CN105316685B - Cold etching agent for displaying ingot type segregation of bearing steel casting blank and preparation method thereof - Google Patents
Cold etching agent for displaying ingot type segregation of bearing steel casting blank and preparation method thereof Download PDFInfo
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- CN105316685B CN105316685B CN201410335598.XA CN201410335598A CN105316685B CN 105316685 B CN105316685 B CN 105316685B CN 201410335598 A CN201410335598 A CN 201410335598A CN 105316685 B CN105316685 B CN 105316685B
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- trinitrophenol
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- 238000005204 segregation Methods 0.000 title claims abstract description 53
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 38
- 239000010959 steel Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000005530 etching Methods 0.000 title abstract description 14
- 238000005266 casting Methods 0.000 title abstract 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000012153 distilled water Substances 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 18
- 239000007787 solid Substances 0.000 claims abstract description 18
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 17
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229950002929 trinitrophenol Drugs 0.000 claims abstract description 13
- 239000011521 glass Substances 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract 3
- 230000003628 erosive effect Effects 0.000 claims description 20
- 239000000126 substance Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 16
- 230000007797 corrosion Effects 0.000 claims description 11
- 238000005260 corrosion Methods 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 238000005275 alloying Methods 0.000 claims description 5
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 238000005660 chlorination reaction Methods 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 26
- 230000000694 effects Effects 0.000 abstract description 6
- 238000005096 rolling process Methods 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 abstract 2
- 239000003814 drug Substances 0.000 abstract 2
- 238000004134 energy conservation Methods 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 description 8
- 229920000742 Cotton Polymers 0.000 description 6
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 6
- 238000007689 inspection Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000005864 Sulphur Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 229910052748 manganese Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 238000009749 continuous casting Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 230000002068 genetic effect Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- ing And Chemical Polishing (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
A cold etching agent for displaying the ingot type segregation of bearing steel casting blanks comprises the following components in percentage by weight: 4-6 g of trinitrophenol, 7-12 g of ferric trichloride, 15-30 ml of nitric acid, 15-30 ml of hydrochloric acid and 300-400 ml of distilled water. Putting a quantitative trinitrophenol and ferric trichloride solid medicament into a glass container, adding 200 ml of distilled water, and dissolving the solid medicament; then adding nitric acid and hydrochloric acid into the aqueous solution of trinitrophenol and ferric trichloride, stirring uniformly, adding the rest of distilled water into the aqueous solution, and fully stirring to finish the preparation of the cold etching agent. The invention has the advantages of high detection speed, little pollution, energy conservation and simple and convenient operation, can clearly show the position, distribution form and appearance of the macrostructure ingot type segregation defect of the bearing billet, has obvious contrast effect, ensures that the edge of the macroscopic defect of the ingot type segregation, the boundary of which flows along with the rolling of the casting blank, is clear, has accurate positioning and can effectively avoid missing detection.
Description
Technical field
It is more particularly to a kind of to be used to show bearing steel strand macrostructure the invention belongs to metallurgical material analytical control field
The cold erosion agent of middle pattern segregation defect and its compound method.
Background technology
Pattern segregation defect is the defects of strand is relatively conventional in continuous casting square billet macrostructure, when being segregated serious, is rolled into
After pole, wire rod, the center for being present in stocking is remained able to, influences interiors of products quality and performance.To hot-rolled rods
Material, the presence of pattern segregation, the tissue at cross section edge and center is caused notable difference occur, some other defects are in line of segragation
Aggregation, technology controlling and process is influenceed in the follow-up operation of rolling, form waste product.Produced for wire product, the pattern segregation meeting of strand
It is genetic on final become a useful person, forms central tissue's segregation of wire rod even steel wire, wire rod tissue occur abnormal.In bearing etc. zero
There is serious cracking phenomena when processing in part, and deteriorates the mechanical property and deep shaping property of product.
The key of bearing steel continuous casting square billet pattern segregation defect is eliminated, first will be in steel billet inspection with effective
The abundant truly reproducing steel billet pattern segregation order of severity of caustic solution, timely handshake result, controls smelting process, really
Guarantor's segregation defects do not bring rolling process below into.Generally use low power hot acid erosion at present, sulphur print examine the ingot shape of steel billet inclined
The macro defects such as analysis.The constituent content mensure method of chemical analysis is also often often used as supplement laboratory facilities.Low power hot acid loses
Method corrosive power is strong, relatively good to the more serious segregation defects display effect of strand of carbon steel.But for steel alloy strand, due to
The presence of alloying element, macrostructure is fine and close, and after deep-etching, overall pattern is corroded, and masks the side of ingot shape defect
Boundary, the border that clear analysis shows ingot shape defect is tended not to, routine inspection is difficult to differentiate, and causes missing inspection.Sulphur print is based on
The presence of the segregation effect contrast segregation defects of element sulphur in steel.General segregation zones, sulphur segregation distribution concentrates on center portion, to ingot
The edge of type line of segragation can not truly show original appearance, therefore pattern segregation defect can not be shown with the mode of sufur printing at all
Come.Chemical composition in-situ study method can only be determined to be segregated position after pattern segregation region is shown, done from exemplary position sampling
Chemical composition analysis, then determine to be segregated the total content of composition, can only be comprehensive point in the case where not showing pattern segregation region
Strand component distributing is analysed, this method is proved effective to quantitative analysis strand segregation defects, but can not intuitively analyze pattern segregation in steel
Distributing position in base, the diagnosis to pattern segregation defect do not have direct reference significance.Due to lacking effective corrosion
Means, make some alloy billet pattern segregation defects usually can not correctly, effectively, truly test out, in continuous casting and rolling technology
On skill line, sent under defect strand, cause product percent defective rise of dispatching from the factory.
The content of the invention
The purpose of the present invention is aimed to solve the problem that with can not completely, clearly show bearing steel base pattern segregation the methods of general acid etching
The problem of defect, there is provided a kind of cold acid etching method of available property corrosion, can original appearance show that bearing steel base pattern segregation lacks
Form is fallen into, so as to avoid the cold erosion agent of missing inspection and its compound method.
Therefore, the solution that the present invention is taken is：
A kind of cold erosion agent for showing bearing steel strand pattern segregation, it is characterised in that its component and content are：
4~6 grams of trinitrophenol, 7~12 grams of ferric trichloride, 15~30 milliliters of nitric acid, 15~30 milliliters of hydrochloric acid, distilled water
300~400 milliliters.
A kind of cold erosion agent compounding method for showing bearing steel strand pattern segregation, it is characterised in that：
7~12 grams of 4~6 grams of trinitrophenol, ferric trichloride solid chemicals are placed in a glass container, add distilled water
200 milliliters, solid chemicals are dissolved；15~30 milliliters of nitric acid, 15~30 milliliters of hydrochloric acid is taken to be added sequentially to trinitrophenol again
With in ferric chloride aqueous solutionses, being added thereto, being sufficiently stirred by the distilled water of surplus after stirring, matching somebody with somebody for cold erosion agent is completed
System；
During preparation, according to C in steel and Si, Cr, Ni alloying element content adjustment formula in trinitrophenol, ferric trichloride and
The content of acid：When alloying element species is more, content is high, increase trinitrophenol, tri-chlorination iron, the 2~3 of the upper limit is up to
Times；Meanwhile matchingly increase nitric acid, hydrochloric acid and amount of distilled water；And nitric acid, hydrochloric acid addition remain equivalent, are limited to below
A reference value, increased sour amount specimen surface in corrosion process occur without excessive erosion phenomenon and be defined.
Beneficial effects of the present invention are：
1st, the present invention can clearly show position, distributional pattern and the shape of bearing steel billet macrostructure pattern segregation defect
Looks.
2nd, the cold erosion agent of the present invention is cold acid etching reagent, not strong, the shown steel matrix of the selective corrosion to steel matrix
Structure be low power solidified structure, show undulating composition interface by lasting selective corrosion effect, contrast effect is obvious, makes
The edge clear for the gross imperfection that this border of pattern segregation rolls and flowed with strand, accurate positioning, can effectively avoid missing inspection.
3rd, the present invention, which has, examines speed fast, and pollution is small, saves the energy, it is easy to operate the features such as, solve with hot acid or
Other cold acid etching methods can not show the problem of bearing steel billet type segregation defects clearly, comprehensively.
Embodiment
Embodiment nitric acid, hydrochloric acid use industry standard solution, i.e. nitric acid（65%）, hydrochloric acid（32.3%）.
Embodiment 1
For showing wt%, P 0.011 wt%, S 0.052 wt% containing C 0.95 wt%, Si 0.15wt%, Mn 0.35,
Cr 1.4 wt%, Ni 0.3 wt%, Cu 0.25 wt%, surplus are Fe bearing steel strand pattern segregation defect form.
Take 4 grams of trinitrophenols, 7 grams of ferric trichloride solid chemicals to be placed in a glass container, add the milli of distilled water 200
Rise, solid chemicals are dissolved.It is stirring evenly and then adding into 15 milliliters of nitric acid, stirs, adds 15 milliliters of hydrochloric acid, stir
Afterwards, then by 100 milliliters of distilled water it is added thereto.It is sufficiently stirred, 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.It is equal that cold erosion agent is dipped in absorbent cotton
Even wiping specimen surface, corrode 5 minutes, wait that visually observing discovery examination face matrix surface to 1/4 region of center portion is presented framed shape
When being segregated vestige, then extend etching time, emphasis corrodes the region, behind frame v shaped segregation region clearly display, immediately to examination face
On rush hot water or cold water, dry up.
Embodiment 2
For showing the wt% containing C 1.03 wt%, Si 0.4 5wt%, Mn 0.45 wt%, P 0.012wt%, S 0.042,
The wt% of Cr 1.5 wt%, Ni 0.3 wt%, Cu 0.24 wt%, Mo 0.30, surplus are that Fe bearing steel strand pattern segregation lacks
Fall into form.
Take 5 grams of trinitrophenols, 10 grams of ferric trichloride solid chemicals to be placed in a glass container, add the milli of distilled water 200
Rise, solid chemicals are dissolved.It is stirring evenly and then adding into 20 milliliters of nitric acid, stirs, adds 20 milliliters of hydrochloric acid, stir
150 milliliters of distilled water are added thereto again afterwards.It is sufficiently stirred, 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.Corrosion decoction is dipped in absorbent cotton
Specimen surface is uniformly wiped, is corroded 5~6 minutes, waits that visually observing discovery examination face matrix surface to 1/4 region of center portion presents
During frame v shaped segregation vestige, then extend etching time, emphasis corrodes the region, after frame v shaped segregation region clearly display after, immediately to
Hot water or cold water is rushed on examination face, is dried up.
Embodiment 3
For showing wt%, Cr containing C 1.05 wt%, Si 0.75wt%, Mn 0.45 wt%, P 0.012wt%, S 0.042
The wt% of 1.6 wt%, Ni 0.3 wt%, Cu0.25 wt%, Mo 0.40, surplus are Fe bearing steel strand pattern segregation defect shape
State.
Take 6 grams of trinitrophenols, 8 grams of ferric trichloride solid chemicals to be placed in a glass container, add the milli of distilled water 200
Rise, solid chemicals are dissolved.It is stirring evenly and then adding into 25 milliliters of nitric acid, stirs, adds 25 milliliters of hydrochloric acid, stir
120 milliliters of distilled water are added thereto again afterwards.It is sufficiently stirred, 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；Corrosion decoction is dipped in absorbent cotton
Specimen surface is uniformly wiped, is corroded 5~6 minutes, waits that visually observing discovery examination face matrix surface to 1/4 region of center portion presents
During frame v shaped segregation vestige, then extend etching time, emphasis corrodes the region, after frame v shaped segregation region clearly display after, immediately to
Hot water or cold water is rushed on examination face, is dried up.
Embodiment 4
For showing the steel grade of embodiment 3：That is wt%, P containing C 1.05 wt%, Si 0.7 5wt%, Mn 0.45
The wt% of 0.012wt%, S 0.042 wt%, Cr 1.6 wt%, Ni 0.3 wt%, Cu0.25 wt%, Mo 0.40, surplus are Fe's
Bearing steel strand pattern segregation defect form.
Take 5 grams of trinitrophenols, 11 grams of ferric trichloride solid chemicals to be placed in a glass container, add the milli of distilled water 200
Rise, solid chemicals are dissolved.It is stirring evenly and then adding into 30 milliliters of nitric acid, stirs, adds 30 milliliters of hydrochloric acid, stir
180 milliliters of distilled water are added thereto again afterwards.It is sufficiently stirred, 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；Corrosion decoction is dipped in absorbent cotton
Specimen surface is uniformly wiped, is corroded 5~6 minutes, waits that visually observing discovery examination face matrix surface to 1/4 region of center portion presents
During frame v shaped segregation vestige, then extend etching time, emphasis corrodes the region, after frame v shaped segregation region clearly display after, immediately to
Hot water or cold water is rushed on examination face, is dried up.
Embodiment 5
For showing the steel grade strand pattern segregation defect form of embodiment 3.
Take 6 grams of trinitrophenols, 7 grams of ferric trichloride solid chemicals to be placed in a glass container, add the milli of distilled water 200
Rise, solid chemicals are dissolved.It is stirring evenly and then adding into 28 milliliters of nitric acid, stirs, adds 28 milliliters of hydrochloric acid, stir
180 milliliters of distilled water are added thereto again afterwards.It is sufficiently stirred, 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；Corrosion decoction is dipped in absorbent cotton
Specimen surface is uniformly wiped, is corroded 5~6 minutes, waits that visually observing discovery examination face matrix surface to 1/4 region of center portion presents
During frame v shaped segregation vestige, then extend etching time, emphasis corrodes the region, after frame v shaped segregation region clearly display after, immediately to
Hot water or cold water is rushed on examination face, is dried up.
Embodiment 6
For showing the steel grade strand pattern segregation defect form of embodiment 3.
Take 6 grams of trinitrophenols, 12 grams of ferric trichloride solid chemicals to be placed in a glass container, add the milli of distilled water 200
Rise, solid chemicals are dissolved.It is stirring evenly and then adding into 22 milliliters of nitric acid, stirs, adds 22 milliliters of hydrochloric acid, stir
200 milliliters of distilled water are added thereto again afterwards.It is sufficiently stirred, 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；Corrosion decoction is dipped in absorbent cotton
Specimen surface is uniformly wiped, is corroded 5~6 minutes, waits that visually observing discovery examination face matrix surface to 1/4 region of center portion presents
During frame v shaped segregation vestige, then extend etching time, emphasis corrodes the region, after frame v shaped segregation region clearly display after, immediately to
Hot water or cold water is rushed on examination face, is dried up.
Corrosive effect：Embodiment 1~6 clearly original appearance can show bearing steel strand pattern segregation macrostructure pattern：
Position, segregation zones size on steel billet cross section, distance away from surface etc..
Claims (2)
1. a kind of cold erosion agent for showing bearing steel strand pattern segregation, it is characterised in that its component and content are：
4~6 grams of trinitrophenol, 7~12 grams of ferric trichloride, 15~30 milliliters of nitric acid, 15~30 milliliters of hydrochloric acid, distilled water 300
~400 milliliters.
A kind of 2. cold erosion agent compounding method of the bearing steel strand pattern segregation of display as claimed in claim 1, it is characterised in that：
7~12 grams of 4~6 grams of trinitrophenol, ferric trichloride solid chemicals are placed in a glass container, add distilled water 200
Milliliter, solid chemicals are dissolved；15~30 milliliters of nitric acid, 15~30 milliliters of hydrochloric acid is taken to be added sequentially to trinitrophenol and three again
In ferric chloride in aqueous solution, the distilled water of surplus is added thereto after stirring, is sufficiently stirred, complete the preparation of cold erosion agent；
During preparation, trinitrophenol in formula, ferric trichloride and acid are adjusted according to C in steel and Si, Cr, Ni alloying element content
Content：When alloying element species is more, content is high, increase trinitrophenol, tri-chlorination iron, be up to 2~3 times of the upper limit；
Meanwhile matchingly increase nitric acid, hydrochloric acid and amount of distilled water；And nitric acid, hydrochloric acid addition remain equivalent, are limited to benchmark below
Value, increased sour amount specimen surface in corrosion process occur without excessive erosion phenomenon and be defined.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410335598.XA CN105316685B (en) | 2014-07-16 | 2014-07-16 | Cold etching agent for displaying ingot type segregation of bearing steel casting blank and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410335598.XA CN105316685B (en) | 2014-07-16 | 2014-07-16 | Cold etching agent for displaying ingot type segregation of bearing steel casting blank and preparation method thereof |
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| CN105316685B true CN105316685B (en) | 2018-02-27 |
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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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 | Corrosive agent for displaying intergranular cracks of continuous casting billet and preparation method thereof |
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| KR100516523B1 (en) * | 2003-06-20 | 2005-09-27 | 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 |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 | Corrosive agent for displaying intergranular cracks of continuous casting billet and preparation method thereof |
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