CN101776624A - Method for testing grain size before blooming of square billets - Google Patents
Method for testing grain size before blooming of square billets Download PDFInfo
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- CN101776624A CN101776624A CN200910243171A CN200910243171A CN101776624A CN 101776624 A CN101776624 A CN 101776624A CN 200910243171 A CN200910243171 A CN 200910243171A CN 200910243171 A CN200910243171 A CN 200910243171A CN 101776624 A CN101776624 A CN 101776624A
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- billet
- square billet
- grain size
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- breaking down
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- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000012360 testing method Methods 0.000 title abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 230000003647 oxidation Effects 0.000 claims abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 10
- 238000004458 analytical method Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 5
- 239000001301 oxygen Substances 0.000 claims abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 34
- 229910052742 iron Inorganic materials 0.000 claims description 17
- 229910000831 Steel Inorganic materials 0.000 claims description 11
- 239000010959 steel Substances 0.000 claims description 11
- 239000011159 matrix material Substances 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 4
- 230000008520 organization Effects 0.000 claims description 4
- 238000010998 test method Methods 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 230000004913 activation Effects 0.000 claims description 2
- 238000012956 testing procedure Methods 0.000 claims description 2
- 238000005096 rolling process Methods 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract 2
- 239000000758 substrate Substances 0.000 abstract 1
- 229910001566 austenite Inorganic materials 0.000 description 23
- 238000011160 research Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000004088 simulation Methods 0.000 description 3
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 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 description 2
- 238000010791 quenching Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005088 metallography Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
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- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
一种测试方坯初轧前晶粒大小的方法，属于材料金相测试技术领域。测试步骤：加热炉温度控制在980-1150℃，残氧量2.5-6％，加热时间2.5-4小时，钢坯出炉后经过高压水除磷，获得方坯表面氧化铁皮；将氧化铁皮经过超声波清洗8-10分钟，制备成扫描电镜分析试样；在扫描电镜下分析氧化铁皮贴近方坯基体一侧的形貌，获得方坯晶界氧化的组织照片；通过晶界氧化组织照片利用Imagetool软件测试方坯初轧前晶粒大小。本发明优点在于，准确获得方坯初轧前晶粒大小，分析方法简单，数据准确。
The invention discloses a method for testing the grain size of a billet before blooming, which belongs to the technical field of material metallographic testing. Test steps: the heating furnace temperature is controlled at 980-1150°C, the residual oxygen content is 2.5-6%, and the heating time is 2.5-4 hours. After the billet is released from the furnace, it is dephosphorized by high-pressure water to obtain the oxide scale on the surface of the billet; the oxide scale is cleaned by ultrasonic waves 8-10 minutes, prepare a scanning electron microscope analysis sample; analyze the morphology of the iron oxide scale close to the billet substrate under the scanning electron microscope, and obtain the structure photo of the grain boundary oxidation of the billet; use Imagetool software to test the grain boundary oxidation structure photo The grain size of billet before blooming. The invention has the advantages of accurately obtaining the grain size of the billet before preliminary rolling, simple analysis method and accurate data.
Description
Technical field
The invention belongs to technical filed of material metallographic test, a kind of method of testing the preceding grain size of square billet breaking down particularly is provided, austenite grain size before the breaking down of research square billet, formulation for the heating cycle of heating furnace, and formulate rational controlled rolling technology the data support is provided, detection method is easy, accurately.
Background technology
Controlled rolling is the emphasis of steel rolling process research always, reasonably the controlled rolling technological requirement to breaking down before austenite structure state, every time deflection, final material structure performance have in depth and understand, by obtain before the breaking down material composition, crystallite dimension and the boundary condition of desirable material structure performance two aspects, formulate steel rolling process parameters such as reasonable passage distortion distribution, process for cooling, so the research of the austenite structure state before the steel billet breaking down has very important meaning.
All the time, the method of the test of austenite grain size all is thermal simulation, quench after adopting austenitizing, picric acid heat etching method shows austenite grain boundary, thermal simulation is also adopted in the formulation of the rolling mill practice of square billet, after the austenite heating, size by test quenching back austenite grain size, formulate controlled rolling technology, this side's drawback has two aspects: one side detection method complexity, and narrow ranges of process parameters needs the suitable picric acid concentration of configuration, the heat time of invading is difficult to grasp the also bad assurance of the sharpness of crystal grain; On the other hand, obtain because austenite structure is thermal simulation after all, can't accurate get obtain square billet and go out heating furnace after, the structural state before the breaking down, the accuracy of data is worth discussion.This method provided by the invention, be equivalent to the original position analysis, structural state by the iron scale grain boundary oxidation of contact steel billet matrix after the de-scaling of test square billet, show the preceding austenitic grain size of breaking down exactly, principle is in the burning process, the austenite grain boundary position is at first oxidized, steel billet is no exception, water under high pressure utilization before the breaking down is cooled off fast on the one hand iron scale is cooled off fast, realize separating of iron sheet and steel billet simultaneously, preserve the replica of the preceding steel billet austenite crystal oxidation of breaking down, directly obtained the preceding austenite grain size data of square billet breaking down.
The invention provides a kind of method of studying the preceding austenite grain size of square billet breaking down, its detection method is simple, effective, has reflected the preceding austenite crystal state of square billet breaking down accurately, has enriched austenite structure research simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of method of testing the preceding grain size of square billet breaking down, detect the preceding austenite grain size of square billet breaking down, simplified conventional heat etching method, solved and to have obtained preceding this difficult problem of austenite grain size data of square billet breaking down.
Testing procedure of the present invention is:
A. furnace temp is controlled at 980-1150 ℃, remaining oxygen 2.5-6%, 2.5-4 hour heat time heating time;
B. through high-pressure water descaling, water pressure 13-16Mpa obtained the square billet scale on surface after steel billet was come out of the stove;
C. iron scale is carried out ultrasonic cleaning 8-10 minute, be prepared into the scanning electron microscope analysis sample;
D. analyze iron scale and press close to the pattern of square billet matrix one side under scanning electron microscope, the Electronic Speculum Control of Voltage obtains square billet iron scale organization picture of grain boundary at 13-15Kv;
E. organize photo to utilize grain size before the breaking down of Imagetool software test square billet by grain boundary oxidation.
Imagetool software of the present invention is a kind of under familiar various typical organizations prerequisite, and can carry out image and the data processing software that basal ration characterizes to tissue.Major function is quantitatively artificial, promptly use quantitative metallography/stereology principle, it is quantitative with software to adopt numeral to take pictures, increase work efficiency, embody digitized characteristics, can determine outside crystallite dimension, phase number percent, the nucleation rate, also can determine crooked crystal boundary length easily, grain shape compares etc. and manually quantitatively to be difficult to the work finished.
Use the basic step of software statistics crystallite dimension:
1, activates this software.Open a graphic file.
2, if will survey crystallite dimension, calibrate Calibrate earlier.In settings menu, click Calibratespacial measurement; The straight line of standardized known length, and input length value are just finished calibration.
3, click the Distance wicket, measure, line of every picture, length value enters the Results window automatically, and provides mean value and variance.
4, be under the state of activation at the Results window, can preserve measurement data
The invention has the advantages that, provide a kind of more quick, directly perceived, clear, accurately test the method for austenite grain size before the square billet breaking down.After being used to analyze square billet and going out heating furnace, austenite crystal state before the breaking down for research square billet heating cycle, the control of breaking down austenite structure provide more direct, method and data easily, is convenient to the analysis and the research of the The whole control operation of rolling.
Description of drawings
Fig. 1 is that the replica scanning electron microscope of the inboard austenite grain boundary oxidation of iron scale before the 130 square billet ultra-low-carbon steel SWRCH-M6 breaking down is organized photo.
Fig. 2 is that the replica scanning electron microscope of the inboard austenite grain boundary oxidation of iron scale before the 130 square billet BP05 breaking down is organized photo.
Embodiment
Embodiment 1
The present invention produces among the 130 square billet ultra-low-carbon steel SWRCH-M6 in Shoudu Iron and Steel Co first wire rolling plants and is applied, and is used to study the preceding square billet austenite grain size size of breaking down, concrete steps:
A. the heating furnace remaining oxygen is controlled at 2.4%, and 1080 ℃ of soaking zone temperature, after square billet goes out heating furnace, after the dephosphorization of 14Mpa high pressure, obtain the square billet scale on surface at 2.5 hours heat time heating times;
B. iron scale was carried out after the ultrasonic cleaning 10 minutes, and be prepared into the scanning electron microscope analysis sample;
C. analyze iron scale under the scanning electron microscope and press close to the pattern of square billet matrix one side, scanning electron microscope voltage 15Kv obtains the square billet organization picture of grain boundary;
D. grain boundary oxidation organizes photo to utilize the preceding grain size of Imagetool software test square billet breaking down.
Embodiment 2
The present invention produces among the 130 square billet BP05 in Shoudu Iron and Steel Co first wire rolling plants and is applied, and is used to study the preceding square billet austenite grain size size of breaking down, concrete steps:
A. the heating furnace remaining oxygen is controlled at 2%, and 1050 ℃ of soaking zone temperature, after square billet goes out heating furnace, after the dephosphorization of 16Mpa high pressure, obtain the square billet scale on surface at 3 hours heat time heating times;
B. iron scale was carried out after the ultrasonic cleaning 10 minutes, and be prepared into the scanning electron microscope analysis sample;
C. analyze iron scale under the scanning electron microscope and press close to the pattern of square billet matrix one side, scanning electron microscope voltage 15Kv obtains the square billet organization picture of grain boundary;
D. grain boundary oxidation organizes photo to utilize the preceding grain size of Imagetool software test square billet breaking down.
Claims (2)
1. method of testing grain size before the square billet breaking down, its feature is being: testing procedure is:
A. furnace temp is controlled at 980-1150 ℃, remaining oxygen 2.5-6%, 2.5-4 hour heat time heating time;
B. through high-pressure water descaling, water pressure 13-16Mpa obtained the square billet scale on surface after steel billet was come out of the stove;
C. iron scale is carried out ultrasonic cleaning 8-10 minute, be prepared into the scanning electron microscope analysis sample;
D. analyze iron scale and press close to the pattern of square billet matrix one side under scanning electron microscope, the Electronic Speculum Control of Voltage obtains square billet iron scale organization picture of grain boundary at 13-15Kv;
E. organize photo to utilize grain size before the breaking down of Imagetool software test square billet by grain boundary oxidation.
2. according to claims 1 described method, described Imagetool software is a kind of under various typical organizations prerequisite, and can carry out image and the data processing software that basal ration characterizes to tissue; Use the step of this software statistics crystallite dimension:
(1) activates this software, open a graphic file;
(2) if will survey crystallite dimension, calibrate Calibrate earlier; In settings menu, click Calibratespacial measurement; The straight line of standardized known length, and input length value;
(3) click the Distance wicket, measure, line of every picture, length value enters the Results window automatically, and provides mean value and variance;
(4) be under the state of activation at the Results window, preserve measurement data.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009102431716A CN101776624B (en) | 2009-12-31 | 2009-12-31 | Method for testing grain size before blooming of square billets |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009102431716A CN101776624B (en) | 2009-12-31 | 2009-12-31 | Method for testing grain size before blooming of square billets |
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| Publication Number | Publication Date |
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| CN101776624A true CN101776624A (en) | 2010-07-14 |
| CN101776624B CN101776624B (en) | 2012-06-27 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104949769A (en) * | 2015-06-23 | 2015-09-30 | 南车戚墅堰机车有限公司 | Method for rapidly finding carburization temperature field change without dependence on temperature measurement system |
| CN107561106A (en) * | 2017-08-31 | 2018-01-09 | 长江存储科技有限责任公司 | A kind of measuring method and device of streak shape morphology characterization parameter |
| CN110487985A (en) * | 2019-08-15 | 2019-11-22 | 钢铁研究总院 | A kind of measurement method of low-alloy steel heat treatment process austenite grain size |
| CN112630255A (en) * | 2020-12-11 | 2021-04-09 | 北京首钢股份有限公司 | Method and device for detecting influence of heating process on quality and performance of variety steel |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1107859C (en) * | 2000-06-01 | 2003-05-07 | 大连理工大学 | Computerized method and device for measuring grain size |
| CN101413786B (en) * | 2008-11-28 | 2011-04-20 | 首钢总公司 | Method for measuring austenite crystal dimension by high temperature laser microscope |
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2009
- 2009-12-31 CN CN2009102431716A patent/CN101776624B/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104949769A (en) * | 2015-06-23 | 2015-09-30 | 南车戚墅堰机车有限公司 | Method for rapidly finding carburization temperature field change without dependence on temperature measurement system |
| CN104949769B (en) * | 2015-06-23 | 2018-04-03 | 南车戚墅堰机车有限公司 | A kind of method that the change of carburizing temperature field is quickly found not against temp measuring system |
| CN107561106A (en) * | 2017-08-31 | 2018-01-09 | 长江存储科技有限责任公司 | A kind of measuring method and device of streak shape morphology characterization parameter |
| CN107561106B (en) * | 2017-08-31 | 2020-06-05 | 长江存储科技有限责任公司 | Method and device for measuring characterization parameters of streak-shaped morphology |
| CN110487985A (en) * | 2019-08-15 | 2019-11-22 | 钢铁研究总院 | A kind of measurement method of low-alloy steel heat treatment process austenite grain size |
| CN112630255A (en) * | 2020-12-11 | 2021-04-09 | 北京首钢股份有限公司 | Method and device for detecting influence of heating process on quality and performance of variety steel |
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| CN101776624B (en) | 2012-06-27 |
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Address after: 100041 Shijingshan Road, Shijingshan District, Shijingshan District, Beijing Patentee after: Shougang Group Co. Ltd. Address before: 100041 Shijingshan Road, Shijingshan District, Shijingshan District, Beijing Patentee before: Capital Iron & Steel General Company |
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