CN103308362A - Sample preparation method of alloying hot-dip galvanized coating section transmission sample - Google Patents
Sample preparation method of alloying hot-dip galvanized coating section transmission sample Download PDFInfo
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- CN103308362A CN103308362A CN2013102365829A CN201310236582A CN103308362A CN 103308362 A CN103308362 A CN 103308362A CN 2013102365829 A CN2013102365829 A CN 2013102365829A CN 201310236582 A CN201310236582 A CN 201310236582A CN 103308362 A CN103308362 A CN 103308362A
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Abstract
The invention relates to a sample preparation method of an alloying hot-dip galvanized coating section transmission sample, and belongs to the field of transmission electron microscope analysis of alloy coatings. The sample preparation method comprises the following steps of: precutting an alloying hot-dip galvanized plate sample, and then fixing the precut sample in a copper pipe; and then cutting the copper pipe into slices along a radial direction, and carrying out thinning, final thinning and carbon coating to finally obtain an alloying hot-dip galvanized coating section film sample suitable for observation of a transmission electron microscope. The sample preparation method disclosed by the invention can be used for relatively easily and conveniently preparing the alloying hot-dip galvanized coating section transmission electron microscope sample and effectively protecting the outer loose phase by dint of G1 glue to prevent the desquamation.
Description
Technical field
The invention belongs to the TEM (transmission electron microscope) analysis technical field of alloy layer, particularly a kind of method for making sample of alloyed zinc hot dip galvanized layer cross section transmission sample.
Background technology
Alloyed hot-dip galvanized steel sheet is (hereinafter to be referred as the GA steel plate, Galvannealed Sheet Steel) be applied to more and more on the automobile with advantages such as its good corrosion resisting property, coating performance and welding performances, Japanese serial car particularly, its panel has all adopted the GA steel plate basically.So-called GA plate refers to that be that 0.11%～0.14% zinc liquid carries out adopting coating diffusion annealing after the galvanizing with steel by aluminum content, obtains the coating iron content at 7%～15% zn-fe alloy coating steel plate.This zinc-iron alloy tissue may contain Γ phase (Fe
3Zn
10-body-centered cubic structure); Γ 1 phase (FeZn
4Or Fe
5Zn
21-face-centred cubic structure); δ phase (FeZn
7Or FeZn
10-hexagonal structure) with ζ (FeZn mutually
13Or FeZn
15-monocline), some specimen surface of owing alloying has the η pure zinc layer.The coating gross thickness is generally at 6～10 μ m, wherein the Γ of internal layer is brittle layer mutually, easily form crackle and matrix stripping, and outer field δ comes off easily with ζ is loose mutually, therefore prevent Γ mutually cracking to come off mutually with δ and ζ be the key of preparation alloying zinc coat cross-sectional sample.When utilizing the so complicated alloy layer of TEM (transmission electron microscope) analysis, require comprising of the thin district of sample above-mentioned all mutually and keep complete.The method that can successfully prepare at present the hot galvanized layer cross-sectional sample of alloying is to utilize focused ion beam (FIB) from alloyed hot-dip zine plate surface etch cross section thin slice, but this method can not effectively prevent outer loose coming off, and sampling is required harsh, with high costs.
Summary of the invention
The object of the present invention is to provide a kind of method for making sample of alloyed zinc hot dip galvanized layer cross section transmission sample.Can comparatively easy preparing comprise all mutually and the sample for use in transmitted electron microscope of complete alloyed zinc hot dip galvanized layer cross section.
The present invention after the bonding is fixed on alloyed hot-dip zine plate sample coating in the copper pipe of external diameter 3.05mm face-to-face, again copper pipe is radially thinly sliced the final alloyed zinc hot dip galvanized layer cross section film sample that obtains suitable transmission electron microscope observing after processing through attenuate, pit and ion milling.
Concrete technology step and parameter are as follows:
1, precut sample: at first testing sample will be cut into suitable size.For alloyed hot-dip zine plate sample coating is bondd face-to-face and the copper pipe of packing in, the size of sample must satisfy certain geometric relationship: be rectangle to sticking sample in cross section a), the diagonal line of rectangle is copper pipe internal diameter 2r, article one, right-angle side is 2 times of thickness of slab, be 2h, another right-angle side is sample width d, and these three limits have consisted of right-angle triangle, therefore the width d of sample is determined by the thickness of slab of copper pipe internal diameter and sample, i.e. d
2=(2r)
2-(2h)
2, Fig. 1 is the schematic cross-section that copper pipe is inlayed sample; B) sample length is greater than copper pipe length 2-3mm, in order to help cementing agent to flow.Use the skive sheet that testing sample is required to cut into elongated strip according to above-mentioned how much.
2, fixed sample: as bonding agent, G1 glue has good flowability at normal temperatures with G1 glue, is solidifying more than 130 ℃, and hardness is a little less than iron and steel after solidifying.To be cut into the coating of testing sample of elongated strip face-to-face to sticking with G1 glue first, left standstill 10～15 minutes, make G1 glue enter in the slit of alloying Several Thiourea Derivatives on Zinc Plate Surface, then the top layer phase that embedding is loose places to heat on 125～130 ℃ of warm tables to make adhesive curing in 10～15 minutes.Vertically be placed in the pit of diameter 3.5mm on the sample bench i.e. copper pipe upper end open, bottom sealing after at room temperature will inserting copper pipe to the sample that glues.Pour into G1 glue from the upper end of copper pipe and leave standstill, rely on flowing of glue to discharge bubble in the copper pipe fully, copper pipe is placed on 125～130 ℃ of warm tables together with sample bench to make adhesive curing in 10～15 minutes again.
3, section: use the vertical copper pipe section of skive sheet, obtain the cross section thin slice of thickness 0.18～0.22mm.
4, attenuate: use successively 1200# and 2000# sand paper hand lapping cross section thin slice, make sample be thinned to 45～55 μ m from 0.18～0.22mm.Use the pit instrument to be that the coating position is recessed in cross section thin slice center and go out a hole, guarantee that the thickness of bottom, hole is 25～35 μ m.
5, whole attenuate: use ion milling, keep the sample stage temperature at-90～-70 ℃, voltage 4.5～5KV, rotating speed 3～3.5rad/min, upper ion gun 5～7o, lower ion gun 3.5～4.5o, attenuate 3～5 hours is until perforation.Reduce voltage to 3～3.5KV and continue bombardment 5～10min, finish the attenuate of sample behind the cleaning sample surfaces, take out sample.Cracked for preventing through the cross section thin slice of attenuate, with G1 glue or carbonaceous conductive glue sample is sticked on the copper ring the alloyed zinc hot dip galvanized layer of the vertical sample of major axis of slotted eye in the middle of the copper ring behind the taking-up sample.
6, plating carbon: G1 glue is a kind of resin, and is non-conductive, needs to plate carbon before therefore observing.Sample is put into the high vacuum vapor deposition instrument, and plated surface one deck carbon forms conductive layer, and sample preparation is finished.
The invention has the advantages that: the preparation of relative simple the sample for use in transmitted electron microscope of alloyed zinc hot dip galvanized layer cross section, can effectively protect outer loose phase by G1 glue, prevent from coming off.
Description of drawings
Fig. 1 is the schematic cross-section that copper pipe is inlayed sample.Wherein, alloyed zinc hot dip galvanized layer 1, steel substrate 2, G1 glue 3, copper pipe 4.
Fig. 2 is the fixing schematic diagram of sample.Wherein, G1 glue 3, copper pipe 4, sample 5, sample bench 6.
Embodiment
Embodiment 1:
The preparation of the alloyed zinc hot dip galvanized layer cross section sample for use in transmitted electron microscope of DX56D+Z
(1) precut sample: through measuring as can be known sample thickness of slab 0.6mm, the copper pipe internal diameter is 2.4mm, with the geometric relationship of copper pipe, calculates the sample width and should be 2.0 mm per sample.Sample is cut into 2.0mm wide, long 2 of 15mm.
(2) fixed sample: 2 strip samples that will cut, left standstill 15 minutes at 130 ℃ hot platforms after sticking with G1 glue, treated that glue solidifies fully.Then put into copper pipe and fix with G1 glue, be placed in the pit of sample bench, after bubble is discharged fully, be placed on 130 ℃ the hot platform and left standstill 15 minutes.
(3) section: use the vertical copper pipe cutting of high-precision skive sheet, acquisition thickness is that 0.2mm, diameter are the disk of 3.05mm.
(4) attenuate: use 1200# and 2000# sand paper hand lapping cross section thin slice to 50 μ m; Use the pit instrument to reduce in advance 30 μ m.
(5) whole attenuate: under-80 ℃ of conditions, use ion milling, setting voltage 5KV, rotating speed 3.5rad/min, upper ion gun 6o, lower ion gun 4o after boring a hole, reduces voltage to 3KV continuation bombardment 5min cleaning sample surfaces.Stop cooling, after the sample stage temperature reaches room temperature, take out sample, sample is sticked on the copper ring of slotted eye with G1 glue, the vertical sample zinc coat of major axis of slotted eye in the middle of the copper ring.
(6) plate carbon: the sample that glues is placed in the high vacuum vapor deposition instrument plates carbon.
The sample preparation effect observation.Under transmission electron microscope, observe sample, can see whole coating overall picture in the suitable zone of observing of thickness, intact near a side of steel matrix, crackle does not appear, and outer being embedded in fully in the G1 glue.Careful observation can pick out Γ phase, Γ 1 phase, δ phase and ζ mutually one by one in conjunction with selected diffraction.Wherein neighbour's steel substrate and have a palisade feature be the Γ phase of fragility; For outer field ζ phase, more loose, but owing to G1 glue infiltrates in all slits, so ζ does not come off mutually.
Claims (3)
1. the method for making sample of an alloyed zinc hot dip galvanized layer cross section transmission sample is characterized in that, processing step and parameter are as follows:
1) precut sample: the size of sample satisfies certain geometric relationship:
Be rectangle to sticking sample in cross section, the diagonal line of rectangle is copper pipe internal diameter 2r, and right-angle side is 2 times of thickness of slab, i.e. 2h, and another right-angle side is sample width d, these three limits have consisted of right-angle triangle; The width d of sample is by the thickness of slab decision of copper pipe internal diameter and sample, i.e. d
2=(2r)
2-(2h)
2
Sample length is greater than copper pipe length 2-3mm, so that cementing agent flows; Use the skive sheet that testing sample is required to cut into elongated strip according to above-mentioned how much;
2) fixed sample: use G1 glue as bonding agent, to be cut into the coating of testing sample of elongated strip face-to-face to sticking, left standstill 10～15 minutes, make G1 glue enter in the slit of alloying Several Thiourea Derivatives on Zinc Plate Surface, then the top layer phase that embedding is loose places to heat on 125～130 ℃ of warm tables to make adhesive curing in 10～15 minutes; Vertically be placed in the pit of diameter 3.5mm on the sample bench i.e. copper pipe upper end open, bottom sealing after at room temperature will inserting copper pipe to the sample that glues; Pour into G1 glue from the upper end of copper pipe and leave standstill, rely on flowing of glue to discharge bubble in the copper pipe fully, copper pipe is placed on 125～130 ℃ of warm tables together with sample bench to make adhesive curing in 10～15 minutes again;
3) section: with the vertical copper pipe section of skive sheet, obtain the cross section thin slice of thickness 0.18～0.22mm;
4) attenuate: use successively 1200# and 2000# sand paper hand lapping cross section thin slice, make sample be thinned to 45～55 μ m from 0.18～0.22mm; Use the pit instrument to be that the coating position is recessed in cross section thin slice center and go out a hole, guarantee that the thickness of bottom, hole is 25～35 μ m;
5) whole attenuate: use ion milling, keep the sample stage temperature at-90～-70 ℃, voltage 4.5～5KV, rotating speed 3～3.5rad/min, upper ion gun 5～7o, lower ion gun 3.5～4.5o, attenuate 3～5 hours is until perforation; Reduce voltage to 3～3.5KV and continue bombardment 5～10min, finish the attenuate of sample behind the cleaning sample surfaces, take out sample;
6) plating carbon: sample is put into the high vacuum vapor deposition instrument, and plated surface one deck carbon forms conductive layer, and sample preparation is finished.
2. method according to claim 1 is characterized in that step 2) in G1 glue good flowability is arranged at normal temperatures, solidifying more than 125 ℃, hardness is a little less than iron and steel after solidifying.
3. method according to claim 1, it is characterized in that, cracked for preventing through the cross section thin slice of attenuate in the step 5), with G1 glue or carbonaceous conductive glue sample is sticked on the copper ring the alloyed zinc hot dip galvanized layer of the vertical sample of major axis of slotted eye in the middle of the copper ring behind the taking-up sample.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104075928A (en) * | 2014-06-13 | 2014-10-01 | 北京工业大学 | Method for mechanically thinning grinding wafer transmission electron microscope test sample |
| CN105004588A (en) * | 2015-07-10 | 2015-10-28 | 首钢总公司 | Alloy-galvanized layer scanning electron microscope sectioned sample precision making method |
| CN105300761A (en) * | 2015-10-15 | 2016-02-03 | 武汉钢铁(集团)公司 | Preparation method of TEM electrolysis double-jet film sample of small-size metal material |
| CN105334095A (en) * | 2015-12-01 | 2016-02-17 | 贵州大学 | Sample preparation method and device for metal material transmission electron microscope with diameter of less than 3 mm |
| CN107121446A (en) * | 2017-04-25 | 2017-09-01 | 大连交通大学 | A kind of Cross-section transmission tem sample mechanical pre-thinning method |
| CN107402146A (en) * | 2016-05-18 | 2017-11-28 | 鞍钢股份有限公司 | A kind of preparation method of hot-dip coated cross-sectional Transmission sample |
| CN107607566A (en) * | 2017-08-31 | 2018-01-19 | 湖南人文科技学院 | A kind of bimetal recombination line Cross-section transmission sample preparation methods |
| CN107643309A (en) * | 2017-08-31 | 2018-01-30 | 武汉钢铁有限公司 | The analysis method of electrical steel surface coating |
| CN111982948A (en) * | 2020-08-27 | 2020-11-24 | 矿冶科技集团有限公司 | Preparation method of scanning electron microscope section sample of micron-sized powder |
| 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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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104075928A (en) * | 2014-06-13 | 2014-10-01 | 北京工业大学 | Method for mechanically thinning grinding wafer transmission electron microscope test sample |
| CN104075928B (en) * | 2014-06-13 | 2016-07-06 | 北京工业大学 | A kind of grinding wafer transmission electron microscope sample mechanical reduction method |
| CN105004588A (en) * | 2015-07-10 | 2015-10-28 | 首钢总公司 | Alloy-galvanized layer scanning electron microscope sectioned sample precision making method |
| CN105300761A (en) * | 2015-10-15 | 2016-02-03 | 武汉钢铁(集团)公司 | Preparation method of TEM electrolysis double-jet film sample of small-size metal material |
| CN105334095B (en) * | 2015-12-01 | 2018-07-06 | 贵州大学 | A kind of diameter is less than the method for making sample and device of 3mm metal material transmission electron microscopes |
| CN105334095A (en) * | 2015-12-01 | 2016-02-17 | 贵州大学 | Sample preparation method and device for metal material transmission electron microscope with diameter of less than 3 mm |
| CN107402146A (en) * | 2016-05-18 | 2017-11-28 | 鞍钢股份有限公司 | A kind of preparation method of hot-dip coated cross-sectional Transmission sample |
| CN107121446A (en) * | 2017-04-25 | 2017-09-01 | 大连交通大学 | A kind of Cross-section transmission tem sample mechanical pre-thinning method |
| CN107121446B (en) * | 2017-04-25 | 2019-10-22 | 大连交通大学 | A kind of Cross-section transmission tem sample mechanical pre-thinning method |
| CN107643309A (en) * | 2017-08-31 | 2018-01-30 | 武汉钢铁有限公司 | The analysis method of electrical steel surface coating |
| CN107607566A (en) * | 2017-08-31 | 2018-01-19 | 湖南人文科技学院 | A kind of bimetal recombination line Cross-section transmission sample preparation methods |
| CN107643309B (en) * | 2017-08-31 | 2020-04-07 | 武汉钢铁有限公司 | Analysis method of electrical steel surface coating |
| CN111982948A (en) * | 2020-08-27 | 2020-11-24 | 矿冶科技集团有限公司 | Preparation method of scanning electron microscope section sample of micron-sized powder |
| 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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Application publication date: 20130918 |