CN103439170A - Method for displaying and detecting inhibition layer of hot-dip-coated zinc sheet - Google Patents
Method for displaying and detecting inhibition layer of hot-dip-coated zinc sheet Download PDFInfo
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- CN103439170A CN103439170A CN2013103642763A CN201310364276A CN103439170A CN 103439170 A CN103439170 A CN 103439170A CN 2013103642763 A CN2013103642763 A CN 2013103642763A CN 201310364276 A CN201310364276 A CN 201310364276A CN 103439170 A CN103439170 A CN 103439170A
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Abstract
A method for displaying and detecting an inhibition layer of a hot-dip-coated zinc sheet belongs to the technical field of physical detection of metal. The technical scheme is that a hot-dip-coated zinc sheet sample is used as an anode, the platinum electrode is used as an auxiliary electrode, and the saturated calomel electrode is used as a reference electrode; constant potential electrolysis is conducted in an electrolyte of sodium chloride and hydrochloric acid, with the electric potential range of the relative saturated calomel electrode at -1.030 V to -0.980 V, so that the zinc layer is dissolved; the current-time curve of the electrolysis process is recorded, when the electrolysis current is reduced to zero, the zinc layer is dissolved completely, and the reaction stops; the sample is taken out, washed with deionized water and acetone, dried, and observed and detected regarding the inhibition layer through a scanning electron microscope. The invention has the advantages that the method can accurately control the experiment process, and the inhibition layer can be maintained and displayed completely while the zinc layer is removed through electrolysis.
Description
Technical field
The invention belongs to metal physics detection technique field.Be particularly related to a kind of method that shows and detect heat zinc coating plate inhibition layer.
Background technology
In the heat zinc coating plate production run, often in zinc liquid, add appropriate aluminium, make to form between steel matrix and zinc coating the Fe-Al compound layer of thin layer, to suppress the diffusion reaction between zinc-iron, improve coating performance, this layer of Fe-Al compound layer is called and suppresses layer.Suppress layer to the hot galvanizing sheet quality and organize critical effect, many defects on heat zinc coating plate surface have substantial connection with the inhibition layer.
In order to be furtherd investigate suppressing layer, need to cover the zinc coating suppressed above layer and remove, make to suppress layer and show, so that it is directly observed and detects.But, owing to suppressing layer as thin as a wafer, this brings great difficulty to sample preparation, its difficult point is how accurately to control the dissolution degree of zinc layer, complete reservation and demonstration inhibition layer when surperficial pure zinc layer is removed.Show that at present the common method that suppresses layer is the chemical reagent etch, soon sample is immersed in acid etching solution surperficial zinc layer is dissolved, and makes to suppress layer and shows.But this method is difficult to realize the accurate control to experimentation, the degree that pure zinc layer dissolves can only be with naked eyes and micro-judgment, slightly there is deviation just can also dissolve suppressing layer, the sample made like this is difficult to complete reservation and shows suppress layer, can't be as whether there being the criterion that suppresses layer defects.
Summary of the invention
The object of the present invention is to provide a kind of demonstration and detect the method that heat zinc coating plate suppresses layer, what in the solution classic method, exist can't accurately control zinc layer dissolution degree, is difficult to the problem that complete reservation and demonstration suppress layer.
Technical scheme of the present invention is achieved in that
1, preparation sodium chloride-electrolysis of hydrochloric acid liquid, proportioning is by weight percentage: 3～20% sodium chloride, 0.5%～5% hydrochloric acid, surplus is deionized water.
2, take the heat zinc coating plate sample as anode, platinum electrode is auxiliary electrode, and saturated calomel electrode is contrast electrode, in sodium chloride-electrolysis of hydrochloric acid liquid,-1.030V～-carry out potentiostatic deposition in the potential range of 0.980V (relative saturation mercurous chloride electrode), dissolve pure zinc layer.
3, record the electric current-time curve in electrolytic process, when Faradaic current is reduced to zero, pure zinc layer is dissolved fully, now stops immediately reaction.
4, take out sample, cleaned with deionized water and acetone successively, after drying, by scanning electron microscope, to suppressing layer, observed and detect.
Principle of the present invention is based on the dissolution potential of pure zinc layer and suppresses the difference of layer dissolution potential, by controlling current potential, makes the pure zinc layer selective dissolution, and suppress layer, is retained and shows.
The invention has the advantages that:
1, adopt the mode of potentiostatic deposition, can complete reservation and demonstration inhibition layer when removing pure zinc layer.
2, experimentation has reaction end clearly, can accurately control experimentation.
3, the present invention adopts conventional electrochemical electrolysis device, simple and convenient under laboratory environment.
The accompanying drawing explanation
Fig. 1 is the electrolysis unit schematic diagram that the present invention adopts.Wherein, sample 1, platinum electrode 2, saturated calomel electrode 3.
Embodiment
Embodiment 1:
1, preparation sodium chloride-electrolysis of hydrochloric acid liquid, proportioning is by weight percentage: 5% sodium chloride, 2% hydrochloric acid, surplus is deionized water.
2, take heat zinc coating plate sample 1 as anode, platinum electrode 2 is auxiliary electrode, and saturated calomel electrode 3 is contrast electrode, in sodium chloride-electrolysis of hydrochloric acid liquid, with current potential-1.000V(relative saturation mercurous chloride electrode) carry out potentiostatic deposition, dissolve pure zinc layer.
3, record the electric current-time curve in electrolytic process, when Faradaic current is reduced to zero, pure zinc layer is dissolved fully, now stops immediately reaction.
4, take out sample, cleaned with deionized water and acetone successively, after drying, by scanning electron microscope, to suppressing layer, observed and detect.
The pure zinc layer of finding the galvanized sheet surface after observing is completely removed, and suppress layer and be retained and show, and complete shape and appearance.
Embodiment 2:
1, preparation sodium chloride-electrolysis of hydrochloric acid liquid, proportioning is by weight percentage: 5% sodium chloride, 2% hydrochloric acid, surplus is deionized water.
2, take heat zinc coating plate sample 1 as anode, platinum electrode 2 is auxiliary electrode, and saturated calomel electrode 3 is contrast electrode, in sodium chloride-electrolysis of hydrochloric acid liquid, with current potential-1.030V(relative saturation mercurous chloride electrode) carry out potentiostatic deposition, dissolve pure zinc layer
3, record the electric current-time curve in electrolytic process, when Faradaic current is reduced to zero, pure zinc layer is dissolved fully, now stops immediately reaction.
4, take out sample, cleaned with deionized water and acetone successively, after drying, by scanning electron microscope, to suppressing layer, observed and detect.
The pure zinc layer of finding the galvanized sheet surface after observing is completely removed, suppresses layer and is retained demonstration and complete shape and appearance.
Embodiment 3:
1, preparation sodium chloride-electrolysis of hydrochloric acid liquid, proportioning is by weight percentage: 10% sodium chloride, 1% hydrochloric acid, surplus is deionized water.
2, take heat zinc coating plate sample 1 as anode, platinum electrode 2 is auxiliary electrode, and saturated calomel electrode 3 is contrast electrode, in sodium chloride-electrolysis of hydrochloric acid liquid, with current potential-1.010V(relative saturation mercurous chloride electrode) carry out potentiostatic deposition, dissolve pure zinc layer.
3, record the electric current-time curve in electrolytic process, when Faradaic current is reduced to zero, pure zinc layer is dissolved fully, now stops immediately reaction.
4, take out sample, cleaned with deionized water and acetone successively, after drying, by scanning electron microscope, to suppressing layer, observed and detect.
The pure zinc layer of finding the galvanized sheet surface after observing is completely removed, suppresses layer and is retained demonstration and complete shape and appearance.
Claims (1)
1. one kind shows and detects the method that heat zinc coating plate suppresses layer, it is characterized in that, comprises the following steps:
(1) preparation sodium chloride-electrolysis of hydrochloric acid liquid, proportioning is by weight percentage: 3～20% sodium chloride, 0.5%～5% hydrochloric acid, surplus is deionized water;
(2) take the heat zinc coating plate sample as anode, platinum electrode is auxiliary electrode, and saturated calomel electrode is contrast electrode, in sodium chloride-electrolysis of hydrochloric acid liquid, at the relative saturation mercurous chloride electrode ,-1.030V～-carry out potentiostatic deposition in the potential range of 0.980V, dissolve pure zinc layer;
(3) record the electric current-time curve in electrolytic process, when Faradaic current is reduced to zero, pure zinc layer is dissolved fully, now stops reaction;
(4) take out sample, cleaned with deionized water and acetone successively, after drying, by scanning electron microscope, to suppressing layer, observed and detect.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105004588A (en) * | 2015-07-10 | 2015-10-28 | 首钢总公司 | Alloy-galvanized layer scanning electron microscope sectioned sample precision making method |
| CN106092709A (en) * | 2016-06-07 | 2016-11-09 | 武汉钢铁股份有限公司 | The preparation method of heat zinc coating plate interface inhibition layer feature detection sample and device |
| CN111665109A (en) * | 2020-06-19 | 2020-09-15 | 武汉钢铁有限公司 | Preparation device and method of galvanized steel sheet matrix metallographic sample |
| CN113514528A (en) * | 2021-03-10 | 2021-10-19 | 首钢集团有限公司 | Method for measuring compactness of hot-dip galvanized sheet inhibition layer |
| CN114280120A (en) * | 2021-12-29 | 2022-04-05 | 上海大学 | Method for detecting protective slag type linear defects on surface of hot-galvanized automobile outer plate |
| CN114280121A (en) * | 2021-12-29 | 2022-04-05 | 上海大学 | Al-containing hot galvanizing automobile outer plate surface2O3Method for detecting inclusion linear defects |
| CN114318342A (en) * | 2021-12-31 | 2022-04-12 | 马鞍山钢铁股份有限公司 | Corrosion solution for removing galvanized layer of steel plate and method for displaying galvanized steel plate inhibition layer |
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| JPS63215940A (en) * | 1987-03-04 | 1988-09-08 | Nkk Corp | Preparation of sample for micro observation of painted film section |
| CN101476099A (en) * | 2009-01-22 | 2009-07-08 | 华南理工大学 | Method for steel product batch hot dip galvanizing |
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| JPS63215940A (en) * | 1987-03-04 | 1988-09-08 | Nkk Corp | Preparation of sample for micro observation of painted film section |
| CN101476099A (en) * | 2009-01-22 | 2009-07-08 | 华南理工大学 | Method for steel product batch hot dip galvanizing |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105004588A (en) * | 2015-07-10 | 2015-10-28 | 首钢总公司 | Alloy-galvanized layer scanning electron microscope sectioned sample precision making method |
| CN106092709A (en) * | 2016-06-07 | 2016-11-09 | 武汉钢铁股份有限公司 | The preparation method of heat zinc coating plate interface inhibition layer feature detection sample and device |
| CN111665109A (en) * | 2020-06-19 | 2020-09-15 | 武汉钢铁有限公司 | Preparation device and method of galvanized steel sheet matrix metallographic sample |
| CN111665109B (en) * | 2020-06-19 | 2023-09-19 | 武汉钢铁有限公司 | Preparation device and method for metallographic sample of galvanized steel sheet matrix |
| CN113514528A (en) * | 2021-03-10 | 2021-10-19 | 首钢集团有限公司 | Method for measuring compactness of hot-dip galvanized sheet inhibition layer |
| CN113514528B (en) * | 2021-03-10 | 2024-05-10 | 首钢集团有限公司 | Method for measuring compactness of inhibition layer of hot dip galvanized sheet |
| CN114280120A (en) * | 2021-12-29 | 2022-04-05 | 上海大学 | Method for detecting protective slag type linear defects on surface of hot-galvanized automobile outer plate |
| CN114280121A (en) * | 2021-12-29 | 2022-04-05 | 上海大学 | Al-containing hot galvanizing automobile outer plate surface2O3Method for detecting inclusion linear defects |
| CN114318342A (en) * | 2021-12-31 | 2022-04-12 | 马鞍山钢铁股份有限公司 | Corrosion solution for removing galvanized layer of steel plate and method for displaying galvanized steel plate inhibition layer |
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| CN103439170B (en) | 2015-08-26 |
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Address after: 100041 Shijingshan Road, Shijingshan District, Shijingshan District, Beijing Patentee after: Shougang Group Co. Ltd. Address before: 100041 Shijingshan Road, Shijingshan District, Shijingshan District, Beijing Patentee before: Capital Iron & Steel General Company |