CN103454294A - Method for quantitatively evaluating structures of various phases in hot-rolled TRIP steel - Google Patents

Method for quantitatively evaluating structures of various phases in hot-rolled TRIP steel Download PDF

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CN103454294A
CN103454294A CN201310359250XA CN201310359250A CN103454294A CN 103454294 A CN103454294 A CN 103454294A CN 201310359250X A CN201310359250X A CN 201310359250XA CN 201310359250 A CN201310359250 A CN 201310359250A CN 103454294 A CN103454294 A CN 103454294A
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phase
ebsd
bainite
ferrite
analysis
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CN103454294B (en
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牛亚慧
张珂
洪慧敏
金传伟
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Institute Of Research Of Iron & Steel shagang jiangsu Province
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Abstract

The invention relates to a method for quantitatively evaluating the structure of each phase in hot-rolled TRIP steel, which utilizes an electron back-scattering diffraction device equipped on a scanning electron microscope to quantitatively measure the FCC phase (residual austenite) and the BCC phase (ferrite, bainite and martensite) of the hot-rolled TRIP steel, and distinguishes the residual austenite according to the obvious difference of the structures of the FCC phase and the BCC phase; and according to the quality difference of three similar structural phase chrysanthemum pool patterns of ferrite, bainite and martensite, the gray value difference in a chrysanthemum pool zone contrast BC (band contrast) diagram in EBSD processing software is utilized to quantitatively distinguish the three phases, so that the multiphase separation and quantitative analysis of the hot-rolled TRIP steel are realized.

Description

A kind of method of each phase constitution in quantitative evaluation analysis of producing hot rolled TRIP
Technical field
The invention belongs in steel and organize field of measuring technique, particularly a kind of employing EBSD (Electron Backscattered Diffraction) technology is distinguished heterogeneous structure ferrite in the TRIP steel, bainite, martensite, is reached retained austenite four mutually and quantitative analysis methods.
Background technology
TRIP (Transformation Induced Plasticity) steel is transformation induced plasticity steel, by phase-change induced property effect, makes retained austenite in steel that the martensitic phase change occur under the plastic yield effect, thereby improves intensity and the toughness of steel.Generally contain ferrite, bainite, austenite structure in the TRIP steel, after deformation induced phase transformation occurs, also have martensitic stucture.Austenite belongs to face-centred cubic structure, according to the difference of structure, be easy to it is distinguished, and the structure of all the other three-phases such as ferrite is very similar, is difficult to directly the three be distinguished.
The heterogeneous classic method of distinguishing of TRIP steel has following two kinds: 1. metallographic decoration method, the method utilizes different tissues degree of staining difference to distinguish, can differentiate ferrite and bainite after this method is painted, but, for the TRIP steel that the M/A island is arranged, colouring can't directly distinguish retained austenite and martensite; 2. large low-angle boundary and inverse pole figure imaging method, the method is at first different with the FCC phase structure according to BCC, realize separating of BCC phase and FCC phase, in recycling ferrite and bainite, (in bainite structure, low-angle boundary is many for grain-oriented difference, in ferritic structure, high-angle boundary is many), realize that ferrite separates with bainite, recycle the content that software for calculation independently obtains the three, the same indistinguishable retained austenite of the method and martensite.
Summary of the invention
The object of the present invention is to provide a kind of EBSD of employing effectively to distinguish the method for heterogeneous structure in analysis of producing hot rolled TRIP and quantitative test thereof, mainly utilize the EBSD device on scanning electron microscope to be distinguished and quantitative test the ferrite in the TRIP steel, bainite, martensite and retained austenite.
Concrete technology step of the present invention is as follows:
1. the method for each phase constitution in a quantitative evaluation analysis of producing hot rolled TRIP, specifically carry out according to the following steps:
1) get analysis of producing hot rolled TRIP sample small sample to be measured, sample is block, and upper and lower surface is parallel, and the cross section that needs image data is refined;
2) sample refined is placed on Full-automatic polishing machine and carries out meticulous polishing, make surfacing to be measured unstressed, be placed in rapidly absolute ethyl alcohol and clean and dry up;
3) sample of polishing is put into to mordant and corroded, corrosion is under optical microscope, seeing crystal boundary; Wherein, described mordant is: 2~4% nitals;
4) described sample is carried out to the EBSD analysis, in selecting mutually, choose BCC phase and FCC phase;
5) step-length of selecting is less than 0.1 μ m;
6) after the EBSD data acquisition completes, open analysis software, collected EBSD data carried out to following analyzing and processing:
Utilize EBSD phase resolution techniques to be separated retained austenite, press the bimodal gray-scale value scope in BC gray scale histogram, bainite and ferrite are differentiated, then it is painted that the three-phase of having distinguished is carried out to colour, is martensite and do not mark the look zone;
7) according to the area ratio of three-phase cromogram, utilize the direct statistical computation of EBSD software, draw the content of this three-phase, then draw martensitic content by conversion, finally determine the ratio of four phases in analysis of producing hot rolled TRIP.
Further, the processing mode of described step 6) replaces with: first utilize EBSD phase resolution techniques to carry out independence to retained austenite in BC figure painted, press again the bimodal gray-scale value scope in BC gray scale histogram, bainite and ferrite being carried out to different colours painted, is martensite and do not mark the look zone.
Perhaps, the processing mode of described step 6) replaces with: first press the bimodal gray-scale value scope in BC gray scale histogram, bainite and ferrite are carried out to different colours painted, it is painted that recycling EBSD phase resolution techniques is carried out independence to retained austenite in BC figure, and do not mark the look zone, is martensite.
In utilizing EBSD research iron and steel organizational process, utilize the difference of phase structure residual austenite soma can be distinguished from the TRIP steel, and ferrite, bainite and martensite belongs to the analog structure phase, be difficult to direct separation, but because the otherness of three-phase distortion of lattice causes Kikuchi style quality difference, can carry out the resolution of quantification to this three-phase according to the Kikuchi band contrast figure BC value in the EBSD process software, use the gray-scale value (between 0-255) of BC gray scale frequency plot directly to distinguish ferrite and bainite, residue is martensite mutually, thereby reach heterogeneous resolution and the quantitative test of TRIP steel.
The invention has the beneficial effects as follows: the method is tested and can be realized that ferrite in analysis of producing hot rolled TRIP, bainite, martensite and retained austenite are distinguished and quantitative test by EBSD.The method quantitative result is comparatively accurate, and can better reflect the phase distributing position, obtains qualitative distribution and quantitative result simultaneously.
The accompanying drawing explanation
The micro-organization chart that Fig. 1 is analysis of producing hot rolled TRIP EBSD Experimental Area in embodiment 1;
Fig. 2 is the BC figure obtained after the analysis of producing hot rolled TRIP Data Processing in Experiment in embodiment 1;
Fig. 3 is retained austenite color-patch map in analysis of producing hot rolled TRIP BC figure in embodiment 1;
Fig. 4 is analysis of producing hot rolled TRIP BC gray scale frequency plot in embodiment 1;
Fig. 5 is ferrite, bainite, retained austenite in analysis of producing hot rolled TRIP BC figure in embodiment 1, martensite is painted and the quantitative distribution plan of four phases.
Embodiment
Embodiment 1
1) adopt line to cut the sample of suitable size, with flint glass paper, six faces of sample are roughly ground, make upper and lower surface parallel, then the face to wanted image data is refined on full-automatic sample grinder;
2) sample is placed in to meticulous mechanical buffing on Full-automatic polishing machine, selecting granularity is 0.02 μ m left and right, polishing time is the 3min left and right, until do not observe obvious cut at 50~100 times of lower specimen surfaces of metaloscope, the polishing sample is cleaned rapidly in absolute ethyl alcohol, and uses the hair dryer hot blast drying;
3) polishing no marking sample is carried out to light corrosion fast, extent of corrosion is to seeing that crystal boundary is advisable under can optical microscope; Wherein mordant used is: 4% nital;
4) by NEC JSM-7001 type field emission scanning electron microscope, sample is carried out to microstructure observation, utilize the HKL Channel 5EBSD system be equipped with to carry out the EBSD data acquisition to the same area, when data are processed, selecting is BCC phase and FCC phase mutually; The microcell organization chart obtained as shown in Figure 1;
Set step-length 0.075 μ m while 5) gathering chooses the zone of 75 μ m * 75 μ m areas and carries out the EBSD experiment under 1000 times, the data that record is demarcated;
6) after the EBSD data acquisition completes, open analysis software, collected EBSD data carried out to following analyzing and processing:
1. distinguish the retained austenite phase: not punctuate and the mistake punctuate removed in experimental result are removed noise afterwards step by step, process data into again Kikuchi band contrast BC figure (as shown in Figure 2), in BC figure, utilize the body-centred structure of BCC phase and the centroid structure difference of FCC phase first the FCC in the TRIP steel to be given into mutually colored, with redness, mean, be about to retained austenite and directly distinguish, as shown in Figure 3;
2. define Bainite Phases of Some or ferritic phase: according to the height of bainite and the corresponding gray scale numerical value of ferrite Kikuchi style difference in quality, peak to BC gray scale frequency plot (as shown in Figure 4) is divided, gray scale numerical value 15~75 scopes are preserved into to independent data, define this scope and correspond to Bainite Phases of Some; Perhaps, gray scale numerical value 75~115 scopes are preserved into to independent data, define this scope and correspond to ferritic phase.
3. distinguish bainite, ferrite and martensite: by Bainite Phases of Some and remaining BCC phase (being ferrite), perhaps ferritic phase is given into colored with remaining BCC phase (being bainite), with yellow and green, mean respectively, and the zone of not painted (whitening look) is martensite, as shown in Figure 5;
4. quantitative test: according to heterogeneous color distribution (as shown in Figure 5), utilize HKL EBSD-Channel5 software quantitatively to calculate bainite, ferrite and the retained austenite of giving color, result shows that ferrite content is 56.70%, bainite content is 37.30%, residual austenite content is 3.83%, according to normalization, calculates that known martensite content is 2.17%.

Claims (3)

1. the method for each phase constitution in a quantitative evaluation analysis of producing hot rolled TRIP, is characterized in that, specifically carries out according to the following steps:
1) get analysis of producing hot rolled TRIP sample small sample to be measured, sample is block, and upper and lower surface is parallel, and the cross section that needs image data is refined;
2) sample refined is placed on Full-automatic polishing machine and carries out meticulous polishing, make surfacing to be measured unstressed, be placed in rapidly absolute ethyl alcohol and clean and dry up;
3) sample of polishing is put into to mordant and corroded, corrosion is under optical microscope, seeing crystal boundary; Wherein, described mordant is: 2~4% nitals;
4) described sample is carried out to the EBSD analysis, in selecting mutually, choose BCC phase and FCC phase;
5) step-length of selecting is less than 0.1 μ m;
6) after the EBSD data acquisition completes, open analysis software, collected EBSD data carried out to following analyzing and processing:
Utilize EBSD phase resolution techniques to be separated retained austenite, press the bimodal gray-scale value scope in BC gray scale histogram, bainite and ferrite are differentiated, then it is painted that the three-phase of having distinguished is carried out to colour, is martensite and do not mark the look zone;
7) according to the area ratio of three-phase cromogram, utilize the direct statistical computation of EBSD software, draw the content of this three-phase, then draw martensitic content by conversion, finally determine the ratio of four phases in analysis of producing hot rolled TRIP.
2. the method for each phase constitution in a kind of quantitative evaluation analysis of producing hot rolled TRIP according to claim 1, it is characterized in that, described step 6) replaces with following mode analyzing and processing: first utilize EBSD phase resolution techniques to carry out independence to retained austenite in BC figure painted, press again the bimodal gray-scale value scope in BC gray scale histogram, bainite and ferrite being carried out to different colours painted, is martensite and do not mark the look zone.
3. the method for each phase constitution in a kind of quantitative evaluation analysis of producing hot rolled TRIP according to claim 1, it is characterized in that, described step 6) replaces with following mode analyzing and processing: first press the bimodal gray-scale value scope in BC gray scale histogram, bainite and ferrite are carried out to different colours painted, it is painted that recycling EBSD phase resolution techniques is carried out independence to retained austenite in BC figure, and do not mark the look zone, is martensite.
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CN103969277A (en) * 2014-04-29 2014-08-06 江苏省沙钢钢铁研究院有限公司 Characterization method for distinguishing multiphase iron scale in hot rolled silicon steel
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CN105806867A (en) * 2016-05-25 2016-07-27 江苏省沙钢钢铁研究院有限公司 Analysis method for quantitatively evaluating alloy element segregation in high-temperature alloy
CN105956312A (en) * 2016-05-17 2016-09-21 洛阳Lyc轴承有限公司 Method for distinguishing high-carbon-chromium bearing steel quenching structures
JP2018525604A (en) * 2016-06-29 2018-09-06 Jfeスチール株式会社 Separation visualization method of austenite phase, martensite phase and bainite-ferrite matrix in bainite steel and bainite steel slab for microstructure observation
CN110987991A (en) * 2019-11-18 2020-04-10 上海航天精密机械研究所 Method for counting ultra-fine ferrite phase in austenitic stainless steel welding seam
WO2022243576A1 (en) 2021-05-17 2022-11-24 Asociacion Centro Tecnologico Ceit Method for the quantitative assessment of the area affected by the transformation of ferrite in dual-phase steels

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103969277A (en) * 2014-04-29 2014-08-06 江苏省沙钢钢铁研究院有限公司 Characterization method for distinguishing multiphase iron scale in hot rolled silicon steel
CN104090033A (en) * 2014-07-16 2014-10-08 大连理工大学 Method for establishing FDTD (Finite Difference Time Domain) ultrasonic detection simulation model of coarse crystal material based on EBSD (Electron Back-Scattered Diffraction) spectrum
CN104090033B (en) * 2014-07-16 2016-06-15 大连理工大学 Coarse grain material FDTD ultrasound detection Building of Simulation Model method based on EBSD collection of illustrative plates
CN105956312A (en) * 2016-05-17 2016-09-21 洛阳Lyc轴承有限公司 Method for distinguishing high-carbon-chromium bearing steel quenching structures
CN105956312B (en) * 2016-05-17 2019-02-22 洛阳Lyc轴承有限公司 A method of distinguishing high-carbon-chromium bearing steel quenching structure
CN105806867A (en) * 2016-05-25 2016-07-27 江苏省沙钢钢铁研究院有限公司 Analysis method for quantitatively evaluating alloy element segregation in high-temperature alloy
CN105806867B (en) * 2016-05-25 2018-11-06 江苏省沙钢钢铁研究院有限公司 Analysis method for quantitatively evaluating alloy element segregation in high-temperature alloy
JP2018525604A (en) * 2016-06-29 2018-09-06 Jfeスチール株式会社 Separation visualization method of austenite phase, martensite phase and bainite-ferrite matrix in bainite steel and bainite steel slab for microstructure observation
CN110987991A (en) * 2019-11-18 2020-04-10 上海航天精密机械研究所 Method for counting ultra-fine ferrite phase in austenitic stainless steel welding seam
WO2022243576A1 (en) 2021-05-17 2022-11-24 Asociacion Centro Tecnologico Ceit Method for the quantitative assessment of the area affected by the transformation of ferrite in dual-phase steels

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