CN110344060B - Corrosive agent for displaying coating structure of zinc-iron alloy hot-dip galvanized steel sheet and preparation and use methods thereof - Google Patents

Corrosive agent for displaying coating structure of zinc-iron alloy hot-dip galvanized steel sheet and preparation and use methods thereof Download PDF

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Publication number
CN110344060B
CN110344060B CN201910620362.3A CN201910620362A CN110344060B CN 110344060 B CN110344060 B CN 110344060B CN 201910620362 A CN201910620362 A CN 201910620362A CN 110344060 B CN110344060 B CN 110344060B
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zinc
iron alloy
coating structure
dip galvanized
steel sheet
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CN110344060A (en
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杨峥
王德宝
刘志军
牟祖茂
张峰
徐辉
程志远
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Maanshan Iron and Steel Co Ltd
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Maanshan Iron and Steel Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00Etching metallic material by chemical means
    • C23F1/10Etching compositions
    • C23F1/14Aqueous compositions
    • C23F1/16Acidic compositions
    • C23F1/30Acidic compositions for etching other metallic material
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Coating With Molten Metal (AREA)
  • Investigating And Analyzing Materials By Characteristic Methods (AREA)
  • ing And Chemical Polishing (AREA)

Abstract

The corrosive agent consists of a nitric acid alcohol solution and a picric acid alcohol solution, wherein the picric acid is weak in acidity in the raw material composition, and after the mixture of the picric acid and nitric acid is used, a layer of protective film can be formed on the surface of a sample, so that the etching speed and depth of a zinc layer are inhibited to a certain extent, an obvious etching step between the zinc layer and a substrate is avoided, and a clear zinc-iron alloy coating structure is obtained. The corrosive agent has simple configuration, low toxicity and easy stable corrosive effect.

Description

Corrosive agent for displaying coating structure of zinc-iron alloy hot-dip galvanized steel sheet and preparation and use methods thereof
Technical Field
The invention belongs to the technical field of metal material detection, and particularly relates to a corrosive agent for displaying a coating structure of a zinc-iron alloy hot-dip galvanized steel sheet, and a preparation method and a use method thereof.
Background
After the hot-dip galvanized steel strip is discharged from the plating tank, the hot-dip galvanized steel strip enters an alloying treatment furnace to be heated again, so that iron elements are diffused to a zinc layer, and a uniform zinc-iron alloy layer is formed on a coil, namely the zinc-iron alloy hot-dip galvanized steel strip. According to the Fe-Zn phase diagram, an alpha phase, a gamma phase and a gamma phase are generated in sequence in a typical hot dip galvanized structure1Phase, delta phase, zeta phase, eta phase. However, it is found from the literature that the alloyed hot-dip galvanized steel sheet actually observed mainly contains Γ phase and Γ phase1Phase, delta phase. Proper corrosion of Zn-Fe alloy layer can obtain its composition structure, study the growth rule of coating and the relation between coating structure and performanceAnd optimizing alloying process parameters.
The existing zinc-iron alloy corrosion method mainly adopts nitric acid alcohol or amyl alcohol nitrate solution, or the corrosion degree is not easy to control, so that satisfactory corrosion effect is difficult to obtain; or has high toxicity, which brings danger to the testing personnel.
Disclosure of Invention
In order to solve the technical problems, the invention provides a corrosive agent for displaying a coating structure of a zinc-iron alloy hot-dip galvanized steel sheet, and a preparation and use method thereof.
The technical scheme adopted by the invention is as follows:
a corrosive agent for displaying a coating structure of a zinc-iron alloy hot-dip galvanized steel sheet is composed of a nitric acid alcohol solution and a picric acid alcohol solution.
The volume ratio of the nitric acid alcohol solution to the picric acid alcohol solution is 1-1.2:1, and preferably 1: 1.
The volume concentration of the nital solution is 1-2%. The mass concentration of the picric acid alcohol solution is 1-2%. After the two acid liquids with the concentrations are mixed, the erosion speed and the depth of the zinc layer can be controlled, and a clear zinc-iron alloy coating structure is obtained.
The alcohol used for preparing the nitric acid alcohol solution and the picric acid alcohol solution is absolute ethyl alcohol.
The invention also provides a preparation method of the corrosive for displaying the coating structure of the zinc-iron alloy hot-dip galvanized steel sheet, which is to directly and uniformly mix the nitric acid alcohol solution and the picric acid alcohol solution.
The invention also provides a use method of the corrosive for displaying the coating structure of the zinc-iron alloy hot-dip galvanized steel sheet.
Further, the etching time is 10 to 20 seconds. The control can obtain a clear zinc-iron alloy coating structure in such a time.
Compared with the prior art, the corrosive for displaying the coating structure of the zinc-iron alloy hot-dip galvanized steel sheet provided by the invention is simple in configuration, low in toxicity and easy to obtain a stable corrosion effect. In the raw material composition, picric acid is weak in acidity, and after the picric acid is mixed with nitric acid for use, a layer of protective film can be formed on the surface of a sample, so that the etching speed and depth of a zinc layer are inhibited to a certain extent, an obvious etching step between the zinc layer and a substrate is avoided, and a clear zinc-iron alloy coating structure is obtained.
Drawings
FIG. 1 is a structural drawing of a Zn-Fe alloy coating layer obtained in the example of the present invention
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
The sample for performing the phase structure corrosion study on the coating of the zinc-iron alloy hot-dip galvanized steel sheet is a DX51D + ZF steel sheet, the alloying temperature of the steel sheet is 550 ℃, and the Al content in a zinc pot is 0.14 percent. After diffraction analysis, the plating structure of the coating consists of a gamma phase and a delta phase.
Taking a zinc-iron alloy hot-dip galvanized steel plate with the size of 20mm by 20mm, and carrying out cross section inlaying, grinding and polishing on a sample.
Respectively preparing 1-2% nitric acid alcoholic solution and 1-2% picric acid alcoholic solution, mixing the nitric acid alcoholic solution and the picric acid alcoholic solution with equal volumes, and standing to room temperature.
The polished sample is etched for about 10 seconds by the mixed solution to obtain a clear zinc-iron alloy coating structure, and the result is shown in fig. 1.
Comparative example 1
The volume ratio of the 1-2% nitric acid alcohol solution to the 1-2% picric acid alcohol solution in example 1 was changed from 1-1.2:1 to 2:1, and the resulting zinc-iron alloy plating structure was as shown in fig. 2, in which Γ phase, Γ 1, and δ phase were partially distinguishable, but Γ phase was more deeply corroded.
Comparative example 2
The volume concentrations of the 1-2% nitric acid alcohol solution and the 1-2% picric acid alcohol solution in example 1 were replaced by the volume concentrations of the 0.5% nitric acid alcohol solution and the 0.5% picric acid alcohol solution, and the erosion time was replaced by 20s, so that the obtained zinc-iron alloy coating structure is shown in fig. 3, from which it can be seen that the corrosion pits are relatively serious, but the coating structure is not clearly shown.
Comparative example 3
The mixed solution of 1-2% nitric acid alcohol solution and 1-2% picric acid alcohol solution in example 1 is replaced by only 1-2% nitric acid alcohol solution, and the obtained zinc-iron alloy plating layer structure is shown in fig. 4, and it can be seen from the figure that the excessive etching phenomenon of most regions is serious, obvious etching pits are formed, the edge of the plating layer is etched seriously, and obvious steps are formed between the plating layer and the substrate and the protective layer.
The above detailed description of an etchant for showing the coating structure of a zinc-iron alloy hot-dip galvanized steel sheet and a method for preparing and using the same with reference to the embodiments is illustrative and not restrictive, and several embodiments may be enumerated within the scope defined, so that variations and modifications thereof may be made without departing from the general inventive concept within the scope of the present invention.

Claims (5)

1. The corrosive agent for displaying the coating structure of the zinc-iron alloy hot-dip galvanized steel sheet is characterized by consisting of a nitric acid alcohol solution and a picric acid alcohol solution.
The volume ratio of the nitric acid alcohol solution to the picric acid alcohol solution is 1-1.2: 1;
the volume concentration of the nital solution is 1-2%;
the mass concentration of the picric acid alcohol solution is 1-2%.
2. The etchant for displaying the coating structure of a zinc-iron alloy hot-dip galvanized steel sheet according to claim 1, wherein the alcohol used for preparing the nitric acid alcohol solution and picric acid alcohol solution is absolute ethyl alcohol.
3. The method for preparing an etchant for displaying a coating structure of a zinc-iron alloy hot-dip galvanized steel sheet according to claim 1 or 2, wherein the aqueous solution of nitric acid and the aqueous solution of picric acid are directly mixed to be uniform.
4. The use method of the corrosive agent for displaying the coating structure of the zinc-iron alloy hot-dip galvanized steel sheet according to claim 1 or 2, characterized in that after grinding and polishing the cross section of the zinc-iron alloy hot-dip galvanized steel sheet sample, the clear zinc-iron alloy coating structure can be obtained by etching with the corrosive agent.
5. Use according to claim 4, characterized in that the etching time is 10-20 seconds.
CN201910620362.3A 2019-07-10 2019-07-10 Corrosive agent for displaying coating structure of zinc-iron alloy hot-dip galvanized steel sheet and preparation and use methods thereof Active CN110344060B (en)

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