CN109211647A - The galvanized sheet corrosive agent of titanium containing vanadium and its preparation and application - Google Patents
The galvanized sheet corrosive agent of titanium containing vanadium and its preparation and application Download PDFInfo
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- CN109211647A CN109211647A CN201811209091.4A CN201811209091A CN109211647A CN 109211647 A CN109211647 A CN 109211647A CN 201811209091 A CN201811209091 A CN 201811209091A CN 109211647 A CN109211647 A CN 109211647A
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- galvanized sheet
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- 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
- G01N1/32—Polishing; Etching
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23F—NON-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
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/28—Acidic compositions for etching iron group metals
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23F—NON-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
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/30—Acidic compositions for etching other metallic material
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Abstract
The invention belongs to metallographic grain size detection technique fields, and in particular to one kind galvanized sheet corrosive agent of titanium containing vanadium and its preparation and application.When corroding the galvanized sheet of titanium containing vanadium for existing corrosive agent, corrode the problems such as obtained grain structure is unintelligible, the present invention provides a kind of galvanized sheet corrosive agent of titanium containing vanadium, by solution A and hydrogen peroxide solution, 1 ︰ 1~3 is mixed by volume, and wherein solution A forms are as follows: the water of the oxalic acid of 6~10 parts by weight, the concentrated sulfuric acid of 3~9 parts by volume and 80~140 parts by volume.The present invention also provides the caustic solutions of above-mentioned corrosive agent, comprising the following steps: takes the galvanized sheet of titanium containing vanadium, dips above-mentioned corrosive agent with absorbent cotton after cleaning, be wiped repeatedly the zinc-plated plate surface of titanium containing vanadium, until surface becomes silver gray.Corrosive agent of the invention can improve corrosive effect, can obtain clearly grain structure.Caustic solution of the invention is easy to operate, reproducible, provides effective method for metal lographic examination.
Description
Technical field
The invention belongs to metallographic grain size detection technique fields, and in particular to one kind galvanized sheet corrosive agent of titanium containing vanadium and its system
Standby and application method.
Background technique
Vanadium titanium finds broad application in the steel industry as a kind of alloy addition element.Galvanized sheet is good because having
A variety of excellent characteristics such as corrosion resisting property, coating performance, welding performance and appearance property, are widely used in every profession and trade, especially
It is automobile industry, galvanized sheet has become one of most popular plate on automobile.However, in the production of the galvanized sheet of titanium containing vanadium
Cheng Zhong, the surface of galvanized sheet often will appear various defects, and the generation of these defects and production technology are closely related.Therefore, divide
It is imperative to analyse defect Producing reason.Wherein, the grain size for observing material is one of important content of Metallographic Analysis, existing
The display effect of V-Ti metallographic structure is bad, brings many difficulties to production and inspection body.
Therefore, when carrying out the test of the galvanized sheet grain size of titanium containing vanadium, usually first to be corroded with corrosive agent.It is common rotten
Erosion agent has FeCl3HCl solution, chloroazotic acid etc., but existing corrosive agent corrosive effect is bad, and obtained grain structure is unsharp to ask
Topic.
Summary of the invention
The technical problem to be solved in the present invention are as follows: when the existing corrosive agent corrosion galvanized sheet of titanium containing vanadium, the crystal grain that corrodes
Organize the problems such as unintelligible.
The technical solution of present invention solution above-mentioned technical problem are as follows: a kind of galvanized sheet corrosive agent of titanium containing vanadium is provided.The corrosion
By solution A and hydrogen peroxide solution, 1 ︰ 1~3 is mixed by volume for agent, and wherein solution A forms are as follows: the grass of 6~10 parts by weight
The water of acid, the concentrated sulfuric acid of 3~9 parts by volume and 80~140 parts by volume.
Wherein, in the above-mentioned galvanized sheet of titanium containing vanadium corrosive agent, the concentration of the concentrated sulfuric acid is 95~98wt%.
Wherein, in the above-mentioned galvanized sheet of titanium containing vanadium corrosive agent, the volumetric concentration of the hydrogen peroxide is 30~40%.
Preferably, in the above-mentioned galvanized sheet of titanium containing vanadium corrosive agent, the water in the solution A is distilled water.
Wherein, when the unit of the parts by weight is gram, the unit of the parts by volume is milliliter；When the unit of the parts by weight
For kilogram when, the unit of the parts by volume is to rise.
The present invention also provides a kind of preparation methods of the above-mentioned galvanized sheet of titanium containing vanadium corrosive agent, comprising the following steps:
The oxalic acid of 6~10 parts by weight is weighed, the concentrated sulfuric acid of 3~9 parts by volume is added in the water of 80~140 parts by volume, mixes
It is even, obtain solution A；Solution A ︰ hydrogen peroxide solution=1 ︰ 1~3 measures solution A and hydrogen peroxide by volume again, mixes, is contained
Vanadium titanium galvanized sheet corrosive agent.
The present invention also provides a kind of application methods of the above-mentioned galvanized sheet of titanium containing vanadium corrosive agent, comprising the following steps:
The galvanized sheet of titanium containing vanadium is taken, above-mentioned corrosive agent is dipped with absorbent cotton after cleaning, is wiped repeatedly the zinc-plated plate surface of titanium containing vanadium,
Until surface becomes silver gray.
It further, further include cleaning, dry step after wiping in the application method of the above-mentioned galvanized sheet of titanium containing vanadium corrosive agent
Suddenly.
Further, in the application method of the above-mentioned galvanized sheet of titanium containing vanadium corrosive agent, after the cleaning is first rinses with clear water,
It is cleaned again with dehydrated alcohol or boiling water.
The invention has the benefit that
The present invention provides a kind of galvanized sheet corrosive agent of titanium containing vanadium, which can improve corrosive effect, can obtain clear
Clear grain structure.The present invention also provides the caustic solution using above-mentioned corrosive agent to the galvanized sheet of titanium containing vanadium, this method operations
Simply, reproducible, effective method is provided for metal lographic examination.
Detailed description of the invention
Fig. 1 is the etching pit pattern of the sample containing V-Ti of the embodiment of the present invention 1；
Fig. 2 is the etching pit pattern of the sample containing V-Ti of the embodiment of the present invention 2；
Fig. 3 is the etching pit pattern of the sample containing V-Ti of the embodiment of the present invention 3；
Fig. 4 is etching pit pattern of the comparative example 4 of the present invention using the existing corrosive sample containing V-Ti；
Fig. 5 is comparative example 5 of the present invention using the gold for corroding the galvanized sheet of titanium containing vanadium sample when matching not within the scope of the present invention
Phase erosion profile.
Specific embodiment
The present invention provides a kind of galvanized sheet corrosive agent of titanium containing vanadium, by solution A and hydrogen peroxide solution 1 ︰ 1~3 by volume
It mixes, wherein solution A forms are as follows: the oxalic acid of 6~10 parts by weight, the concentrated sulfuric acid of 3~9 parts by volume and 80~140 parts by volume
Water.
Wherein, in the above-mentioned galvanized sheet of titanium containing vanadium corrosive agent, the volumetric concentration of the concentrated sulfuric acid is 95~98wt%.
Wherein, in the above-mentioned galvanized sheet of titanium containing vanadium corrosive agent, the volumetric concentration of the hydrogen peroxide is 30~40%.
Wherein, in the above-mentioned galvanized sheet of titanium containing vanadium corrosive agent, the water in the solution A is distilled water.
Wherein, in the above-mentioned galvanized sheet of titanium containing vanadium corrosive agent, when the unit of the parts by weight is gram, the unit of the parts by volume
For milliliter；When the unit of the parts by weight is kilogram, the unit of the parts by volume is to rise.
Contain vanadium, titanium, the zinc-plated metal plate in surface in the chemical component that the galvanized sheet of titanium containing vanadium of the invention refers to.Inventor
When being corroded using existing corrosive agent to the galvanized sheet of titanium containing vanadium, discovery corrosive effect is bad, the crystal grain group corroded
It knits unintelligible.For this purpose, inventor screens corrosive agent.Inventor has selected oxalic acid and the concentrated sulfuric acid prepares corrosive agent, hair
Existing oxalic acid and concentrated sulfuric acid mixing absolutely not corrosive effect.Accidental, inventor joined portion in oxalic acid, concentrated sulfuric acid mixture
Divide hydrogen peroxide, as a result, it has been found that having restored the corrosiveness to the galvanized sheet of titanium containing vanadium again.Analysis reason may be because of are as follows: dioxygen
Water plays oxidation, and the oxidisability of hydrogen peroxide is also stronger in acid stronger solution, and it is zinc-plated that dioxygen water energy will contain vanadium titanium
Plate superficial oxidation, to obtain clearly organization chart picture.
Therefore, inventor has finally determined the oxalic acid when 6~10 parts by weight, 3~9 volumes by a large amount of experiments repeatedly
After the concentrated sulfuric acid of part and the water mixing of 80~140 parts by volume, 1~3 times of overall solution volume of hydrogen peroxide is added, it is molten after preparation
Liquid has preferable corrosivity, and the grain structure that corrosion can be made to obtain is apparent.Each ingredient of corrosive agent of the present invention cooperates,
Collective effect, only within the scope of said ratio, the corrosive effect that has just finally achieved.
The present invention also provides a kind of preparation methods of the above-mentioned galvanized sheet of titanium containing vanadium corrosive agent, comprising the following steps:
The oxalic acid of 6~10 parts by weight is weighed, the concentrated sulfuric acid of 3~9 parts by volume is added in the water of 80~140 parts by volume, mixes
It is even, obtain solution A；Solution A ︰ hydrogen peroxide solution=1 ︰ 1~3 measures solution A and hydrogen peroxide by volume again, mixes, is contained
Vanadium titanium galvanized sheet corrosive agent.
The present invention also provides a kind of application methods of the galvanized sheet of titanium containing vanadium corrosive agent, comprising the following steps:
The galvanized sheet of titanium containing vanadium is taken, above-mentioned corrosive agent is dipped with absorbent cotton after cleaning, is wiped repeatedly the zinc-plated plate surface of titanium containing vanadium,
Until surface becomes silver gray.
It further, further include cleaning, dry step after wiping in the application method of the above-mentioned galvanized sheet of titanium containing vanadium corrosive agent
Suddenly.
Further, in the application method of the above-mentioned galvanized sheet of titanium containing vanadium corrosive agent, after the cleaning is first rinses with clear water,
It is cleaned again with dehydrated alcohol or boiling water.
Explanation will be further explained to a specific embodiment of the invention by embodiment below, but do not indicated this
The protection scope of invention is limited in range described in embodiment.
Embodiment 1 corrodes the galvanized sheet of titanium containing vanadium with corrosive agent of the present invention
At room temperature, it weighs 6g oxalic acid to be placed in a beaker, measures the 4ml concentrated sulfuric acid respectively and 80ml distilled water is put into added with oxalic acid
Beaker in, be uniformly mixing to obtain solution A；30% hydrogen peroxide solution for measuring 84ml obtains solution B, and solution A and solution B are filled
Divide to be uniformly mixed and obtains corrosive agent.Full corrosive agent is dipped in absorbent cotton, is wiped repeatedly the zinc-plated plate surface of titanium containing vanadium, until surface occurs
Silver gray, then surface is rinsed well with clear water, finally dried up with washes of absolute alcohol, it is big in metallography microscope microscopic observation grain size
It is small.Etching pit shape appearance figure is shown in Fig. 1.
Embodiment 2 corrodes the galvanized sheet of titanium containing vanadium with corrosive agent of the present invention
At room temperature, it weighs 8g oxalic acid to be placed in a beaker, measures the 5ml concentrated sulfuric acid respectively and 100ml distilled water is put into added with grass
In the beaker of acid, it is uniformly mixing to obtain solution A；30% hydrogen peroxide solution for measuring 100ml obtains solution B, by solution A and solution
B, which is sufficiently mixed, uniformly obtains corrosive agent.Full corrosive agent is dipped in absorbent cotton, is wiped repeatedly the zinc-plated plate surface of titanium containing vanadium, until surface
There is silver gray, then rinse surface well with clear water, is finally dried up with washes of absolute alcohol, in metallography microscope microscopic observation crystal grain
Spend size.Etching pit shape appearance figure is shown in Fig. 2.
Embodiment 3 corrodes the galvanized sheet of titanium containing vanadium with corrosive agent of the present invention
At room temperature, it weighs 10kg oxalic acid to be placed in a beaker, measures the 8L concentrated sulfuric acid respectively and 130L distilled water is put into added with grass
In the beaker of acid, it is uniformly mixing to obtain solution A；30% hydrogen peroxide solution for measuring 130L obtains solution B, by solution A and solution B
It is sufficiently mixed and uniformly obtains corrosive agent.Full corrosive agent is dipped in absorbent cotton, is wiped repeatedly the zinc-plated plate surface of titanium containing vanadium, until surface goes out
Existing silver gray, then surface is rinsed well with clear water, it is finally dried up with washes of absolute alcohol, in metallography microscope microscopic observation grain size
Size.Etching pit shape appearance figure is shown in Fig. 3.
Comparative example 4 corrodes the galvanized sheet of titanium containing vanadium using existing corrosive agent
Using existing corrosive agent FeCl3HCl solution (mass-volume concentration 3%) corrodes the galvanized sheet of titanium containing vanadium, obtains
Result as shown in Figure 4.Fig. 4 shows, existing corrosive agent FeCl3After the corrosion of~HCl solution, the galvanized sheet surface portion of titanium containing vanadium
Ferrite grain boundaries, which do not corrode, to be come out, and corrosion interface is unintelligible, and effect is bad.
Comparative example 5 corrodes the galvanized sheet of titanium containing vanadium when matching not within the scope of the present invention
At room temperature, it weighs 4g oxalic acid to be placed in a beaker, measures the 2mL concentrated sulfuric acid respectively and 60mL distilled water is put into added with oxalic acid
Beaker in, be uniformly mixing to obtain solution A；30% hydrogen peroxide solution for measuring 60mL obtains solution B, and solution A and solution B are filled
Divide to be uniformly mixed and obtains corrosive agent.Full corrosive agent is dipped in absorbent cotton, is wiped repeatedly the zinc-plated plate surface of titanium containing vanadium, until surface occurs
Silver gray, then surface is rinsed well with clear water, finally dried up with washes of absolute alcohol, it is big in metallography microscope microscopic observation grain size
It is small.Etching pit shape appearance figure is shown in Fig. 5.
By Examples 1 to 3 and comparative example 4,5 it is found that using the galvanized sheet corrosive agent of titanium containing vanadium of the invention and caustic solution,
Available clearer goldc grains tissue.Caustic solution of the present invention is easy to operate, convenient to carry out, is suitable for promoting the use of.
Claims (9)
1. the galvanized sheet corrosive agent of titanium containing vanadium, it is characterised in that: by 1 ︰ 1~3 mixing by volume of solution A and hydrogen peroxide solution
At wherein solution A forms are as follows: the water of the oxalic acid of 6~10 parts by weight, the concentrated sulfuric acid of 3~9 parts by volume and 80~140 parts by volume.
2. the galvanized sheet of titanium containing vanadium corrosive agent according to claim 1, it is characterised in that: the concentration of the concentrated sulfuric acid be 95~
98wt%.
3. the galvanized sheet of titanium containing vanadium corrosive agent according to claim 1, it is characterised in that: the volumetric concentration of the hydrogen peroxide is
30~40%.
4. the galvanized sheet of titanium containing vanadium corrosive agent according to claim 1, it is characterised in that: the water in the solution A is distillation
Water.
5. the galvanized sheet of titanium containing vanadium corrosive agent according to claim 1, it is characterised in that: the unit of the parts by weight is gram
When, the unit of the parts by volume is milliliter；When the unit of the parts by weight is kilogram, the unit of the parts by volume is to rise.
6. the preparation method of the described in any item galvanized sheet of titanium containing the vanadium corrosive agent of Claims 1 to 5, comprising the following steps:
The oxalic acid of 6~10 parts by weight is weighed, the concentrated sulfuric acid of 3~9 parts by volume is added in the water of 80~140 parts by volume, mixes, obtains
To solution A；Solution A ︰ hydrogen peroxide solution=1 ︰ 1~3 measures solution A and hydrogen peroxide by volume again, mixes, and obtains the plating of titanium containing vanadium
Zine plate corrosive agent.
7. the application method of the described in any item galvanized sheet of titanium containing the vanadium corrosive agent of Claims 1 to 5, which is characterized in that including with
Lower step:
The galvanized sheet of titanium containing vanadium is taken, above-mentioned corrosive agent is dipped with absorbent cotton after cleaning, is wiped repeatedly the zinc-plated plate surface of titanium containing vanadium, until
Surface becomes silver gray.
8. the application method of the galvanized sheet of titanium containing vanadium corrosive agent according to claim 7, it is characterised in that: further include after wiping
Cleaning, dry step.
9. the application method of the galvanized sheet of titanium containing vanadium corrosive agent according to claim 8, it is characterised in that: the cleaning is first
After being rinsed with clear water, then cleaned with dehydrated alcohol or boiling water.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811209091.4A CN109211647B (en) | 2018-10-17 | 2018-10-17 | Corrosion agent for vanadium-titanium-containing galvanized plate and preparation and use methods thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811209091.4A CN109211647B (en) | 2018-10-17 | 2018-10-17 | Corrosion agent for vanadium-titanium-containing galvanized plate and preparation and use methods thereof |
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| CN109211647B CN109211647B (en) | 2021-06-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113913827A (en) * | 2021-09-09 | 2022-01-11 | 东风汽车集团股份有限公司 | Quenching and tempering zinc-plated carbon steel metallographic corrosive agent and application thereof |
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| CN101140271A (en) * | 2007-10-10 | 2008-03-12 | 攀钢集团攀枝花钢铁研究院 | Galvanizing plate layered detecting method |
| CN102680304A (en) * | 2012-05-04 | 2012-09-19 | 东北电力科学研究院有限公司 | Method for rapidly displaying titaniferous inclusions in field condition based on corrosion principle |
| CN105136629A (en) * | 2015-08-24 | 2015-12-09 | 首钢总公司 | Display method of zinc crystal grains on the surface of galvanizing plate |
| CN106323721A (en) * | 2016-11-23 | 2017-01-11 | 武汉钢铁股份有限公司 | Galvanized sheet surface defect analysis method |
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2018
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Patent Citations (4)
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| CN101140271A (en) * | 2007-10-10 | 2008-03-12 | 攀钢集团攀枝花钢铁研究院 | Galvanizing plate layered detecting method |
| CN102680304A (en) * | 2012-05-04 | 2012-09-19 | 东北电力科学研究院有限公司 | Method for rapidly displaying titaniferous inclusions in field condition based on corrosion principle |
| CN105136629A (en) * | 2015-08-24 | 2015-12-09 | 首钢总公司 | Display method of zinc crystal grains on the surface of galvanizing plate |
| CN106323721A (en) * | 2016-11-23 | 2017-01-11 | 武汉钢铁股份有限公司 | Galvanized sheet surface defect analysis method |
Non-Patent Citations (1)
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| 迟少宁: "应用化学抛光法检查钢的正火晶粒度", 《物理测试》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113913827A (en) * | 2021-09-09 | 2022-01-11 | 东风汽车集团股份有限公司 | Quenching and tempering zinc-plated carbon steel metallographic corrosive agent and application thereof |
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