CN104111230B - Classified display and quantitative detection method for martensite and residual austenite in M-A island - Google Patents
Classified display and quantitative detection method for martensite and residual austenite in M-A island Download PDFInfo
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- 238000001514 detection method Methods 0.000 title abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 60
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 43
- 239000010959 steel Substances 0.000 claims abstract description 43
- 239000000463 material Substances 0.000 claims abstract description 38
- 229910001563 bainite Inorganic materials 0.000 claims abstract description 34
- 238000005260 corrosion Methods 0.000 claims abstract description 34
- 230000007797 corrosion Effects 0.000 claims abstract description 34
- 238000005498 polishing Methods 0.000 claims abstract description 30
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 20
- 239000000956 alloy Substances 0.000 claims abstract description 20
- 238000000227 grinding Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 10
- 229910001568 polygonal ferrite Inorganic materials 0.000 claims abstract description 8
- 230000000717 retained effect Effects 0.000 claims description 44
- 238000005530 etching Methods 0.000 claims description 20
- 238000004458 analytical method Methods 0.000 claims description 17
- 238000002604 ultrasonography Methods 0.000 claims description 11
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
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- 239000006071 cream Substances 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 6
- 238000005088 metallography Methods 0.000 claims description 6
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- 238000005275 alloying Methods 0.000 claims description 5
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- 229910001149 41xx steel Inorganic materials 0.000 claims description 3
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- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 claims description 3
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- 239000010432 diamond Substances 0.000 claims description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910000851 Alloy steel Inorganic materials 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- HQFCOGRKGVGYBB-UHFFFAOYSA-N ethanol;nitric acid Chemical compound CCO.O[N+]([O-])=O HQFCOGRKGVGYBB-UHFFFAOYSA-N 0.000 claims description 2
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 10
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- 238000004445 quantitative analysis Methods 0.000 abstract description 2
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- 229910000794 TRIP steel Inorganic materials 0.000 description 1
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- 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 1
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- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
The invention relates to microstructure classified display and quantitative detection technology in iron and steel material, belongs to the field of iron and steel material, and particularly relates to a classified display and quantitative detection method for martensite and residual austenite in low-alloy granular bainite steel martensite/austenite island (M-A island). The method comprises steps: (1) a grinding and mechanical polishing method is used for preparing a low-alloy granular bainite steel metallographic sample; (2) an electrolytic polishing method is used for removing the stress layer on the surface of the metallographic sample, a nitric acid alcohol solution of 2wt% to 6wt% is then used for carrying out pre-corrosion for 5 to 15s, and absolute alcohol is finally used for ultrasonic cleaning for 10 to 20m; (3) the metallographic sample after ultrasonic cleaning is placed in a furnace free of atmosphere protection at the temperature of 150 to 300 DEG C for heat preservation for 2 to 6 hours, and when getting out of the furnace, the metallographic sample is placed in a dryer and cooled in the air till the room temperature; (4) the microscopic structure is observed in a metallographic microscope, wherein polygonal ferrite and bainitic ferrite are bluish violet, the martensite is brown and the residual austenite is off-white; and (5) distribution of each phase of the structure and quantitative analysis are carried out.
Description
Technical field
The present invention relates to microstructure classification shows and quantitative measurement technology in ferrous materials, belong to field of iron and steel, it is special
It is not that martensite is shown with the classification of retained austenite in a kind of low-alloy nodular bainite steel martensite/austenite island (M-A islands)
Show and quantitative detecting method.
Background technology
Low-alloy nodular bainite steel is due to preferable obdurability, excellent hydrogen embrittlement energy and appropriate high temperature creep-resisting
Performance, is widely used and large-scale hydrogenation reactor, nuclear power cylinder body and some the strength of materials and resistance to elevated temperatures are had necessarily
On the part of requirement.But, with the continuous expansion and the continuous increase of nuclear power power of hydrogenation plant scale, hydrogenation reaction wall
Thick and nuclear pressure container wall thickness is dramatically increased.Therefore, grain is readily obtained due to the restriction of cooling rate during actual heat treatment
Shape bainite or grain structure, the content on the martensite/austenite island (M-A islands) in this granular bainite, pattern, size,
It is distributed the mechanical property to steel and produces material impact, particularly low temperature impact properties.Therefore, accurate observation, the granular bayesian of resolution
Body or grain structure Zhong M-A islands, and martensite and retained austenite in M-A islands, it is excellent for the microstructure of understanding material
The performance for changing material is particularly significant.Using quantitative metallographic analysis technology to the difficult point of nodular bainite steel fabric analysiss it is：It is right
The identification and extraction of feature organization, with traditional etching pit method, can only obtain the gray level image of microscopic structure, each phase
Between be not enough substantially difficult to differentiate between due to contrast.And utilize current colour metallograpy corrosion technology, it is also difficult to distinguish in M-A islands
Martensite and retained austenite, so as to cause the part material particular in fabric analysiss to be ignored, are unfavorable for determining for feature organization
Amount analysis.
Chinese patent application (publication number CN101382494A, publication date 2009-3-11, applicant：Wuhan iron and steel (group)
Company), display and the quantitative detecting method of retained austenite or island-like martensite-austenite in a kind of TRIP steel are proposed, mainly
, by traditional colour metallograpy corrosion technology, using LePara reagents, (sodium metabisulfite solution and picric acid ethanol are molten for content
Liquid mixes by a certain percentage) tissue after polishing is corroded, to the polygonal ferrite in tissue, bainite ferrite with
And M-A islands carry out quantitative metallography corrosion, but horse of the sample prepared using the caustic solution under metallurgical microscope, in M-A islands
Family name's body and retained austenite are all white, it is difficult to the quantitative statisticses on metallographic further to both.
With the continuous development of research meanses, although there is some means characterize the residual austenite in clear tissue at present
The scale of construction is (such as：Using method of magnetic measure or XRD measurement tissues in remained austenite content), but above-mentioned means not only process of the test
Complexity, and the integrated information of the amount on material structure Zhong M-A islands, distribution, size can not more intuitively be observed.And in scanning
The martensite and austenite in M-A islands can be differentiated under Electronic Speculum using electron backscattered technology (EBSD), while can also observe office
Portion region M-A islands distribution, but due to the martensite in M-A islands it is identical with matrix bainite ferrite structure, it is difficult to differentiate M-A
Martensite and bainite ferrite in island.What is more important, the sample preparation of EBSD technologies and observation process complexity, limit which wide
General application.
The content of the invention
In order to overcome the shortcomings of above-mentioned technology, it is an object of the invention to provide a kind of low-alloy nodular bainite steel geneva
In body/austenite island (M-A islands), martensite shows and quantitative detecting method that with the classification of retained austenite the method is can be bright
The aobvious simple high efficiency method for distinguishing martensite and retained austenite in M-A islands, is easy in scientific research and research and development of products to granular shellfish
The discriminating of family name body Gang Zhong M-A islands microstructure and detection by quantitative.
The technical scheme is that：
The classification of martensite and retained austenite in a kind of M-A islands shows and quantitative detecting method that its step is as follows：
(1) low-alloy nodular bainite steel test block to be detected is intercepted by sampling standard, using grinding, mechanical polishing mode
Prepare metallographic specimen；
(2) metallographic specimen Surface stress layer is removed with electrolytic polishing method, then using the nitric acid wine of 2wt%～6wt%
Sample after pre-etching is finally put into ultrasound wave cleaning used in dehydrated alcohol by smart solution pre-etching 5～15 seconds；
(3) metallographic specimen after clean ultrasound wave is placed in 150～300 DEG C without in atmosphere protection stove, and insulation 2～6 is little
When, it is placed in after coming out of the stove in exsiccator, is cooled to room temperature in atmosphere；
(4) in the tissue of metallography microscope Microscopic observation low-alloy nodular bainite steel：Polygonal ferrite and bainite ferrum
Ferritic is in bluish violet, and martensite is in brown, and retained austenite is in ecru；
(5) using quantitative analysis software to respectively mutually being observed and quantitative analyses in tissue.
The classification of martensite and retained austenite in described M-A islands shows and quantitative detecting method, using grinding, machinery
After polishing mode prepares metallographic specimen, need to carry out electrobrightening to sample using dehydrated alcohol-perchloric acid-distilled water solution,
To eliminate the decomposition that stress in sample making course causes retained austenite；Electrolytic polishing process is：40～60V of voltage, electric current 4～
6mA, -20 DEG C～-30 DEG C of electrolysis temperature；Polishing fluid：The perchloric acid alcoholic solution of 5～10wt%, 10～15wt% distilled water with
And the dehydrated alcohol of 75～85wt%, polishing time is in 30s～60s.
The classification of martensite and retained austenite in described M-A islands shows and quantitative detecting method, using 2wt%～
The nital pre-etching of 6wt% 5～15 seconds, can slightly see tissue clearly, under metallurgical microscope then by pre- corruption
Sample after erosion is put into ultrasound wave used in dehydrated alcohol and cleans 10～20 minutes, removes corrosion product.
The classification of martensite and retained austenite in described M-A islands shows and quantitative detecting method, ultrasound wave is cleaned
Metallographic specimen afterwards is placed in 150～260 DEG C without the sub- inside holding of atmosphere protection stove 2～6 hours, makes observation surface under perusal
Blueing color is advisable.
The classification of martensite and retained austenite in described M-A islands shows and quantitative detecting method, in metallurgical microscope
Lower observation, differentiates various phases in tissue by color contrast, and polygonal ferrite and bainite ferrite are in bluish violet, geneva
Body is in brown, and retained austenite is in ecru, differentiates each phase by color distinction and carries out quantitative analyses.
The classification of martensite and retained austenite in described M-A islands shows and quantitative detecting method, main in low-alloy steel
Alloying element content is less than 5wt.%, and material microstructure is based on granular bainite.
The classification of martensite and retained austenite in described M-A islands shows and quantitative detecting method, the granular shellfish of low-alloy
Family name's body steel be alloying element content less than the CrMo systems of 5wt.%, NiCr systems, MnMoNi systems, SiMn systems, SiMnMo systems,
CrMnSi systems, CrMnMo systems or CrNiMo systems.
The classification of martensite and retained austenite in described M-A islands shows and quantitative detecting method, grinds sample in gold
Roughly ground on phase sample Plane surface grinding machine, respectively with 150#, 400#, 800#, 1200#, 2000# abrasive paper for metallograph on Automatic Grinding Prototype
Fine grinding, perusal do not see obvious cut, are that subsequent mechanical polishing is prepared.
The classification of martensite and retained austenite in described M-A islands shows and quantitative detecting method, mechanically polishes rotating speed
In 250～350r/min, adopt polishing grinding cream for W2.5 granularities diamond polishing cream, after polishing, specimen surface is smooth has no time
Minute surface and examine under a microscope without tiny cut.
The classification of martensite and retained austenite in described M-A islands shows and quantitative detecting method, with temperature retention time
Extend, specimen surface can take out from calorstat by greyish white-orange-royal purple color change, when sample is in bluish violet and be placed in drying
In device, room temperature is cooled in atmosphere；According to the film forming thickness principle that can produce preferable interference effect, film forming thickness control exists
300～600 angstroms of scopes.
The ultimate principle of the present invention is as follows：
After the metallographic specimen that test specimens to be checked are prepared using conventional method, need to carry out at electrobrightening sample first
Reason, this is because the retained austenite in sample in M-A islands is possible to grinding and stress/strain occurs in polishing specimen
Caused decomposition, so as to have a negative impact to the precision of testing result.And impacted can be answered by electrobrightening process
Power layer is got rid of, while not producing new stress.
After electrobrightening, sample needs gently to corrode in the nital of 2～6wt%, the Main Function of light corrosion
There are two, one is, as the resistance to corrosion of each phase in material is different, rugged shape to be produced in material surface Jing after corrosion
Looks, so as to different patterns are presented under metallurgical microscope；Two is the tissue after light corrosion, can be produced in follow-up oxidizing process
The different oxidation product of life, so as to different color and lusters are presented under metallurgical microscope.
After light corrosion, the corrosion product that specimen surface will be attached to after corrosion using ultrasound wave is needed to remove, it is to avoid to follow-up
Oxidizing process have a negative impact.
Sample after light corrosion is placed on the main purpose aoxidized in 150～300 DEG C of stoves without atmosphere protection is：
Microscopic structure after light corrosion is carried out into heat-tinting because it is different be organized in light corrosion process in produce different corrosion and produce
Thing, and different color and lusters after different corrosion products is oxidized, are presented, so as to reach the purpose for differentiating different tissues.The temperature of oxidation
Degree can not be too high, to avoid causing retained austenite in M-A islands to decompose, affects certainty of measurement.According to low-alloy granular bainite
The decomposition temperature of steel retained austenite, determines that highest oxidation temperature is 300 DEG C.
Advantages of the present invention and beneficial effect are：
1st, the sample prepared using common etching pit method can only see ferrite clearly, and martensite/austenite island exists
On picture, profile is not obvious.Although can be the good area of ferrite and M-A islands using LePera reagent etching pits technology
Separate, but the nuance in M-A islands can not be distinguished well.Technology proposed by the present invention, can not only area well
Ferrite, M-A islands in other granular bainite, and can be good at the martensite and austenite in M-A islands individually to differentiate
Come, such that it is able to effectively respectively quantitative analyses material property is had crucial effect martensite and retained austenite content and
Distribution situation.
2nd, the present invention is applied widely, and low-alloy nodular bainite steel can be less than 5wt.% for alloying element content
CrMo systems, NiCr systems, MnMoNi systems, SiMn systems, SiMnMo systems, CrMnSi systems, the low-alloy such as CrMnMo systems or CrNiMo systems
Bainitic steel, conventional alloy designations can be but be not limited to 2.25Cr1Mo-0.25V, G18CrMo2-6, SA508-3,
15CrMoVA, 18Cr2Ni4WA, 12CrNi3,35SiMnMo, 15SiMnVTi or 25SiMoVB etc..
3rd, present invention application is simple, experimental repeatability is good, analytical data reliability, relative to being set using modern advanced technology
It is standby, not only have good economy and avoid the loaded down with trivial details of sample preparation, no matter in scientific research or product development or have
Good economic and social benefit.
Description of the drawings
Fig. 1 is metallographic of 1 material of embodiment (2.25Cr-1Mo-0.25V steel is Jing normalizing+air cooling process) Jing after general corrosion
Figure.
Fig. 2 is that 1 material of embodiment (2.25Cr-1Mo-0.25V steel Jing normalizings+air cooling process) is corroded using Lepara reagents
Metallograph afterwards.
Fig. 3 is that 1 material of embodiment (2.25Cr-1Mo-0.25V steel Jing normalizings+air cooling process) is aoxidized using the inventive method
Metallograph after corrosion.
Fig. 4 is the spectrum for surveying residual austenite content before and after 1 metallographic specimen heat erosion of embodiment is incubated using XRD.
Fig. 5 is metallograph of 2 material of embodiment (G18CrMo2-6 steel is Jing normalizing+sand cooling process) Jing after general corrosion.
Fig. 6 is metallograph of 2 material of embodiment (G18CrMo2-6 steel is Jing normalizing+sand cooling process) Jing after the corrosion of LePera reagents.
After Fig. 7 is caustic solution of 2 material of embodiment (G18CrMo2-6 steel is Jing normalizing+sand cooling process) using the present invention
Metallograph.
Fig. 8 is metallograph of 3 material of embodiment (SA508-3 steel is Jing normalizing+air cooling process) Jing after general corrosion.
Fig. 9 is metallograph of 3 material of embodiment (SA508-3 steel is Jing normalizing+air cooling process) Jing after the corrosion of LePera reagents.
Figure 10 is the gold after caustic solution of 3 material of embodiment (SA508-3 steel is Jing normalizing+air cooling process) using the present invention
Phasor.
Specific embodiment
In a specific embodiment, the martensite in low-alloy nodular bainite steel of the present invention in martensite/austenite island
Classification with retained austenite shows and quantitative detecting method that its step is as follows：
(1), after intercept low-alloy nodular bainite steel steel sample to be measured, it is prepared into a certain size metallographic
Sample；
(2) metallographic specimen Jing grind, mechanically polish and electrobrightening after, the nitric acid ethanol first with 2～6wt% is molten
The light etch of liquid, etch time are 5～15 seconds, recycle ultrasound wave to clean sample.
(3) metallographic specimen after clean ultrasound wave is placed in 150～300 DEG C of stoves without atmosphere protection, insulation 2～6
Hour, it is placed in after coming out of the stove in exsiccator, is cooled to room temperature in atmosphere；
(4) in the tissue of metallography microscope Microscopic observation low-alloy nodular bainite steel：Polygonal ferrite and bainite ferrum
Ferritic is in bluish violet, and martensite is in brown, and retained austenite is in ecru；
(5) to respectively mutually carrying out quantitative analyses in tissue.
In order to embody the comprehensive information reliable, simple, economic and that metallographic structure can be obtained of the inventive method well.
In follow-up specific embodiment, other two kinds of method of contrast that the present invention is enumerated, for illustrate the present invention have other two
The superiority for characterizing metallographic structure method is planted, but the two kinds of method of contrast for adopting are not meant to be limited by protection of the present invention.
In order to confirm that the present invention has wider range of application, and in view of the feasibility of practical operation, present invention choosing
Select in three kinds of typical low-alloy nodular bainite steels as case study on implementation, respectively 2.25Cr-1Mo-0.25V steel,
G18CrMo2-6 steel and SA508-3 steel.
Embodiment 1
1st, prepared by sample
A () the present embodiment prepares metallographic specimen, sample generally 10 × 10 using 2.25Cr-1Mo-0.25V steel normalizing states
The square of × 10mm or 8 × 8 × 8mm orCylinder.For sample size does not have specific requirement, but select
The sample should be representative.
B () grinds sample and is roughly ground on metallographic specimen Plane surface grinding machine, on Automatic Grinding Prototype respectively with 150#, 400#,
Refine on 800#, 1200#, 2000# abrasive paper for metallograph, obvious cut is not seen in perusal, be that subsequent mechanical polishing is prepared.
C () mechanically polishes.Polishing rotating speed is advisable in 250～350r/min, adopts polishing grinding cream for W2.5 (1.5 μm～2.5
μm) the diamond polishing cream of granularity, the smooth minute surface having no time of specimen surface examine under a microscope without tiny cut after polishing.
(d) electrobrightening.For the reliability of experiment, prevent in grind away process as stress causes retained austenite point
Solution, all ground samples of the present invention all increase by one electrobrightening operation.Electrolytic polishing process is：Voltage 50V, electric current
5mA, -20 DEG C～-30 DEG C of electrolysis temperature；Polishing fluid：The perchloric acid alcoholic solution of 8wt%, 12wt% distilled water and 80wt%
Dehydrated alcohol, polishing time is advisable in 30s～60s.
2nd, the pre-etching of sample
Sample concentration is the 8～15s of nital pre-etching time of 4wt%, with washes of absolute alcohol simultaneously immediately
Dried up with hot hair dryer, pre-etching should not be too deep, otherwise after heated oxide, organize too dark, the sample after pre-etching is to metallography microscope
Microscopic observation can be seen tissue clearly and be advisable than more visible.
3rd, oven heat oxide etch
The good sample of pre-etching is placed in into the calorstat without atmosphere protection with quartzy culture dish, Thermostat Temperature Control is existed
180～240 DEG C or so, temperature retention time is determined according to the color change situation of specimen surface after oxidation.Prolonging with temperature retention time
It is long, specimen surface can take out from calorstat typically by greyish white-orange-royal purple color change, when sample is in bluish violet be placed in it is dry
In dry device, room temperature is cooled in atmosphere.According to the film forming thickness principle that can produce preferable interference effect, film forming thickness is general
In 300～600 angstroms of scopes, temperature retention time is that 2～4 hours corrosive effects are optimal to the present embodiment under this condition for control.
4th, the observation of microscopic structure and image acquisition
(a) due in granular bainite microstructure in the embodiment of the present invention M-A islands it is all relatively fine, for preferably quantitative point
Martensite and retained austenite in analysis M-A islands, metallurgical microscope is using laser co-focusing (display effect and simple microscope one
Cause) observation, when observation using 20 ×, 50 ×, 100 ×, 200 × objective lens；
B () switches on power, select white light source, adjusts suitable aperture and field stop, and random selection 5～10 is different
Visual field, each visual field clap the clear metallograph of 1000,2000 amplifications respectively, and typical metallograph is as shown in Figure 3.
In order to contrast the characteristics of showing the present invention, the metallographic of same sample after using general corrosion method and the corrosion of LePera reagents
Figure is respectively as depicted in figs. 1 and 2.
5th, the metallograph tissue identification of phases and quantitative analyses
Using Analy SIS quantitative analysis softwares to respectively mutually carrying out quantitative analyses in tissue；Extract phase character：Granular shellfish
Family name's body matrix or polygonal ferrite display bluish violet, martensite are in brown, retained austenite is ecru, and it is fixed that image is carried out
Amount analysis, measures M-A islands mean intercept for 2.4 μm, and wherein in M-A islands, martensite content is 7.5wt%, residual austenite content
For 4.8wt%, (as the density contrast of each phase is less, approximate thinks that volume fraction is equal with mass fraction, is easy to measure with XRD
Value contrast), 0.12/μm of density on M-A islands2.Metallographic statistical result using present invention corrosion is rotten with using LePera reagents
Erosion metallographic statistics, XRD survey remained austenite content contrast as shown in table 1, and the result of test is fine with what other method of testings were coincide.
Table 1 is using different method of testings to geneva in the 2.25Cr-1Mo-0.25V nodular bainite steel M-A islands of embodiment 1
Body and the Statistical Comparison of retained austenite.
Remained austenite content in the forward and backward tissue of oxide etch is measured with XRD to be basically unchanged, measurement data such as table 1 and Fig. 4
It is shown, the better heat stability of the low-alloy nodular bainite steel below 260 DEG C is illustrated, oxidation processes are not resulted in material
The decomposition of retained austenite.
Embodiment 2
The present embodiment is G18CrMo2-6 steel using material, and, Jing after normalizing+sand cooling process, microscopic structure is mainly by grain for sample
Shape bainite and a small amount of acicular ferrite are constituted.The sample making course of the present embodiment is the same with the method for embodiment 1, but due to this reality
Apply a material corrosion resistance poor, 2wt% nital 5～10s of etching time are adopted in pre-etching, while constant temperature oxygen
Change temperature be adjusted to 160～180 DEG C, temperature retention time be 4～6 hours.
Fig. 5 is metallograph of the present embodiment material Jing after general corrosion, and Fig. 6 is that the present embodiment material Jing LePera reagents are rotten
Metallograph after erosion, Fig. 7 are the metallograph after the caustic solution of the present embodiment materials'use present invention.
As can be seen that general corrosion can only partly differentiate the micro-structural feature of the present embodiment material from above-mentioned three figure,
M-A cannot be differentiated；The present embodiment material Zhong M-A islands can be gone out respectively after the corrosion of LePera caustic, but M-A cannot be gone out respectively
Martensite and retained austenite in island；Martensite and austenite in Neng Jiang M-A islands of the present invention shown in different color,
It is capable of achieving quantitative analyses and statistics to above two tissue.
Embodiment 3
The present embodiment is SA508-3 steel using material, and, Jing after normalizing+air cooling process, microscopic structure is mainly by granular for sample
Bainite is constituted.The sample making course of the present embodiment is the same with 1 method of embodiment, and 5wt% nitals are adopted during pre-etching
5～8s of etching time, constant temperature oxidation film-forming temperature are adjusted to 240～280 DEG C, and temperature retention time is 2～4 hours.
Fig. 8 is metallograph of the present embodiment material Jing after general corrosion, and Fig. 9 is that the present embodiment material Jing LePera reagents are rotten
Metallograph after erosion, Figure 10 are the metallograph after the caustic solution of the present embodiment materials'use present invention.
As can be seen that general corrosion can only partly differentiate the micro-structural feature of the present embodiment material from above-mentioned three figure,
M-A cannot be differentiated；The present embodiment material Zhong M-A islands can be gone out respectively after the corrosion of LePera caustic, but M-A cannot be gone out respectively
Martensite and retained austenite in island；Martensite and austenite in Neng Jiang M-A islands of the present invention shown in different color,
It is capable of achieving quantitative analyses and statistics to above two tissue.
Embodiment result shows that microstructure classification in ferrous materials of the present invention shows the method with quantitative measurement, as far as possible
Microstructure characteristics are carried out comprehensively to characterize as far as possible using better simply means, only combined by conventional etching pit technology
Low-temperature oxidation developing technology, the identification and detection by quantitative for the microstructure in such steel provide guarantee, further promote product
Research and development exploitation, achieves significant economic benefit and social benefit.
Claims (7)
1. in a kind of M-A islands, the classification of martensite and retained austenite shows and quantitative detecting method, it is characterised in that its step
It is as follows：
(1) low-alloy nodular bainite steel test block to be detected is intercepted by sampling standard, using grinding, prepared by mechanical polishing mode
Metallographic specimen；
(2) metallographic specimen Surface stress layer is removed with electrolytic polishing method, then the nitric acid ethanol using 2wt%～6wt% is molten
Sample after pre-etching is finally put into ultrasound wave cleaning used in dehydrated alcohol by liquid pre-etching 5～15 seconds；
(3) metallographic specimen after clean ultrasound wave is placed in 150～300 DEG C without in atmosphere protection stove, is incubated 2～6 hours, goes out
Furnace rear is placed in exsiccator, is cooled to room temperature in atmosphere；
(4) in the tissue of metallography microscope Microscopic observation low-alloy nodular bainite steel：Polygonal ferrite and bainite ferrite
In bluish violet, martensite is in brown, and retained austenite is in ecru；
(5) using quantitative analysis software to respectively mutually being observed and quantitative analyses in tissue；
Using grinding, mechanical polishing mode is prepared after metallographic specimen, is needed using dehydrated alcohol-perchloric acid-distilled water solution pair
Sample carries out electrobrightening, to eliminate the decomposition that stress in sample making course causes retained austenite；Electrolytic polishing process is：Voltage
40～60V, 4～6mA of electric current, -20 DEG C～-30 DEG C of electrolysis temperature；Polishing fluid：The perchloric acid alcoholic solution of 5～10wt%, 10～
The dehydrated alcohol of 15wt% distilled water and 75～85wt%, polishing time is in 30s～60s；
Using the nital pre-etching 5～15 seconds of 2wt%～6wt%, tissue can be slightly seen under metallurgical microscope clearly
, the sample after pre-etching is put into into ultrasound wave used in dehydrated alcohol then and is cleaned 10～20 minutes, remove corrosion product；
With the prolongation of temperature retention time, specimen surface, can be from constant temperature when sample is in bluish violet by greyish white-orange-royal purple color change
Take out in case and be placed in exsiccator, be cooled to room temperature in atmosphere；It is former according to the film forming thickness that can produce preferable interference effect
Reason, film forming thickness are controlled in 300～600 angstroms of scopes.
2. show and quantitative detecting method according to the classification of martensite and retained austenite in the M-A islands described in claim 1, its
It is characterised by, the metallographic specimen after ultrasound wave is cleaned is placed in 150～260 DEG C without the sub- inside holding of atmosphere protection stove 2～6 hours,
Observation surface blueing color under perusal is made to be advisable.
3. show and quantitative detecting method according to the classification of martensite and retained austenite in the M-A islands described in claim 1, its
It is characterised by, in metallography microscope Microscopic observation, various phases, polygonal ferrite and bayesian in tissue is differentiated by color contrast
Body ferrite is in bluish violet, and martensite is in brown, and retained austenite is in ecru, differentiates each phase by color distinction and carries out determining
Amount analysis.
4. show and quantitative detecting method according to the classification of martensite and retained austenite in the M-A islands described in claim 1, its
It is characterised by, in low-alloy steel, main alloying element content is less than 5wt.%, and material microstructure is based on granular bainite.
5. show and quantitative detecting method according to the classification of martensite and retained austenite in the M-A islands described in claim 1, its
It is characterised by, low-alloy nodular bainite steel is alloying element content less than the CrMo systems of 5wt.%, NiCr systems, MnMoNi
System, SiMn systems, SiMnMo systems, CrMnSi systems, CrMnMo systems or CrNiMo systems.
6. show and quantitative detecting method according to the classification of martensite and retained austenite in the M-A islands described in claim 1, its
Be characterised by, grind sample and roughly ground on metallographic specimen Plane surface grinding machine, on Automatic Grinding Prototype respectively with 150#, 400#, 800#,
Refine on 1200#, 2000# abrasive paper for metallograph, obvious cut is not seen in perusal, be that subsequent mechanical polishing is prepared.
7. show and quantitative detecting method according to the classification of martensite and retained austenite in the M-A islands described in claim 1, its
Be characterised by, mechanical polishing rotating speed in 250～350r/min, adopt polishing grinding cream for W2.5 granularities diamond polishing cream,
The smooth minute surface having no time of specimen surface examine under a microscope without tiny cut after polishing.
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