CN107402146A - Preparation method of hot-dip coating section transmission sample - Google Patents
Preparation method of hot-dip coating section transmission sample Download PDFInfo
- Publication number
- CN107402146A CN107402146A CN201610329644.4A CN201610329644A CN107402146A CN 107402146 A CN107402146 A CN 107402146A CN 201610329644 A CN201610329644 A CN 201610329644A CN 107402146 A CN107402146 A CN 107402146A
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- hot
- steel plates
- preparation
- dip
- steel
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- 230000005540 biological transmission Effects 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000003618 dip coating Methods 0.000 title abstract description 6
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 59
- 239000010959 steel Substances 0.000 claims abstract description 59
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000007747 plating Methods 0.000 claims abstract description 13
- 238000005520 cutting process Methods 0.000 claims abstract description 11
- 238000005246 galvanizing Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 230000008569 process Effects 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 11
- 238000000992 sputter etching Methods 0.000 claims description 8
- 238000002474 experimental method Methods 0.000 claims description 7
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- 238000011017 operating method Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000005272 metallurgy Methods 0.000 claims 1
- 238000009739 binding Methods 0.000 abstract description 3
- 230000027455 binding Effects 0.000 abstract description 3
- 241001391944 Commicarpus scandens Species 0.000 abstract description 2
- 238000007598 dipping method Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 35
- 239000011248 coating agent Substances 0.000 description 12
- 238000000576 coating method Methods 0.000 description 12
- 239000000758 substrate Substances 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 8
- 229910052725 zinc Inorganic materials 0.000 description 8
- 239000011701 zinc Substances 0.000 description 8
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 239000003292 glue Substances 0.000 description 5
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect 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
- 238000007654 immersion Methods 0.000 description 2
- 125000006850 spacer group Chemical group 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000005269 aluminizing Methods 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- -1 zinc-aluminum-magnesium Chemical compound 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Coating With Molten Metal (AREA)
Abstract
The invention discloses a method for preparing a transmission sample of a hot-dip coating section, which comprises the steps of selecting two steel plates, respectively processing a plurality of holes on the surfaces of the two steel plates, overlapping and fixing the two steel plates together with a gasket, forming a gap between the two steel plates, putting the fixed steel plates into a hot-dip galvanizing simulator for a hot-dip coating test, starting a stirrer in a hot-dip galvanizing pot, enabling a plating solution to smoothly flow into a plate gap, solidifying the plating solution in the gap in a subsequent cooling section, enabling the two steel plates to form metallurgical bonding, carrying out linear cutting on the edge of the hole along the cross section of the plate, and grinding and ion thinning to obtain a thin-region transmission electron microscope observation sample. According to the invention, the two steel plates are metallurgically combined together through the steel plate surface processing and hot dipping process, so that the binding force of the steel plates is greatly improved, the steel plates are not easy to break in the subsequent grinding and ion thinning processes, the success rate of the preparation of the transmission sample of the section of the hot-dip coating is effectively improved, and a more accurate and excellent thin area can be obtained.
Description
Technical field
The invention belongs to sample analysis field of measuring technique, more particularly to a kind of preparation of hot-dip coated cross-sectional Transmission sample
Method
Background technology
It is hot-dip coated that there is excellent anti-corrosion barrier propterty, it is used widely in fields such as building, automobile, household electrical appliances,
With scientific and technological progress and the raising of product requirement (performance, environmental-protecting performance etc.), various novel hot-dip coating are increasingly developed
Out, such as galvanneal coating, zinc-aluminum-magnesium coating.Therefore need more accurately to understand hot-dip coated architectural feature, especially
Be it is hot-dip coated combined with substrate after tissue, shape characteristic and layer/base junction the characteristics of closing, i.e., it is hot-dip coated to be tied between substrate
Whether conjunction is firm, whether can play a part of excellent protective substrate.
The sophisticated equipments such as current scanline Electronic Speculum, electron probe have turned into the advanced meanses of detection coating, but its multiplication factor
It is limited, particularly it is difficult to observe by the various microscopic informations that coating is combined with substrate.Transmission electron microscope multiplication factor can reach 50,000
More than times, the detailed information that coating/substrate combines is clear that, but need to prepare the cross-sectional sample of coating, sample system
It is larger to make difficulty.
Making for coating cross-sectional Transmission sample at present is prepared using copper ring or copper pipe method more.A.Chakraborty
Et al. the band plating aspect of two coating samples is bonded together using special glue, then carry out appropriate size cutting, will
The sample of well cutting is inserted in the copper pipe of 3mm diameters, fritter cutting along the section of copper pipe, and the thin slice of well cutting is carried out into machinery
Grinding, when being ground to sufficiently thin, using ion milling equipment to carrying out reduction processing among the sample of bonding, finally by sample
Be put into transmission electron microscope observing, patent CN 102519771 A, CN 103308362 A, CN 103487303 A also using similar
Means, or with copper ring or with copper pipe, and Seal treatment is carried out to carry out the preparation of transmission cross section sample using organic resin.
But this method is greatly influenceed by glue performance and sample performance, especially in mechanical grinding process, due to
The final thickness of grinding is typically at 30 to 100 microns, and now sample is in filminess, and non-deformability is very poor, though bond glue
It is cured, but fragility is stronger, especially under filminess, easily brittle failure.There is researcher to prevent sample from departing from copper pipe, adopt
The method filled with resin, but in the case of very thin, the resin of solidification equally has stronger fragility, (pressure and is rubbed in mechanical force
Wipe power) effect under be easy to brittle failure, make sample depart from copper ring.During ion milling, adhesive glue, resin material and coating material
There is larger performance difference in material, adhesive glue easily fall in flakes, cause two basic change sample to separate, or thin area concentrates on bonding
Jiao Chu, and there is no thin area on the sample to be observed, it can not be observed under transmission electron microscope.Therefore the sample preparation success rate of this method
Low, the thin area of sample is less.
The content of the invention
To overcome current hot-dip coated cross-sectional Transmission sample sample preparation success rate low, the problems such as thin area is less is obtained, the present invention
Purpose be to provide a kind of preparation method of hot-dip coated cross-sectional Transmission sample, this method is by hot-dip coated by two steel plate smeltings
Gold is combined together, it is not necessary to which the bonding of third-party binding agent, sample preparation success rate is higher, and it is more to obtain thin area, beneficial to more preferable
Viewed in transmittance.
A kind of preparation method of hot-dip coated cross-sectional Transmission sample, its operating procedure are as follows：
1) two steel plates are chosen and process multiple holes respectively on surface；
2) surface of steel plate after processing is cleaned up, two steel plates is stacked and are fixed together, between accompany pad, two
Gap is formed between steel plate；
3) steel plate fixed is put into progress hot-dip experiment in galvanizing simulator, starts stirring in hot-dip galvanized pot
Device is mixed, plating solution is smoothly flowed into plate stitch, in subsequent cooling section, the plating solution solidification in gap, two steel plates is formed smelting
Gold combines；
4) after hot-dip experiment, wire cutting is carried out along sheet material cross section at the edge in hole, by the sample after cutting along transversal
Face is ground, and carries out ion milling processing to ground sample, obtains thin area's transmission electron microscope observing sample.
The hole count of two steel plates is identical in the step 1) and mutual correspondence, is dislocation arrangement, two steel between corresponding aperture
Although being provided with pad between plate, gap is still smaller between two steel plates, and into after zinc pot, the gas in gap is not easy to flow out,
Hinder inflow of the zinc liquid to gap between two steel plates, to avoid such case, during drilling, by between the corresponding hole of two steel plates somewhat
Dislocation, this conveniently can flow into slit by guiding plating solution.The dislocation distance at two corresponding aperture centers is 1mm~5mm, the size sum in hole
Amount typically requires that Kong Yue is more more close better depending on steel plate size.
Spacer thickness is 0.2mm~1.0mm in the step 2).Spacer thickness is too thin, the gas row being unfavorable in gap
Go out the inflow with plating solution, it is too thick, it is unfavorable for ion milling processing, it is difficult to obtain coating/substrate interface Chu Bao areas.
The distance between adjacent holes of plate surface is less than 3mm in the step 1).Pitch of holes is larger, is stitched between two sheet materials
Gas storage in gap is more, is unfavorable for gas discharge.
Pad quantity is 1~4 in the step 2), is distributed in the center or periphery of steel plate.
Adopt and be bolted together between steel plate and pad for two in the step 2).
Hole on step 1) the light plate surface is circular, oval or square.
The present invention can be used for the hot-dip coatings such as galvanizing by dipping, hot-dip aluminizing, dip galvanized aluminum magnesium, the selection and hot-dip of steel plate
The setting of technique is set by actual process requirement.
The present invention has the advantages that compared with prior art：
The present invention makes to form metallurgical junction by solidifying plating solution between steel plate by surface of steel plate processing and or immersion
Close, adhesion greatly improves, not easy to break during follow-up grinding, ion milling, and it is saturating to effectively increase hot dip layer cross section
The success rate of sample preparation is penetrated, and more accurate and excellent thin area can be obtained.Through transmission electron microscope observing, obtain the thin area of sample compared with
It is more, and can effectively observe the microscopic information of coating/substrate joint portion.
Brief description of the drawings
The hot-dip coated cross-sectional Transmission sample preparation schematic diagrames of Fig. 1；
Fig. 2 is Fig. 1 left view.
In figure：A, b- steel plates (hot dip substrate)；C- pads；1- holes；2- bolts.
Embodiment
The preparation method of the present invention is described further below in conjunction with the accompanying drawings.
It is prepared by the cross-sectional Transmission sample of embodiment IF steel dip galvanizeds.
As shown in Figure 1, 2, a, b two is taken to open Ultra-low carbon (IF steel) steel plate that thickness is 2.0mm, plate size 120mm*
220mm。
1) drill：Drill as circular hole 1 (can also punching press ovalisation or square), bore dia 8mm, distance between holes
A is 2mm, and the center of circle dislocation distance in the corresponding hole of two steel plates is 2mm；
2) cleaning is fixed：Two steel plates are deoiled with acetone, then cleaned with alcohol in ultrasonic wave, are dried up；0.5mm is thick
Sheet metal shim clip (sheet metal shim size is 10mm*30mm) between two steel plates, pad are two, and center is with holes, respectively
Fix and (can also be fixed using rivet) positioned at steel plate both ends and by means of bolt 2；Pad c quantity can also be 1 or 3~4,
According to steel plate depending on size, when steel plate is smaller, only with 1 pad, the center of steel plate to be measured may be generally disposed at
Position；When steel plate is bigger, 3~4 pads can be used, are distributed in the center or periphery of steel plate to be measured.
3) hot-dip：The steel plate fixed is put into progress hot-dip experiment in galvanizing simulator, opened in zinc pot
Agitator, plating solution is smoothly flowed into plate stitch, hot-dip experiment is carried out using defined or immersion, after steel plate goes out zinc pot,
Zinc liquid between two sheet materials cools down rapidly, the plating solution solidification in gap, two steel plates is formed metallurgical binding；
4) sample is subsequently prepared：Long 3mm is gone out along cross-sectional cut in hole edge using wire cutting, thick 0.2mm fritter,
Pat is fixed in the special sample milling machine of transmission and is ground, 50 microns of thickness are ground to, to two plates in ion milling device
Middle zinc layers joint portion is thinned, and finally carries out viewed in transmittance.
Through transmission electron microscope observing, obtain that the thin area of sample is more, and can effectively observe the microcosmic letter of coating/substrate joint portion
Breath.
Surface of steel plate to be measured is processed into multiple holes by the present invention using mechanical means, by two steel plate processed middle pads
Enter pad, fixed sheet material with bolt, hot-dip experiment is carried out using galvanizing simulator.Liquid during hot dip in zinc pot
Hole of the metal along sheet material is flowed into the gap between two sheet materials naturally, and after steel plate goes out zinc pot cooling, the plating solution between two sheet materials coagulates
Gu and by two steel plate metallurgical bindings together, subsequent steel plate cuts appropriate size sample through means such as wire cuttings along cross section,
Transmission electron microscope observing is carried out after ground, ion milling.
Claims (7)
1. a kind of preparation method of hot-dip coated cross-sectional Transmission sample, it is characterised in that operating procedure is as follows：
1) two steel plates are chosen and process multiple holes respectively on surface；
2) surface of steel plate after processing is cleaned up, two steel plates is stacked and are fixed together, between accompany pad, two steel
Gap is formed between plate；
3) steel plate fixed is put into progress hot-dip experiment in galvanizing simulator, starts the stirring in hot-dip galvanized pot
Device, plating solution is smoothly flowed into plate stitch, in subsequent cooling section, the plating solution solidification in gap, two steel plates is formed metallurgy
With reference to；
4) after hot-dip experiment, wire cutting is carried out along sheet material cross section at the edge in hole, the sample after cutting is entered along cross section
Row grinding, and ion milling processing is carried out to ground sample, obtain thin area's transmission electron microscope observing sample.
2. the preparation method of hot-dip coated cross-sectional Transmission sample according to claim 1, it is characterised in that two in step 1)
The hole count of steel plate is identical and mutual correspondence, is dislocation arrangement between corresponding aperture, the dislocation distance at two corresponding aperture centers for 1mm~
5mm。
3. the preparation method of hot-dip coated cross-sectional Transmission sample according to claim 1, it is characterised in that padded in step 2)
Piece thickness is 0.2mm~1.0mm.
4. the preparation method of hot-dip coated cross-sectional Transmission sample according to claim 1, it is characterised in that steel in step 1)
The distance between adjacent holes of plate surface is less than 3mm.
5. the preparation method of hot-dip coated cross-sectional Transmission sample according to claim 1, it is characterised in that the step 2)
Middle pad quantity is 1~4, is distributed in the center or periphery of steel plate.
6. the preparation method of hot-dip coated cross-sectional Transmission sample according to claim 1, it is characterised in that the step 2)
In two adopt and be bolted together between steel plate and pad.
7. the preparation method of hot-dip coated cross-sectional Transmission sample according to claim 1, it is characterised in that the step 1)
Hole on light plate surface is circular, oval or square.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610329644.4A CN107402146B (en) | 2016-05-18 | 2016-05-18 | Preparation method of hot-dip coating section transmission sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610329644.4A CN107402146B (en) | 2016-05-18 | 2016-05-18 | Preparation method of hot-dip coating section transmission sample |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107402146A true CN107402146A (en) | 2017-11-28 |
| CN107402146B CN107402146B (en) | 2020-05-29 |
Family
ID=60394111
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610329644.4A Active CN107402146B (en) | 2016-05-18 | 2016-05-18 | Preparation method of hot-dip coating section transmission sample |
Country Status (1)
| Country | Link |
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| CN (1) | CN107402146B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111796121A (en) * | 2020-07-22 | 2020-10-20 | 广东省焊接技术研究所（广东省中乌研究院） | Strong texture structure metal transmission electron microscopic characterization sample preparation method |
| CN112557133A (en) * | 2020-11-10 | 2021-03-26 | 鞍钢股份有限公司 | Method for preparing hot-dip coating transmission sample by reduction-oxidation delamination method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100865764B1 (en) * | 2007-07-05 | 2008-10-29 | 강원대학교산학협력단 | A method for thickness measurement of dipping coating layer on wire |
| CN102323119A (en) * | 2011-05-25 | 2012-01-18 | 武汉钢铁(集团)公司 | Method for preparing rust layer sample for being observed by scanning electron microscope |
| CN102519771A (en) * | 2011-12-30 | 2012-06-27 | 青岛大学 | Method for preparing cross section transmission electron microscope sample |
| CN103308362A (en) * | 2013-06-14 | 2013-09-18 | 首钢总公司 | Sample preparation method of alloying hot-dip galvanized coating section transmission sample |
| CN103487303A (en) * | 2013-09-30 | 2014-01-01 | 首钢总公司 | Method for preparing cross-section transmission electron microscope sample of cold-rolled sheet |
-
2016
- 2016-05-18 CN CN201610329644.4A patent/CN107402146B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100865764B1 (en) * | 2007-07-05 | 2008-10-29 | 강원대학교산학협력단 | A method for thickness measurement of dipping coating layer on wire |
| CN102323119A (en) * | 2011-05-25 | 2012-01-18 | 武汉钢铁(集团)公司 | Method for preparing rust layer sample for being observed by scanning electron microscope |
| CN102519771A (en) * | 2011-12-30 | 2012-06-27 | 青岛大学 | Method for preparing cross section transmission electron microscope sample |
| CN103308362A (en) * | 2013-06-14 | 2013-09-18 | 首钢总公司 | Sample preparation method of alloying hot-dip galvanized coating section transmission sample |
| CN103487303A (en) * | 2013-09-30 | 2014-01-01 | 首钢总公司 | Method for preparing cross-section transmission electron microscope sample of cold-rolled sheet |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111796121A (en) * | 2020-07-22 | 2020-10-20 | 广东省焊接技术研究所（广东省中乌研究院） | Strong texture structure metal transmission electron microscopic characterization sample preparation method |
| CN112557133A (en) * | 2020-11-10 | 2021-03-26 | 鞍钢股份有限公司 | Method for preparing hot-dip coating transmission sample by reduction-oxidation delamination method |
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| Publication number | Publication date |
|---|---|
| CN107402146B (en) | 2020-05-29 |
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