2016-02-03 | 广西玉柴机器股份有限公司 | Metallographic specimen and hardness specimen embedding method |
| CN105259002A (en) * | 2015-11-16 | 2016-01-20 | 武汉科技大学 | Preparation method of high-magnetic-induction grain-oriented silicon steel EBSD samples |
| CN105259002B (en) * | 2015-11-16 | 2018-03-13 | 武汉科技大学 | A kind of preparation method of high magnetic induction grain-oriented silicon steel EBSD samples |
| CN108362233A (en) * | 2018-01-29 | 2018-08-03 | 中国第汽车股份有限公司 | A kind of detection method of micro hole roughness |
| CN109448878A (en) * | 2018-11-13 | 2019-03-08 | 中国核动力研究设计院 | The vacuum mosaic technology of sample after a kind of irradiation |
| CN109448878B (en) * | 2018-11-13 | 2020-05-05 | 中国核动力研究设计院 | Vacuum inlaying process for irradiated sample |
| CN109633209A (en) * | 2019-01-31 | 2019-04-16 | 长江存储科技有限责任公司 | Test sample and preparation method thereof |
| CN110057994A (en) * | 2019-05-05 | 2019-07-26 | 南通市产品质量监督检验所 | A kind of metallographic method identification steel product electrogalvanizing and hot galvanizing test method |
| CN113701702A (en) * | 2021-08-11 | 2021-11-26 | 山东钢铁集团日照有限公司 | Pre-forming sample preparation method for evaluating corrugation degree of floating-coating-free automobile panel |
| CN115876819A (en) * | 2023-03-03 | 2023-03-31 | 中国电建集团山东电力建设第一工程有限公司 | Cold inlaying method for preparing porous metallographic specimen for SEM by adding carbon fibers |
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Application publication date: 20151028 |