CN102866170A - Method for evaluating forms, sizes and distributions of free cementites in aluminum killed steel - Google Patents
Method for evaluating forms, sizes and distributions of free cementites in aluminum killed steel Download PDFInfo
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Abstract
The invention relates to a method for evaluating forms, sizes and distributions of free cementites in aluminum killed steel, belongs to the technical field of free carbon detection in steel, and solves the problems of qualitative and quantitative representations of the forms, the sizes and the distributions of the free cementites in the aluminum killed steel. A representation method comprises the following steps of: carrying out EBSD (Electron Back-Scattered Diffraction) face scanning on a sample after carrying out electrolytic polishing on the sample, receiving a diffraction signal by an EBSD probe and forming an image, and thus obtaining a pattern contrast quality map which represents the qualities of Kikuchi patterns by different contrasts; as the surface stresses are residual on free cementite particles, the Kikuchi patterns are vague, and most of the particles represent zero solution characteristics; compared with the patterns of ferrites, the differences of the pattern contrasts of the Kikuchi patterns are obviously larger; and thus the data analyzing is carried out on the sizes and the forms of the free cementite particles and the distributions of the free cementite particles in a matrix by virtue of the characteristics and EBSD processing software, and the content, the sizes and the distributions of the free cementite particles in a selected region are measured.
Description
Technical field
The invention belongs to steel Free Carbon detection technique field, particularly relate to a kind of method of estimating free cementite in the aluminium killed steel, size and distribution, by qualitative, the quantitatively characterizing of EBSD (EBSD is the hand-written letter abbreviations of the English word of " Electron Back-Scattered Diffraction ") technology to form, size and the distribution of the free cementite in the aluminium killed steel.
Background technology
Development along with auto industry and household electrical appliances industry, for the low-carbon (LC) annealed sheet steel comparatively vast potential for future development has been arranged, especially carbon aluminium-killed steel has good performance because of it and lower cost of alloy is widely used at automobile and the common inner and outer plates of household electrical appliances, but aluminium killed steel also exists obvious deficiency, i.e. free cementite particle form in annealing process, the formation of size and distribution and control, the scholar who has thinks that the existence meeting of thick carbide particle (free cementite) causes cracking and finally affects its drawing performance near the crystal boundary in punching course.Therefore, be necessary qualitative and quantitative analysis is carried out in content, form, size and the distribution of free cementite in the carbon aluminium-killed steel, traditional method is to adopt metallographic method, with the free cementite etch out, in its form of optical microphotograph Microscopic observation and distribution, but the characterizing method of the form of estimating free cementite, size and the distribution of qualitative, quantitative is also actually rare.
This patent has developed the method that a kind of simultaneously qualitative, quantitative characterizes free cementite, size and distribution, for the annealing process optimization of aluminium killed steel is laid a good foundation by the Electron Back-Scattered Diffraction technology.
Summary of the invention
The object of the present invention is to provide a kind of method of estimating free cementite in the aluminium killed steel, size and distribution, by qualitative, the quantitatively characterizing of EBSD technology to form, size and the distribution of the free cementite in the aluminium killed steel, especially estimate form, size and the distribution of free cementite by style contrast quality and null solution feature.
The proposition of the method mainly by field emission scanning electron microscope entrained annex EBSD measure, its measuring principle can simply be summarised as: from the filament emission electronics, form the electron beam light source, focusing by condenser and object lens, obtain the less bundle spot of a diameter, be radiated at the sample polished surface of inclination certain angle, from sample, inspire backscattered electron, the diffraction pattern that these backscattered electrons form gathers and sends to computing machine through the EBSD probe, the scanning yoke control electron beam of Electronic Speculum carries out point by point scanning, finally obtained to represent with different contrasts the style contrast Quality Map of Kikuchi style quality, because the Kikuchi style of free cementite is smudgy, most particles present the null solution feature, its contrast is obviously different from matrix, utilize this feature to the size of free cementite particle among the figure, data analysis is carried out in form and the distribution in matrix thereof, measures the content of free cementite particle in the selected areas, size, form and distribution.
The present invention mainly realizes the sign of free cementite, size and distribution in the aluminium killed steel by the EBSD technology, the method comprises the setting of preparation of samples, electron beam state, the selection of sweep parameter, the steps such as the processing of orientation data and data analysis, concrete steps are as follows:
1, preparation of samples
The basic demand of EBSD sample effects on surface is smooth, cleaning, and without the residual deformation layer of sample making course.Sample size requires length 10～15mm, width 5～10mm, and thickness 0.5～3mm, and guarantee that upper and lower surface is parallel, and remove residual stress by the effects on surface electropolishing, finally obtain smooth, clean, a bright polished surface and carry out face scanning.
2, set the electron beam state
In order to obtain comparatively clearly Kikuchi style, need to some parameters of Electronic Speculum be arranged, such as accelerating potential, line, lens isis, sample tilt angle, the parameters such as operating distance.According to the needs that EBSD analyzes, the optimum condition of its electron beam is accelerating potential 15～20kV, line 1～10nA, and 60～70 ° at sample stage angle of inclination, operating distance WD is 13～20mm, 3# or 4# lens isis all can.
3, the selection of sweep parameter
Not only to set the electron beam state, also need according to the size form of free cementite sweep parameter to be set, such as step-length, enlargement factor, calibration file, crystal structure and style acquisition time etc., the setting principle of step-length is that 1/5～1/10 of free cementite particle size is the best, the selection of enlargement factor mainly is to set according to the content of free cementite particle in the visual field, be generally 1000～5000 times, the selection of calibration file mainly arranges according to the electron beam state, common crystal structure has body centred cubic (bcc), also have face-centered cubic (fcc) and quadrature etc., the style acquisition time will be set according to actual conditions, time is too short, the local resolution of face scanning result is unclear, and overlong time is more time-consuming, can not in time analyze the result.
4, data are processed and are analyzed
Behind the face end of scan, need to process the data result, need EBSD analysis software opposite scanning result to process this moment again, at first remove at the interface null solution point of part in the visual field, remove singular point and mistake punctuate again, can obtain take ferrite as matrix, the style contrast Quality Map of the granular free cementite of simultaneous, grain orientation distribution plan, crystallite dimension, the results such as length breadth ratio, utilize style contrast and null solution characteristic to size, the form of free cementite, distribute and carry out Data Management Analysis.
The advantage of the method is: the first is take electron beam as light source, its resolution is far above visible light source, and the point by point scanning by electron beam, realize that backscattered electron carries diffracted signal and carries out orientation mapping, utilize the strong and weak difference of diffracted signal of each phase to realize the stratification of each phase contrast in the image, distribute to obtain Kikuchi style contrast Quality Map and null solution; It two is by the EBSD analysis software in the style contrast Quality Map each to be carried out measurements and calculations mutually.
Advantage of the present invention is, by EBSD technology and corresponding analysis software, utilizes style contrast and null solution characteristic can realize meticulous analysis is carried out in size, form and the distribution of free cementite in the aluminium killed steel.
Be to utilize the EBSD technology that the microstructure in the mild carbon steel (ferritic phase and free cementite particle) is carried out face scanning, its EBSD probe receives diffracted signal and carries out imaging, acquisition represents the style contrast Quality Map of Kikuchi style quality with different contrasts, because the Kikuchi style of free cementite is smudgy, most particles present the null solution feature, its contrast is obviously different from matrix, utilize this feature to the size of free cementite particle among the figure, data analysis is carried out in form and the distribution in matrix thereof, measures the content of free cementite particle in the selected areas, size, form and distribution.
Description of drawings
The distribution of free cementite particle in matrix that represents with the null solution form in Fig. 1 aluminium killed steel.
The distribution of free cementite particle in matrix that represents with the form of style contrast in Fig. 2 aluminium killed steel.
The size distribution plot of free cementite in Fig. 3 aluminium killed steel.
The area distribution plot of free cementite in Fig. 4 aluminium killed steel.
The aspect ratio distribution figure of free cementite in Fig. 5 aluminium killed steel.
Embodiment
Size, form and the distribution of free cementite particle in the SPCC aluminium killed steel
1, preparation of samples.According to EBSD sample preparation requirement, at first the bulk sample line is cut to the thin slice sample of long 10mm, wide 10mm, thickness 1mm, guarantee that upper and lower surface is parallel, then carry out the pre-grinding and polishing on surface, carry out again electropolishing, remove the stressor layers on surface, guarantee that the Kikuchi style is high-visible.
2, electron beam state.In order to obtain tiny bundle spot, need to adjust accelerating potential, probe current, the parameters such as operating distance, the top condition that this test is selected: accelerating potential 15kV, probe current 2.5nA, this moment, beam spot diameter, was less than 100nm, operating distance 15mm, the 3# lens isis is selected at 70 ° at sample stage angle of inclination simultaneously.
3, sweep parameter.After electron beam has set, need to set the face scanning major parameter of EBSD scanning software Flamenco, such as step-length, enlargement factor, calibration file and style acquisition time etc., consider content and the physical size of free cementite particle in the visual field, select suitable sweep parameter, step-length 0.06 μ m, 1000 times of enlargement factors, crystal structure is body centred cubic (bcc), style acquisition time 15h.
4, data are processed.The data that obtain by the EBSD scanning software need further to carry out the data processing by analysis software Project manager, comprising removing noise, singular point and mistake punctuate etc.The purpose of denoising is that the null solution point of the single or several block of pixels on the interface is filled up, so that the interface is complete, and then removes the interior singular point of crystal grain and mistake punctuate.Matrix is ferrite in the face scintigram, its Kikuchi style is clear, and it is hard and have a residual stress to be distributed in free cementite particle in the matrix, most without the Kikuchi style in the process of demarcating, therefore it shows as null solution feature (see figure 1), be presented in the style contrast Quality Map (see figure 2) with certain contrast simultaneously, therefore utilize this point by analysis software this null solution feature to be carried out data statistics, calculate size and the area (its data see Table 1) of each free cementite particle, recycling Origin software is to the free cementite diameter, area and length breadth ratio data are drawn, obtain respectively free cementite size distribution plot (see figure 3) and area distribution plot (see figure 4), and aspect ratio distribution figure (see figure 5), simultaneously length breadth ratio and form are connected, and be defined, length breadth ratio greater than 1 less than 2 be block, length breadth ratio greater than 2 less than 4 be corynebacterium, length breadth ratio greater than 4 be strip (seeing Table 2).
To sum up analyze as can be known, free cementite particle mainly is interspersed in ferrite crystal grain in the aluminium killed steel, and distribute on the crystal boundary less, the size majority of free cementite is less than 1 μ m, its average-size is about 0.5 μ m; The area majority of free cementite is less than 1 μ m
2, the mean value of its area is about 0.3 μ m
2The form majority of free cementite is take block and corynebacterium as main, and strip is less.
The tables of data of free cementite diameter, area and length breadth ratio in table 1 aluminium killed steel
The free cementite particle proportion of different shape in table 2 aluminium killed steel
Claims (1)
1. method of estimating free cementite in the aluminium killed steel, size and distribution may further comprise the steps:
(1) preparation of samples: the basic demand of carrying out the sample effects on surface of EBSD scanning is smooth, cleaning, and without the residual deformation layer of sample making course; Sample size requires length 10～15mm, width 5～10mm, and thickness 0.5～3mm, and guarantee that upper and lower surface is parallel, remove residual stress by the effects on surface electropolishing.
(2) set the electron beam state: set accelerating potential, line, lens isis, sample tilt angle, operating distance; According to the needs that EBSD analyzes, its beam voltage 15～20kV, line 1～10nA, 60～70 ° at sample stage angle of inclination, operating distance WD is 13～20mm, 3# or 4# lens isis;
(3) the face sweep parameter is set: step-length: 1/5～1/10 of free cementite particle size, enlargement factor: 1000～5000 times;
(4) data are processed and are analyzed: behind the face end of scan, need EBSD analysis software opposite scanning result to process again, remove part null solution point, singular point and the mistake punctuate at the interface in the visual field, acquisition take ferrite as matrix, the style contrast Quality Map of the granular free cementite of simultaneous, grain orientation distribution plan, crystallite dimension, length breadth ratio result utilizes style contrast and null solution characteristic to size, the form of free cementite, distributes to carry out Data Management Analysis.
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| CN103336323A (en) * | 2013-03-18 | 2013-10-02 | 内蒙古工业大学 | Method for manufacturing high-frequency optical gratings through multiple scanning electron beam lithography |
| CN103529065A (en) * | 2013-10-10 | 2014-01-22 | 中国石油天然气集团公司 | Measurement method for effective grain size of structural steel with complex microstructure |
| CN103837557A (en) * | 2014-01-21 | 2014-06-04 | 首钢总公司 | Method of representing microstructure of scale on section of hot-rolled steel plate by adoption of EBSD |
| CN104280413A (en) * | 2014-10-16 | 2015-01-14 | 江苏省沙钢钢铁研究院有限公司 | Method for counting length-width ratio of manganese sulfide impurity in steel |
| CN107894433A (en) * | 2017-10-10 | 2018-04-10 | 首钢集团有限公司 | A kind of method of quantitatively characterizing composite diphase material principal phase tissue crystallite dimension |
| CN109254022A (en) * | 2018-10-24 | 2019-01-22 | 首钢智新迁安电磁材料有限公司 | A method of measurement crystallite dimension |
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| CN103336323A (en) * | 2013-03-18 | 2013-10-02 | 内蒙古工业大学 | Method for manufacturing high-frequency optical gratings through multiple scanning electron beam lithography |
| CN103336323B (en) * | 2013-03-18 | 2017-03-01 | 内蒙古工业大学 | The method that Multiple-Scan electron beam lithography makes high-frequency grating |
| CN103529065A (en) * | 2013-10-10 | 2014-01-22 | 中国石油天然气集团公司 | Measurement method for effective grain size of structural steel with complex microstructure |
| CN103529065B (en) * | 2013-10-10 | 2015-11-18 | 中国石油天然气集团公司 | Measure the method for the effective particle size of complicated heterogeneous microstructure steel |
| CN103837557A (en) * | 2014-01-21 | 2014-06-04 | 首钢总公司 | Method of representing microstructure of scale on section of hot-rolled steel plate by adoption of EBSD |
| CN103837557B (en) * | 2014-01-21 | 2016-03-30 | 首钢总公司 | EBSD is adopted to characterize the method for hot rolled steel plate cross section iron scale micromechanism |
| CN104280413A (en) * | 2014-10-16 | 2015-01-14 | 江苏省沙钢钢铁研究院有限公司 | Method for counting length-width ratio of manganese sulfide impurity in steel |
| CN107894433A (en) * | 2017-10-10 | 2018-04-10 | 首钢集团有限公司 | A kind of method of quantitatively characterizing composite diphase material principal phase tissue crystallite dimension |
| CN109254022A (en) * | 2018-10-24 | 2019-01-22 | 首钢智新迁安电磁材料有限公司 | A method of measurement crystallite dimension |
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Application publication date: 20130109 |