CN106525542A - Etching agent for displaying macrostructure of low-carbon steel continuous casting and preparation method - Google Patents

Etching agent for displaying macrostructure of low-carbon steel continuous casting and preparation method Download PDF

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Publication number
CN106525542A
CN106525542A CN201611177859.5A CN201611177859A CN106525542A CN 106525542 A CN106525542 A CN 106525542A CN 201611177859 A CN201611177859 A CN 201611177859A CN 106525542 A CN106525542 A CN 106525542A
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CN
China
Prior art keywords
reagent
macrostructure
low
content
nitric acid
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Pending
Application number
CN201611177859.5A
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Chinese (zh)
Inventor
杨鑫
于景坤
唐广鹏
靳恩东
刘朝阳
侯星慧
温天朋
张小芳
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Northeastern University China
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Northeastern University China
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Application filed by Northeastern University China filed Critical Northeastern University China
Priority to CN201611177859.5A priority Critical patent/CN106525542A/en
Publication of CN106525542A publication Critical patent/CN106525542A/en
Pending legal-status Critical Current

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Classifications

    • 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
    • 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
    • C23F1/28Acidic compositions for etching iron group metals

Abstract

The invention discloses an etching agent for displaying a macrostructure and defects of a low-carbon steel or ultra-low carbon steel continuous casting and a preparation method. The etching agent is prepared from the following components: 1.5 to 6.0g of magnesium chloride (MgCl2.6H2O), 1.0 to 5.0g of cuprous chloride (CuCl.2H20), 1,000 to 1,200ml of deionized water, 30 to 200ml of nitric acid, 50 to 300ml of absolute ethanol (C2H5OH) and 10 to 100ml of sodium dodecyl benzene sulfonate (C18H29NaO3S). The etching agent is prepared according to a certain preparation method. The etching agent has the advantages of high efficiency, high operability, high safety coefficient and low cost, and can clearly display the macrostructure and defect forms of the low-carbon steel or ultra-low carbon steel continuous casting.

Description

A kind of corrosion reagent and preparation method for showing low-carbon (LC) steel continuous casting billet macrostructure
Technical field
This invention belong to ferrous metallurgy materials analysis agents useful for same technical field, and in particular to for show mild steel or Corrosion reagent of continuous casting of ultralow carbon steel base macrostructure and defect and preparation method thereof.
Background technology
In steelmaking process for the inspection of continuous casting steel billet be ensure slab quality important step, macroscopic examination technology It is one of important means of continuous casting billet quality inspection, its method is easy, can judge to quicklook billet quality and steel Internal defect that may be present.At present, the method for inspection of continuous casting billet macrostructure have sulphur print, hot aciding, cold aciding and Electrolytic etching method etc..Sulphur print therein mainly reflects the segregation status of sulphur in steel, can not show substantially the low power crystal grain group of steel Knit, and with the reduction of sulfur content in steel, the further reduction of sulphide inculsion, the application of sulphur print are subject to certain limitation; Hot acid etch corrosive power is strong, can clearly show that macrostructure defect, but some mild steel or ultra-low-carbon steel are connected The tissue morphology display capabilities of strand are not enough, and the heating-up temperature and soak time of hot acid etch is difficult to control, and easily occurs rotten Erosion is not enough or excessive corrosion, and defect is not fully shown that defect is artificially amplified sometimes sometimes;Cold acid etching method belongs to selective Corrosion, it is not necessary to descaling bath and heater, erosion degree are easier to grasp, and the defect of steel is more serious, segregation is more severe, corrosion effect Fruit is better, and for ultra-low-carbon steel, does not almost have what segregation as C, S, P element content are all relatively low, general cold aciding It is also not enough to macrostructure and defect display capabilities;And galvano-cautery method need to use special equipment, restrictive condition is more.
Not enough and cold acid corrosion macrostructure based on the macrostructure corrosion technology of current mild steel or ultra-low-carbon steel Corrosion reagent it is rare, this invention provides that a kind of efficiency is fast, workable, safety coefficient is high, low cost, and can be clear Show the macrostructure corrosion tests of macrostructure form, solve tradition or some caustic solutions be not at present Foot, is that production scene or laboratory search out a kind of economical and effective, easily operated continuous casting steel billet quality inspection method.
The content of the invention
This invention is corroded to mild steel or continuous casting of ultralow carbon steel base sample using specific cold acid corrosion reagent, Macrostructure and defect that observation base sample surface shows, solving hot aciding, the cold aciding in part and sulphur print can not be complete Or the problem of mild steel or ultra-low-carbon steel macrostructure and defect cannot be shown.
This invention is a kind of cold acid type corrosion reagent for detecting mild steel or ultra-low-carbon steel macrostructure and defect, Its composition includes magnesium chloride (MgCl2·6H2O), stannous chloride (CuCl 2H2O), deionized water, nitric acid, absolute ethyl alcohol (C2H5) and neopelex (C OH18H29NaO3S), concrete formulation content is:
Its constituent is as follows:
Wherein the percent concentration of nitric acid is 60~70%, absolute ethyl alcohol (C2H5OH percent concentration) is 99%.
The corrosion reagent of this invention is prepared as follows according to aforementioned ratio:
(1) weigh a number of magnesium chloride (MgCl2·6H2O), stannous chloride (CuCl 2H2O fill in) being put into container A Divide and be well mixed;
(2) take in a certain amount of deionized water addition container A, vibrate and stand the magnesium chloride in wait container A and chlorination Cuprous abundant dissolving;
(3) another extracting container B adds a certain amount of nitric acid (68% mass percent) and absolute ethyl alcohol (C2H5OH), and by nitre Acid and absolute ethyl alcohol (C2H5OH mixed solution) is poured in container A, is eventually adding quantitative neopelex (C18H29NaO3S) reagent, mixes reagent by mechanical oscillation, at drying stands 2~3 hours.
This invention prepares etchant solution with nitric acid as main component with deionized water, according to the carbon in steel during preparation Content adjusting the content of magnesium chloride, stannous chloride and neopelex, to improve corrosion rate.Detergent alkylate Sodium sulfonate is a kind of conventional surfactant, can increase the wetness degree of reaction reagent and steel billet matrix, promotes corrosion anti- The carrying out answered.
The corrosion reagent completed by this invention is directed to the continuous casting billet surface macrostructure of mild steel or ultra-low-carbon steel and lacks Use during sunken detection, which has the advantage that:
(1) can be by routine macrostructure defect such as steel billet macrostructure and center segregation, center porosity and bubble etc. Clearly, intactly show, and the continuous casting steel billet relatively low to the harmful element content such as S, P can also give and clearly display;
(2) corrosion reagent using this invention is not high to the smoothness requirements on the surface of sample, and corrosion rate is fast, corrosion Time is short, and will not form precipitation membrane;
It is (3) simple to operate, it is easy to accomplish, and pollute few, testing cost is substantially reduced.
Description of the drawings
Accompanying drawing 1,2 and 3 is respectively using ultra-low-carbon steel and the low-carbon (LC) steel continuous casting billet cross section of the corrosion of this invention embodiment Local macrostructure aspect graph.Wherein:
Macroscopical macrostructures of the Fig. 1 for Ultra-low carbon car inner plate continuous casting billet sample;
Partial enlarged drawings of the Fig. 2 for Fig. 1;
Local organization defects of the Fig. 3 for low-carbon (LC) acid-cleaning plate continuous casting billet sample.
Specific embodiment
This invention is conducted further description with reference to 2 embodiments.
Embodiment 1
For showing the corrosion examination of the relatively low ultra-low-carbon steel car inner plate continuous casting billet macrostructure form inspection of S, P content Agent, its composition are as follows:
The corrosion reagent of the above composition is prepared in accordance with the following steps:
(1) weigh 5g magnesium chloride and 2.5g stannous chloride add volume for 2000ml container A in and be sufficiently mixed;
(2) deionized water for taking 1000ml is poured in beaker A, vibrates and stand the magnesium chloride in wait container A and chlorination Cuprous abundant dissolving;
(3) the beaker B of 1000ml is separately taken, nitric acid and 100ml percent concentrations that 76ml concentration is 68% is added thereto to For 99% absolute ethyl alcohol, pour into after being sufficiently mixed in container A, in most backward container A, add the DBSA of 20ml Sodium, is mixed by mechanical oscillation, the reagent for preparing is placed on the place of drying and stands 2 hours in case using.
By the low-carbon (LC) car inner plate continuous casting billet specimen surface of certain steel mill's continuous casting workshop cutting after polishing, polishing, Preservative film is closely pasted in steel billet surrounding with glue, then twined with adhesive tape.Corrosion reagent is directly poured in said sample On surface, make surface by reagent it is uniform, fully soak, and constantly wiped with absorbent cotton, place 6min, treat that naked eyes can be clearly See tissue morphology that surface occurs or during defect, scrubbed with warm water, alcohol immediately, finally dried up with air duct, then with guarantor Whole surface is sealed by fresh film, anti-oxidation.
Embodiment 2
For showing the corrosion reagent of the continuous casting billet macrostructure form inspection of low-carbon (LC) acid-cleaning plate, its composition is as follows:
The corrosion reagent of the above composition is prepared in accordance with the following steps:
(1) stannous chloride for weighing the magnesium chloride and 1.5g of 5g adds volume in the container A of 2000ml;
(2) deionized water for taking 1200ml is poured in beaker A, vibrates and stand the magnesium chloride in wait container A and chlorination Cuprous abundant dissolving;
(3) container B of 1000ml is separately taken, it is 99% to be added thereto to nitric acid that 55ml concentration is 68% and 75ml concentration Absolute ethyl alcohol, pours into after being sufficiently mixed in container A, adds the neopelex of 10ml, by machine in most backward container A Tool vibration is mixed, and the reagent for preparing is placed on the place of drying and stands 2.5 hours in case using.
By the low-carbon (LC) acid-cleaning plate continuous casting billet specimen surface of certain steel mill's continuous casting workshop cutting after polishing, polishing, use Preservative film is closely pasted by glue in steel billet surrounding, then is twined with adhesive tape.Corrosion reagent is directly poured in said sample table On face, make surface by reagent it is uniform, fully soak, and constantly wiped with absorbent cotton, through 4~6min, treat that naked eyes can be clear See tissue morphology that surface occurs or during defect, scrubbed with warm water, alcohol immediately, finally dried up with air duct, then used Whole surface is sealed by preservative film, anti-oxidation.

Claims (3)

1. a kind of corrosion reagent for detecting mild steel macrostructure and defect, its composition include:Magnesium chloride, stannous chloride, Deionized water, nitric acid, absolute ethyl alcohol and neopelex, wherein, content of magnesium chloride is 1.5g~6.0g, stannous chloride Content is 1.0g~5.0g, deionized water content is 1000ml~1200ml, nitric acid content is 30ml~200ml, absolute ethyl alcohol Content is 50ml~300ml, sodium dodecyl benzene sulfonate content is 10ml~100ml.
2. a kind of corrosion reagent for detecting mild steel macrostructure and defect according to claim 1, its feature exist In the percent concentration of nitric acid described in reagent is 60~70%, and the percent concentration of absolute ethyl alcohol is 99%.
3. a kind of preparation side for detecting the corrosion reagent of mild steel macrostructure and defect according to claim 1 Method, it is characterised in that this kind of reagent is prepared in accordance with the following steps according to composition and ratio described in claim 1:
(1) weigh a number of magnesium chloride, stannous chloride to be sufficiently mixed in being put into container A uniformly;
(2) take in a certain amount of deionized water addition container A, vibrate and stand the magnesium chloride and stannous chloride in wait container A Fully dissolve;
(3) another extracting container B adds a certain amount of nitric acid and absolute ethyl alcohol, and pours the mixed solution of nitric acid and absolute ethyl alcohol into appearance In device A, quantitative neopelex reagent is eventually adding, mixes reagent by mechanical oscillation, 2 are stood at drying ~3 hours.
CN201611177859.5A 2016-12-19 2016-12-19 Etching agent for displaying macrostructure of low-carbon steel continuous casting and preparation method Pending CN106525542A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110863200A (en) * 2019-11-14 2020-03-06 德龙钢铁有限公司 Low-carbon strip steel microstructure etching agent
CN112649270A (en) * 2018-09-17 2021-04-13 沈阳市启光科技有限公司 Corrosive agent for dendritic crystal corrosion macroscopic examination

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JP2014198862A (en) * 2013-03-29 2014-10-23 大同特殊鋼株式会社 Colored etchant and etching method capable of identifying retained austenite from other structure

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CN101576512A (en) * 2008-05-09 2009-11-11 耿红燕 Cold etching liquid (reagent) for rapidly displaying internal structural flaw of steel
CN102023112A (en) * 2009-09-18 2011-04-20 鞍钢股份有限公司 Corrosive capable of displaying ultra low carbon steel solidification arborescent structure and preparation method thereof
CN102401759A (en) * 2010-09-07 2012-04-04 鞍钢股份有限公司 Freeze-etching agent of ultra-low-carbon steel casting billet macrograph grain structure, and preparation method thereof
JP2014198862A (en) * 2013-03-29 2014-10-23 大同特殊鋼株式会社 Colored etchant and etching method capable of identifying retained austenite from other structure

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112649270A (en) * 2018-09-17 2021-04-13 沈阳市启光科技有限公司 Corrosive agent for dendritic crystal corrosion macroscopic examination
CN110863200A (en) * 2019-11-14 2020-03-06 德龙钢铁有限公司 Low-carbon strip steel microstructure etching agent
CN110863200B (en) * 2019-11-14 2021-11-26 德龙钢铁有限公司 Low-carbon strip steel microstructure etching agent

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Application publication date: 20170322