CN106546468A - The aggressive agent shown for middle carbon continuous casting billet containing manganese steel solidified structure and display packing - Google Patents

The aggressive agent shown for middle carbon continuous casting billet containing manganese steel solidified structure and display packing Download PDF

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Publication number
CN106546468A
CN106546468A CN201610914102.3A CN201610914102A CN106546468A CN 106546468 A CN106546468 A CN 106546468A CN 201610914102 A CN201610914102 A CN 201610914102A CN 106546468 A CN106546468 A CN 106546468A
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China
Prior art keywords
continuous casting
manganese steel
solidified structure
casting billet
containing manganese
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CN201610914102.3A
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Inventor
吕浩
李经哲
马德刚
潘文娜
王建兴
孙洪亮
李梦英
李梦龙
路博勋
王耐
冯慧霄
李波
王健
赫书悦
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Tangshan Iron and Steel Group Co Ltd
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Tangshan Iron and Steel Group Co Ltd
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Priority to CN201610914102.3A priority Critical patent/CN106546468A/en
Publication of CN106546468A publication Critical patent/CN106546468A/en
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    • 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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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating And Analyzing Materials By Characteristic Methods (AREA)

Abstract

The invention discloses a kind of aggressive agent shown for middle carbon continuous casting billet containing manganese steel solidified structure and display packing, its method and step is:(1)Sample of the middle carbon containing manganese steel continuous casting billet is taken, and is polished;(2)By sodium metabisulfite saturated aqueous solution 40~60%, the volume proportion of picric acid saturated alcohols liquid 40~60%, sodium metabisulfite saturated aqueous solution and picric acid saturated alcohols liquid are mixed, is placed 0.5~2 hour;(3)By the inspection placed face down of sample after polishing in aggressive agent, until the solidified structure for checking face shows clearly.In this method, aggressive agent prepares simple, erosion process strong operability;Corrode without the need for hot acid, environmental pollution is little;Erosion effect preferably, after erosion sample through polishing still can pine-tree structure visible in detail, condition is provided with interdendritic composition detection to dendritic arm;After erosion, the solidified structure of sample shows clearly, has better effects under SEM and EPMA, provides advantage with interdendritic composition detection to dendritic arm.

Description

The aggressive agent shown for middle carbon continuous casting billet containing manganese steel solidified structure and display packing
Technical field
Metal structure detection technique field of the present invention, especially one kind are shown for middle carbon continuous casting billet containing manganese steel solidified structure Aggressive agent and display packing.
Background technology
Solidified structure is divided into macrostructure and microscopic structure, and both forms of expression are different, but its forming process phase closely Close, and the properties to strand, particularly mechanical performance produce strong impact.Either static ingot or continuous casting billet, The solidified structure of the two is without essential distinction, but due to the continuous production processes characteristic of continuous casting, the solidified structure of continuous casting billet is present The characteristics of chill is thin, column crystal is flourishing, Center Equiaxial Crystal is few.
Dual phase steel belongs to middle carbon containing the one kind in manganese steel, and which has low yield tensile ratio, high initial manufacture hardening rate, strong Degree and ductility it is good fit the features such as, be widely used in the key positions such as automobile buffer beam, rotary shaft, B posts, in recent years, with The fast development of auto industry, the demand of dual phase steel is also sharply increased therewith.Domestic each big steel enterprise increases double one after another The R&D intensity of phase steel, different enterprise's dual phase steel composition designs are variant, but using high [Mn] component system.And for The higher steel grade of [Mn] content, easily causes continuous casting slab segregation defect, lower procedure thoroughly cannot eliminate, and is genetic to hot rolling material and cold Banded structure is formed on stocking.Banded structure is a kind of defect(ive) structure, can have a strong impact on steel performance, reduces plasticity, the punching of steel Toughness, fracture toughness and the contraction percentage of area are hit, Cold Bending Inconfornmy lattice, punching press percent defective height etc. is caused.Currently for dual phase steel banding The problem of tissue, hot-rolled process thoroughly cannot be eliminated by controlled rolling and controlled cooling, only by the analysis to continuous casting billet solidified structure, really The reason for determining segregation, targetedly to take measures.At present, conventional erosion means can not still meet dendrite morphology and clearly show The requirement shown, it is impossible to dendrite interval and microscopic segregation degree that accurately measurement continuous casting billet is organized, for solution segregation and by segregated zone The problem come, it is impossible to accomplish proposition solution with a definite target in view.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of display and be clearly used for middle carbon continuous casting billet containing manganese steel solidification group Knit the aggressive agent of display;The display packing that middle carbon continuous casting billet containing manganese steel solidified structure shows.
To solve above-mentioned technical problem, the component volume proportioning taken by the present invention is:Sodium metabisulfite saturation is water-soluble Liquid 40~60%, picric acid saturated alcohols liquid 60~40%.
Alcohol of the present invention is ethanol and/or methanol.
Sodium metabisulfite saturated aqueous solution of the present invention and picric acid saturated alcohols liquid are placed 0.5~2 hour after mixing.
The inventive method is:(1)Sampling:Sample of the middle carbon containing manganese steel continuous casting billet is taken, and is polished;
(2)Prepare etchant:By sodium metabisulfite saturated aqueous solution 40~60%, the volume of picric acid saturated alcohols liquid 60~40% Proportioning, sodium metabisulfite saturated aqueous solution and picric acid saturated alcohols liquid is mixed, is placed 0.5~2 hour;
(3)Corrode:By the inspection placed face down of sample after polishing in aggressive agent, until the solidified structure for checking face shows clearly It is clear.
Step described in the inventive method(1)In, it is polished to roughness Ra≤0.1 μm in inspection face.
Step described in the inventive method(3)In, erosion time is 2~5 minutes.
In described in the inventive method, weight/mass percentage composition of the carbon containing primary alloy constituent in manganese steel is:C 0.08%~ 0.25%th, Mn 1.0%~2.0%, S 0~0.020%, P 0~0.020%, Si 0~1.20%, alloy total amount≤5%.
Using the beneficial effect produced by above-mentioned technical proposal it is:Aggressive agent of the present invention prepares simple, erosion process behaviour The property made is strong;Corrode without the need for hot acid, environmental pollution is little;Erosion effect preferably, after erosion, still clearly can see through polishing by sample Pine-tree structure is observed, condition is provided with interdendritic composition detection to dendritic arm.
The inventive method adopts picric acid and adds sodium metabisulfite corrodes for dendrite of the middle carbon containing manganese steel, through invading After erosion, the solidified structure of sample shows clearly, has better effects, to dendritic arm with interdendritic into go-on-go under SEM and EPMA Survey there is provided advantage.
Description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is the sample position structural representation of the present invention;
Fig. 2 is the collected by camera photo in inspection face of the present invention;
Fig. 3 is inspection face optical microscope collection picture of the present invention(50×)Collection photo.
In figure:1- continuous casting billets;2- samples.
Specific embodiment
In this, the characterization processes of the display packing and sample of carbon continuous casting billet containing manganese steel solidified structure adopt following technique Step:(1)Sample position:As shown in figure 1, a quarter, the center of thickness direction of the sample position for 1 width of continuous casting billet Place, the direction of arrow in Fig. 1 are cast direction;With the results contrast of cold acid attack low power, it is contemplated that segregated zone centered on the region With isometry crystalline region.Take the sample 2 of 20mm × 20mm × 25mm;The inspection face of sample 2 is the shade in 20mm × 20mm, i.e. Fig. 1 Part.
(2)Prepare aggressive agent:By sodium metabisulfite(Na2S2O5)Pressed powder and distilled water are made into saturated solution, bitterness Acid(C6H2OH(NO2)3)Solid particle and alcohol are configured to saturated solution;Described alcohol is methanol and/or ethanol;Under room temperature, take partially Sodium bisulfite saturated aqueous solution, the supernatant of picric acid saturated alcohols liquid are as the standard solution for configuring aggressive agent, sub- by laying particular stress on The volume ratio mixing of sulphuric acid saturated aqueous solution of sodium 40~60%, picric acid saturated alcohols liquid 60~40%, shakes up, places at room temperature 0.5~2 hour;Above-mentioned placement process can make Na2S2O5Partial oxidation is into Na2S2O6, erosion effect can be significantly improved.
(3)Sample preparation and erosion:A. according to GB/T 226-91《The macrostructure and defect acid etching method of inspection of steel》Standard is produced Fritter coarse micro-grain sample;Then it is polished, makes roughness Ra≤0.1 μm in inspection face;Finally with alcohol washes, dry up it is stand-by.
B. the hand-held above-mentioned sample for making, is checked placed face down in aggressive agent, inspection face is fully connect with aggressive agent Touch, depth of invasion is 2~5mm;During jiggle sample so that reaction product depart from test check face, can at any time from Observation is taken out in aggressive agent, erosion time checks the solidified structure in face to show clearly after 2~5 minutes;Take out, rushed with dehydrated alcohol Wash, wipe inspection face, finally dried up with hair-dryer.
C. corrode after inspection face on may attachment reaction generate spot, cannot be wiped out with cotton ball soaked in alcohol, now Needs are shallow on buffing machine to be polished, to remove the spot.For the inspection face of attachment spot, dendrite interval can be measured, But which can not be used for detecting micro-area composition, because the result of element meeting Interference Detection micro-area composition contained by attachment.
(4)Measurement:According to the erosion results and experiment purpose in test check face, can be right under 20 times of visual fields of optical microscope The primary dendritic spacing of sample, secondary dendrite arm spacing are measured;The preferable sample of erosion results can be directly used for micro-area composition Detection.
Embodiment 1:In this, the display packing of carbon continuous casting billet containing manganese steel solidified structure adopts following processing steps.
In described in the present embodiment, mass component of the carbon containing manganese steel is:C 0.17%、Mn 1.79%、S 0.002%、P 0.016%th, Si 0.36%, Als 0.038%, Cr 0.51%, Nb 0.034%, Ti 0.046%, N 0.0038%, balance of Fe and Inevitable impurity.
Process conditions:Sodium metabisulfite saturated aqueous solution and picric acid saturated alcohols liquid volume proportion are respectively 50%, in room Temperature is lower to place 2 hours;Erosion time checks the solidified structure in face to show clearly after 4 minutes;Remaining technique is as described above.
Measurement result:Collected by camera photo under 10 times of visual fields is shown in Fig. 2;Optical microscope collection figure when micro-area composition is detected Piece(50×)See Fig. 3;By shown in Fig. 2, Fig. 3, the solidified structure of erosion shows clearly, under optical microscope and ultramicroscope Accurately can be measured.
Embodiment 2:In this, the display packing of carbon continuous casting billet containing manganese steel solidified structure adopts following processing steps.
In described in the present embodiment, mass component of the carbon containing manganese steel is:C 0.16%、Mn 1.81%、S 0.001%、P 0.017%th, Si 0.37%, Als 0.042%, Cr 0.50%, Nb 0.036%, Ti 0.049%, N 0.0029%, balance of Fe and Inevitable impurity.
Process conditions:By sodium metabisulfite saturated aqueous solution 40%, the volume proportion of picric acid saturated alcohols liquid 60%, in room Temperature is lower to place 1 hour;Erosion time checks the solidified structure in face to show clearly after 2 minutes;Remaining technique is as described above.
Measurement result:The solidified structure of erosion shows clearly, and standard can be carried out under optical microscope and ultramicroscope True measurement.
Embodiment 3:In this, the display packing of carbon continuous casting billet containing manganese steel solidified structure adopts following processing steps.
In described in the present embodiment, mass component of the carbon containing manganese steel is:C 0.09%、Mn 1.99%、S 0.001%、P 0.015%th, Si 1.16%, Als 0.043%, Cr 0.033%, Ti 0.014%, N 0.0038%, balance of Fe and inevitably Impurity.
Process conditions:By sodium metabisulfite saturated aqueous solution 60%, the volume proportion of picric acid saturated alcohols liquid 40%, in room Temperature decentralization sets to 0 .5 hours;Erosion time checks the solidified structure in face to show clearly after 5 minutes;Remaining technique is as described above.
Measurement result:The solidified structure of erosion shows clearly, and standard can be carried out under optical microscope and ultramicroscope True measurement.

Claims (7)

1. a kind of aggressive agent shown for middle carbon continuous casting billet containing manganese steel solidified structure, it is characterised in that its component volume proportioning For:Sodium metabisulfite saturated aqueous solution 40~60%, picric acid saturated alcohols liquid 60~40%.
2. the aggressive agent shown for middle carbon continuous casting billet containing manganese steel solidified structure according to claim 1, it is characterised in that: The alcohol is ethanol and/or methanol.
3. the aggressive agent shown for middle carbon continuous casting billet containing manganese steel solidified structure according to claim 1 and 2, its feature exist In:The sodium metabisulfite saturated aqueous solution and picric acid saturated alcohols liquid are placed 0.5~2 hour after mixing.
4. a kind of display packing of middle carbon continuous casting billet containing manganese steel solidified structure, it is characterised in that:(1)Sampling:Middle carbon is taken containing manganese steel The sample of continuous casting billet, and be polished;
(2)Prepare etchant:By sodium metabisulfite saturated aqueous solution 40~60%, the volume of picric acid saturated alcohols liquid 60~40% Proportioning, sodium metabisulfite saturated aqueous solution and picric acid saturated alcohols liquid is mixed, is placed 0.5~2 hour;
(3)Corrode:By the inspection placed face down of sample after polishing in aggressive agent, until the solidified structure for checking face shows clearly It is clear.
5. the display packing for middle carbon continuous casting billet containing manganese steel solidified structure according to claim 4, it is characterised in that:Institute State step(1)In, it is polished to roughness Ra≤0.1 μm in inspection face.
6. the display packing for middle carbon continuous casting billet containing manganese steel solidified structure according to claim 4, it is characterised in that:Institute State step(3)In, erosion time is 2~5 minutes.
7. the display packing for middle carbon continuous casting billet containing manganese steel solidified structure according to claim 4,5 or 6, its feature exist In weight/mass percentage composition of the middle carbon containing primary alloy constituent in manganese steel is:C 0.08%~0.25%, Mn 1.0%~2.0%, S 0~0.020%, P 0~0.020%, Si 0~1.20%, alloy total amount≤5%.
CN201610914102.3A 2016-10-20 2016-10-20 The aggressive agent shown for middle carbon continuous casting billet containing manganese steel solidified structure and display packing Pending CN106546468A (en)

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Citations (4)

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Publication number Priority date Publication date Assignee Title
CN101382494A (en) * 2008-08-26 2009-03-11 武汉钢铁(集团)公司 Method for displaying and quantitatively determining retained austenite or island martensite- austenite in TRIP steel
CN102011119A (en) * 2010-09-17 2011-04-13 马鞍山钢铁股份有限公司 Dual-phase steel color metallographic coloring agent and color display method thereof
CN102175191A (en) * 2011-02-25 2011-09-07 首钢总公司 Quantitative method for area percent of martensite-austenite (MA) island structure
CN105445309A (en) * 2014-08-28 2016-03-30 宝山钢铁股份有限公司 Method for quantitatively analyzing content of martensite in dual phase steel

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101382494A (en) * 2008-08-26 2009-03-11 武汉钢铁(集团)公司 Method for displaying and quantitatively determining retained austenite or island martensite- austenite in TRIP steel
CN102011119A (en) * 2010-09-17 2011-04-13 马鞍山钢铁股份有限公司 Dual-phase steel color metallographic coloring agent and color display method thereof
CN102175191A (en) * 2011-02-25 2011-09-07 首钢总公司 Quantitative method for area percent of martensite-austenite (MA) island structure
CN105445309A (en) * 2014-08-28 2016-03-30 宝山钢铁股份有限公司 Method for quantitatively analyzing content of martensite in dual phase steel

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