CN105316685A - Cold etching agent capable of displaying pattern segregation of bearing steel casting blank and preparation method thereof - Google Patents
Cold etching agent capable of displaying pattern segregation of bearing steel casting blank and preparation method thereof Download PDFInfo
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- CN105316685A CN105316685A CN201410335598.XA CN201410335598A CN105316685A CN 105316685 A CN105316685 A CN 105316685A CN 201410335598 A CN201410335598 A CN 201410335598A CN 105316685 A CN105316685 A CN 105316685A
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Abstract
The invention discloses a cold etching agent capable of displaying the pattern segregation of bearing steel casting blank. The cold etching agent is composed of 4 to 6 grams of trinitrophenol, 7 to 12 grams of iron trichloride, 15 to 30 mL of nitric acid, 15 to 30 mL of hydrochloric acid, and 300 to 400 mL of distilled water. The preparation method comprises the following steps: placing a certain amount of solid trinitrophenol and iron trichloride in a glass container, adding 200 mL of distilled water, dissolving the solid agents; then adding nitric acid and hydrochloric acid into the water solution of trinitrophenol and iron trichloride, evenly stirring, then adding the residual distilled water, and fully stirring to obtain the cold etching agent. The provided cold etching agent has the advantages that the detection speed is quick, the pollution is little, the energy is saved, the operation is convenient, the positions, distribution pattern, and morphology of macrostructure pattern segregation of bearing steel blank can be clearly displayed, the contrast effect is prominent; the edge of the pattern segregation, which flows along with the blank casting, is clear, the positioning is accurate, and the leak detection is effectively avoided.
Description
Technical field
The invention belongs to metallurgical material analytical study field, particularly a kind of cold erosion agent for showing pattern segregation defect in bearing steel strand macrostructure and compound method thereof.
Background technology
In continuous casting square billet macrostructure, pattern segregation defect is the comparatively common defect of strand, when segregation is serious, after rolling into pole, wire rod, still can be present in the center of stocking, affect interiors of products quality and use properties.To hot rolled rod, the existence of pattern segregation, causes the tissue at cross section edge and center to occur notable difference, and some other defects are assembled in line of segragation, in the follow-up operation of rolling, affect technology controlling and process, forms waste product.Wire product is produced, on the pattern segregation of strand can be genetic to and finally become a useful person, forms wire rod even central tissue's segregation of steel wire, wire rod tissue is occurred abnormal.Add at parts such as bearings and occur serious cracking phenomena man-hour, worsen mechanical property and the deep shaping property of product.
Eliminate the key of bearing steel continuous casting square billet pattern segregation defect, first be will by effective caustic solution reproducing steel billet pattern segregation severity fully truly in steel billet inspection, timely handshake result, controls smelting technology, guarantees that segregation defects does not bring rolling process below into.Usually the macro defects such as low power hot acid loses, the pattern segregation of sulphur print inspection steel billet are adopted at present.Chemico-analytic constituent content assay method as a supplement laboratory facilities is also usually used.The hot aciding corrosive power of low power is strong, and to the strand of carbon steel, comparatively macrosegregation Flaw display effectiveness comparison is good.But alloy steel strand, due to the existence of alloying element, macrostructure is fine and close, after being subject to deep-etching, overall pattern is corroded, and masks the border of ingot shape defect, often can not analyse clearly the border showing ingot shape defect, routine inspection is difficult to differentiate, and causes undetected.Sulphur print is based on the segregation effect of element sulphur in steel and sets off by contrast the existence of segregation defects.General segregation zones, sulphur segregation distribution concentrates on heart portion, and original appearance truly can not be manifested the edge in pattern segregation district, therefore pattern segregation defect cannot show by the mode of sufur printing at all.Chemical composition in-situ study method can only determine segregation position after demonstrating pattern segregation region, chemical composition analysis is done from exemplary position sampling, determine the total content of segregation composition again, when not showing pattern segregation region, can only comprehensive analysis strand composition profiles, this method is proved effective to quantitative analysis strand segregation defects, but can not the distributing position of intuitive analysis pattern segregation in steel billet, does not have direct reference significance to the diagnosis of pattern segregation defect.Owing to lacking effective corrosion means, some alloy billet pattern segregation defect usually correctly, effectively, truly cannot be tested out, on casting and rolling process line, send under defect strand, cause product scrap rate rising of dispatching from the factory.
Summary of the invention
Object of the present invention is intended to solve can not the problem of complete, clear display bearing steel billet type segregation defects by methods such as general acid etchings, a kind of cold acid etching method of available property corrosion is provided, original appearance bearing steel billet type segregation defects form be can show, thus undetected cold erosion agent and compound method thereof avoided.
For this reason, the solution that the present invention takes is:
Show a cold erosion agent for bearing steel strand pattern segregation, it is characterized in that, its component and content are:
Trinitrophenol 4 ~ 6 grams, iron trichloride 7 ~ 12 grams, 15 ~ 30 milliliters, nitric acid, hydrochloric acid 15 ~ 30 milliliters, distilled water 300 ~ 400 milliliters.
Show a cold erosion agent compounding method for bearing steel strand pattern segregation, it is characterized in that:
Trinitrophenol 4 ~ 6 grams, iron trichloride 7 ~ 12 grams of solid chemicals are placed in a Glass Containers, add distilled water 200 milliliters, solid chemicals is dissolved; Get 15 ~ 30 milliliters, nitric acid again, hydrochloric acid 15 ~ 30 milliliters joins in trinitrophenol and ferric chloride aqueous solutions successively, after stirring, the distilled water of surplus is added wherein, fully stir, complete the preparation of cold erosion agent;
During preparation, the content according to trinitrophenol in C and Si in steel, Cr, Ni alloying element content adjustment formula, iron trichloride and acid: when alloying element kind is many, content height time, increase trinitrophenol, tri-chlorination iron, be up to 2 ~ 3 times of the upper limit; Meanwhile, nitric acid, hydrochloric acid and the distillation water yield is increased matchingly; And nitric acid, hydrochloric acid add-on remain equivalent, are below limited to benchmark value, with specimen surface in corrosion process, the amount of the acid increased does not occur that excessive erosion phenomenon is as the criterion.
Beneficial effect of the present invention is:
1, the present invention can manifest the position of bearing steel billet macrostructure pattern segregation defect, distributional pattern and pattern clearly.
2, the present invention's cold erosion agent is cold acid etching reagent, not strong to the selective corrosion of steel matrix, the structure of shown steel matrix is low power solidified structure, by the selective corrosion effect display undulating composition interface continued, contrast effect is obvious, the edge clear of the macroscopic defects flowed with strand rolling in this border of pattern segregation, accurate positioning, can effectively avoid undetected.
The features such as 3, to have inspection speed fast in the present invention, pollutes little, save energy, easy and simple to handle, solving can not the difficult problem of clear, comprehensive display bearing steel billet type segregation defects by hot acid or other cold acid etching methods.
Embodiment
Embodiment nitric acid, hydrochloric acid adopt industry standard solution, i.e. nitric acid (65%), hydrochloric acid (32.3%).
Embodiment 1
For display containing C0.95wt%, Si0.15wt%, Mn0.35wt%, P0.011wt%, S0.052wt%, Cr1.4wt%, Ni0.3wt%, Cu0.25wt%, surplus is the bearing steel strand pattern segregation defect form of Fe.
Get 4 grams of trinitrophenols, 7 grams of iron trichloride solid chemicals are placed in a Glass Containers, add distilled water 200 milliliters, solid chemicals is dissolved.Add 15 milliliters of nitric acid after stirring, stir, then add 15 milliliters of hydrochloric acid, after stirring, then 100 ml distilled waters are added wherein.Abundant stirring, completes the preparation of cold erosion agent.
Steel billet cross section specimen surface is processed into the examination face that roughness is Ra≤0.16 μm.The even wiping specimen surface of cold erosion agent is dipped in absorbent cotton, corrode 5 minutes, when visual inspection finds that examination face matrix surface has shaped as frame segregation vestige to 1/4 region in heart portion, extend etching time again, emphasis corrodes this region, after the clear display in shaped as frame segregation zones, immediately to examination face upper punch hot water or cold water, dry up.
Embodiment 2
For display containing C1.03wt%, Si0.45wt%, Mn0.45wt%, P0.012wt%, S0.042wt%, Cr1.5wt%, Ni0.3wt%, Cu0.24wt%, Mo0.30wt%, surplus is the bearing steel strand pattern segregation defect form of Fe.
Get 5 grams of trinitrophenols, 10 grams of iron trichloride solid chemicals are placed in a Glass Containers, add distilled water 200 milliliters, solid chemicals is dissolved.Add 20 milliliters of nitric acid after stirring, stir, then add 20 milliliters of hydrochloric acid, again 150 ml distilled waters are added wherein after stirring.Abundant stirring, completes the preparation of cold erosion agent.
Steel billet cross section specimen surface is processed into the examination face that roughness is Ra≤0.16 μm.The even wiping specimen surface of corrosion liquid is dipped in absorbent cotton, corrode 5 ~ 6 minutes, when visual inspection finds that examination face matrix surface has shaped as frame segregation vestige to 1/4 region in heart portion, extend etching time again, emphasis corrodes this region, after the clear display in shaped as frame segregation zones, immediately to examination face upper punch hot water or cold water, dry up.
Embodiment 3
For display containing C1.05wt%, Si0.75wt%, Mn0.45wt%, P0.012wt%, S0.042wt%, Cr1.6wt%, Ni0.3wt%, Cu0.25wt%, Mo0.40wt%, surplus is the bearing steel strand pattern segregation defect form of Fe.
Get 6 grams of trinitrophenols, 8 grams of iron trichloride solid chemicals are placed in a Glass Containers, add distilled water 200 milliliters, solid chemicals is dissolved.Add 25 milliliters of nitric acid after stirring, stir, then add 25 milliliters of hydrochloric acid, again 120 ml distilled waters are added wherein after stirring.Abundant stirring, completes the preparation of cold erosion agent.
Steel billet cross section specimen surface is processed into the examination face that roughness is Ra≤0.16 μm; The even wiping specimen surface of corrosion liquid is dipped in absorbent cotton, corrode 5 ~ 6 minutes, when visual inspection finds that examination face matrix surface has shaped as frame segregation vestige to 1/4 region in heart portion, extend etching time again, emphasis corrodes this region, after the clear display in shaped as frame segregation zones, immediately to examination face upper punch hot water or cold water, dry up.
Embodiment 4
For showing the steel grade of embodiment 3: namely containing C1.05wt%, Si0.75wt%, Mn0.45wt%, P0.012wt%, S0.042wt%, Cr1.6wt%, Ni0.3wt%, Cu0.25wt%, Mo0.40wt%, surplus is the bearing steel strand pattern segregation defect form of Fe.
Get 5 grams of trinitrophenols, 11 grams of iron trichloride solid chemicals are placed in a Glass Containers, add distilled water 200 milliliters, solid chemicals is dissolved.Add 30 milliliters of nitric acid after stirring, stir, then add 30 milliliters of hydrochloric acid, again 180 ml distilled waters are added wherein after stirring.Abundant stirring, completes the preparation of cold erosion agent.
Steel billet cross section specimen surface is processed into the examination face that roughness is Ra≤0.16 μm; The even wiping specimen surface of corrosion liquid is dipped in absorbent cotton, corrode 5 ~ 6 minutes, when visual inspection finds that examination face matrix surface has shaped as frame segregation vestige to 1/4 region in heart portion, extend etching time again, emphasis corrodes this region, after the clear display in shaped as frame segregation zones, immediately to examination face upper punch hot water or cold water, dry up.
Embodiment 5
For showing the steel grade strand pattern segregation defect form of embodiment 3.
Get 6 grams of trinitrophenols, 7 grams of iron trichloride solid chemicals are placed in a Glass Containers, add distilled water 200 milliliters, solid chemicals is dissolved.Add 28 milliliters of nitric acid after stirring, stir, then add 28 milliliters of hydrochloric acid, again 180 ml distilled waters are added wherein after stirring.Abundant stirring, completes the preparation of cold erosion agent.
Steel billet cross section specimen surface is processed into the examination face that roughness is Ra≤0.16 μm; The even wiping specimen surface of corrosion liquid is dipped in absorbent cotton, corrode 5 ~ 6 minutes, when visual inspection finds that examination face matrix surface has shaped as frame segregation vestige to 1/4 region in heart portion, extend etching time again, emphasis corrodes this region, after the clear display in shaped as frame segregation zones, immediately to examination face upper punch hot water or cold water, dry up.
Embodiment 6
For showing the steel grade strand pattern segregation defect form of embodiment 3.
Get 6 grams of trinitrophenols, 12 grams of iron trichloride solid chemicals are placed in a Glass Containers, add distilled water 200 milliliters, solid chemicals is dissolved.Add 22 milliliters of nitric acid after stirring, stir, then add 22 milliliters of hydrochloric acid, again 200 ml distilled waters are added wherein after stirring.Abundant stirring, completes the preparation of cold erosion agent.
Steel billet cross section specimen surface is processed into the examination face that roughness is Ra≤0.16 μm; The even wiping specimen surface of corrosion liquid is dipped in absorbent cotton, corrode 5 ~ 6 minutes, when visual inspection finds that examination face matrix surface has shaped as frame segregation vestige to 1/4 region in heart portion, extend etching time again, emphasis corrodes this region, after the clear display in shaped as frame segregation zones, immediately to examination face upper punch hot water or cold water, dry up.
Corrosive effect: embodiment 1 ~ 6 all original appearance can manifest bearing steel strand pattern segregation macrostructure pattern clearly: the distance etc. on the position on steel billet cross section, segregation zones size, distance surface.
Claims (2)
1. show a cold erosion agent for bearing steel strand pattern segregation, it is characterized in that, its component and content are:
Trinitrophenol 4 ~ 6 grams, iron trichloride 7 ~ 12 grams, 15 ~ 30 milliliters, nitric acid, hydrochloric acid 15 ~ 30 milliliters, distilled water 300 ~ 400 milliliters.
2. show a cold erosion agent compounding method for bearing steel strand pattern segregation as claimed in claim 1, it is characterized in that:
Trinitrophenol 4 ~ 6 grams, iron trichloride 7 ~ 12 grams of solid chemicals are placed in a Glass Containers, add distilled water 200 milliliters, solid chemicals is dissolved; Get 15 ~ 30 milliliters, nitric acid again, hydrochloric acid 15 ~ 30 milliliters joins in trinitrophenol and ferric chloride aqueous solutions successively, after stirring, the distilled water of surplus is added wherein, fully stir, complete the preparation of cold erosion agent;
During preparation, the content according to trinitrophenol in C and Si in steel, Cr, Ni alloying element content adjustment formula, iron trichloride and acid: when alloying element kind is many, content height time, increase trinitrophenol, tri-chlorination iron, be up to 2 ~ 3 times of the upper limit; Meanwhile, nitric acid, hydrochloric acid and the distillation water yield is increased matchingly; And nitric acid, hydrochloric acid add-on remain equivalent, are below limited to benchmark value, with specimen surface in corrosion process, the amount of the acid increased does not occur that excessive erosion phenomenon is as the criterion.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107761100A (en) * | 2016-08-18 | 2018-03-06 | 宝山钢铁股份有限公司 | Medium high carbon high-strength steel prior austenite grain size visualizingre agent and its application method |
| CN109959671A (en) * | 2019-03-27 | 2019-07-02 | 南京钢铁股份有限公司 | A kind of method of quantitative analysis plate segregation |
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| CN101760742A (en) * | 2009-12-31 | 2010-06-30 | 西安热工研究院有限公司 | Austenitic steel deformation layer and preparation and application method of etchant displayed in matrix structure |
| CN102383131A (en) * | 2011-11-03 | 2012-03-21 | 模德模具(东莞)有限公司 | Formula for corrosive medicinal liquid used for high hardness die steel and preparation method for same |
| CN103510092A (en) * | 2012-06-20 | 2014-01-15 | 鞍钢股份有限公司 | Corrosion agent for displaying intercrystalline cracks of continuous casting steel billet and its preparation method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20040110618A (en) * | 2003-06-20 | 2004-12-31 | 주식회사 포스코 | Etching solution for exposure of austenite grain size and method for manufacture the same, method for exposure of austenite grain size using them |
| CN101760742A (en) * | 2009-12-31 | 2010-06-30 | 西安热工研究院有限公司 | Austenitic steel deformation layer and preparation and application method of etchant displayed in matrix structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107761100A (en) * | 2016-08-18 | 2018-03-06 | 宝山钢铁股份有限公司 | Medium high carbon high-strength steel prior austenite grain size visualizingre agent and its application method |
| CN109959671A (en) * | 2019-03-27 | 2019-07-02 | 南京钢铁股份有限公司 | A kind of method of quantitative analysis plate segregation |
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