CN104111230A - 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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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 for air cooling 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 in ferrous materials shows and quantitative measurement technology, belong to classification demonstration and the quantitative detecting method of the middle martensite of field of iron and steel, particularly a kind of low-alloy nodular bainite steel martensite/austenite island (M-A island) and retained austenite.
Background technology
Low-alloy nodular bainite steel is owing to having better obdurability, excellent anti-hydrogen embrittlement performance and suitable Properties of High Temperature Creep, be widely used and large-scale hydrogenation reactor, nuclear power cylinder body and some have certain requirements on parts to the strength of materials and resistance to elevated temperatures.But along with the continuous expansion of hydrogenation plant scale and the continuous increase of nuclear power power, hydrogenation reactor wall thickness and nuclear pressure container wall thickness significantly increase.Therefore, in actual heat treatment process due to the restriction of cooling rate, easily obtain granular bainite or grain structure, the content on the martensite/austenite island (M-A island) in this granular bainite, pattern, size, distribution produce material impact, particularly low temperature impact properties to the mechanical property of steel.Therefore, accurately observe, differentiate granular bainite or grain structure Zhong M-A island, and martensite and retained austenite in M-A island, the material of performance optimize to(for) the microstructure of understanding material is very important.Adopt quantitative metallographic analysis technology to be the difficult point of nodular bainite steel fabric analysis: the identification to feature organization and extraction, use traditional etching pit method, can only obtain the gray level image of microstructure, between each phase, due to contrast, obvious being difficult to distinguished not.And utilize current colour metallograpy corrosion technology, and be also difficult to distinguish martensite and the retained austenite in M-A island, thereby cause part material particular in the time of fabric analysis to be left in the basket, be unfavorable for the quantitative test of feature organization.
Chinese patent application (publication number CN101382494A, open day 2009-3-11, applicant: Wuhan Iron & Steel (Group) Corp.), retained austenite or island martensite body-austenitic demonstration and quantitative detecting method in a kind of TRIP steel are proposed, main contents are by traditional colour metallograpy corrosion technology, use LePara reagent (Sodium Metabisulfite solution and picral mix by a certain percentage) to corrode the tissue after polishing, to the polygonal ferrite in tissue, quantitative metallography corrosion is carried out on bainite ferrite and M-A island, but use sample prepared by this caustic solution under metaloscope, martensite and retained austenite in M-A island are all white in color, be difficult on metallographic the further quantitative statistics to both.
Along with the development of research means, although there are at present some means can characterize the remained austenite content (as: utilizing method of magnetic measurement or XRD to measure the remained austenite content in tissue) in clear tissue, but above-mentioned means are process of the test complexity not only, and can not observe more intuitively the integrated information of the amount on material structure Zhong M-A island, distribution, size.And under scanning electron microscope, use electron backscattered technology (EBSD) can differentiate martensite and the austenite in M-A island, also can observe regional area M-A island distributes simultaneously, but because the martensite in M-A island is identical with matrix bainite ferrite structure, martensite and bainite ferrite in indistinguishable M-A island.What is more important, the sample preparation of EBSD technology and observation process complexity, limited its widespread use.
Summary of the invention
In order to overcome the deficiency of above-mentioned technology, the object of the present invention is to provide classification demonstration and the quantitative detecting method of the middle martensite in a kind of low-alloy nodular bainite steel martensite/austenite island (M-A island) and retained austenite, the method is obviously to distinguish the simple high efficiency method of martensite and retained austenite in M-A island, is convenient in scientific research and research and development of products, the Identification and determination of nodular bainite steel ZhongM-A island microstructure be detected.
Technical scheme of the present invention is:
Classification demonstration and the quantitative detecting method of martensite and retained austenite in M-A island, its step is as follows:
(1) intercept low-alloy nodular bainite steel test block to be detected by sampling standard, use grinds, mechanical buffing mode is prepared metallographic specimen;
(2) remove metallographic specimen Surface stress layer with electrolytic polishing method, then use the nital pre-etching 5~15 seconds of 2wt%~6wt%, finally the sample after pre-etching is put into absolute ethyl alcohol and use Ultrasonic Cleaning;
(3) metallographic specimen after Ultrasonic Cleaning is placed in to 150~300 DEG C without in atmosphere protection stove, is incubated 2~6 hours, come out of the stove and be placed on exsiccator hollow cold to room temperature;
(4) at the tissue of metallography microscope Microscopic observation low-alloy nodular bainite steel: polygonal ferrite and bainite ferrite are bluish violet, and it is brown that martensite is, and retained austenite is ecru;
(5) utilize quantitative analysis software to respectively observing mutually and quantitative test in tissue.
Classification demonstration and the quantitative detecting method of martensite and retained austenite in described M-A island, use grinds, mechanical buffing mode is prepared after metallographic specimen, need to use absolute ethyl alcohol-perchloric acid-distilled water solution to carry out electropolishing to sample, cause the decomposition of retained austenite to eliminate stress in sample making course; Electrolytic polishing process is: voltage 40~60V, electric current 4~6mA, electrolysis temperature-20 DEG C~-30 DEG C; The absolute ethyl alcohol of perchloric acid alcoholic solution, 10~15wt% distilled water and the 75~85wt% of polishing fluid: 5~10wt%, polishing time is at 30s~60s.
Classification demonstration and the quantitative detecting method of martensite and retained austenite in described M-A island, the nital pre-etching of use 2wt%~6wt% 5~15 seconds, under metaloscope, can slightly see tissue clearly, then the sample after pre-etching is put into absolute ethyl alcohol and used Ultrasonic Cleaning 10~20 minutes, remove corrosion product.
Classification demonstration and the quantitative detecting method of martensite and retained austenite in described M-A island, be placed in 150~260 DEG C without being incubated 2~6 hours in atmosphere protection stove by the metallographic specimen after Ultrasonic Cleaning, makes to observe surface blueing look under visual inspection and be advisable.
Classification demonstration and the quantitative detecting method of martensite and retained austenite in described M-A island, at metallography microscope Microscopic observation, differentiate various phases in tissue by color contrast, polygonal ferrite and bainite ferrite are bluish violet, it is brown that martensite is, retained austenite is ecru, is differentiated each phase and is carried out quantitative test by color distinction.
Classification demonstration and the quantitative detecting method of martensite and retained austenite in described M-A island, in low alloy steel, main alloying element content is no more than 5wt.%, and material microstructure is taking granular bainite as main.
Classification demonstration and the quantitative detecting method of martensite and retained austenite in described M-A island, low-alloy nodular bainite steel is CrMo system, NiCr system, MnMoNi system, SiMn system, SiMnMo system, CrMnSi system, CrMnMo system or the CrNiMo system that alloying element content is no more than 5wt.%.
Classification demonstration and the quantitative detecting method of martensite and retained austenite in described M-A island, grind sample roughly grinds on metallographic specimen Plane surface grinding machine, on Automatic Grinding Prototype respectively with refining on 150#, 400#, 800#, 1200#, 2000# abrasive paper for metallograph, obvious cut is not seen in visual inspection, for follow-up mechanical buffing is prepared.
Classification demonstration and the quantitative detecting method of martensite and retained austenite in described M-A island, mechanical buffing rotating speed is at 250~350r/min, adopting polishing abrasive pastes is the diamond polishing cream of W2.5 granularity, the smooth minute surface of having no time of specimen surface examining under a microscope without tiny cut after polishing.
Classification demonstration and the quantitative detecting method of martensite and retained austenite in described M-A island, with the prolongation of temperature retention time, specimen surface is changed by greyish white-orange-bluish violet, in the time that sample is bluish violet, can from constant temperature oven, takes out and be placed in exsiccator hollow cold to room temperature; According to the film forming thickness principle that can produce good interference effect, film forming thickness is controlled at 300~600 dust scopes.
Ultimate principle of the present invention is as follows:
Prepare after the metallographic specimen of sample to be detected in use conventional method, need to first carry out electropolishing processing to sample, this be because sample ZhongM-A island in retained austenite likely grind with polishing sample process in there is the decomposition that stress/strain causes, thereby can have a negative impact to the precision of testing result.And electropolishing process can be got rid of affected stressor layers, do not produce new stress simultaneously.
After electropolishing, sample need to gently corrode in the nital of 2~6wt%, the Main Function of light corrosion has two, the one, due to the resistance to corrosion difference of each phase in material, after corrosion, produce rugged pattern at material surface, thereby present different patterns under metaloscope; The 2nd, the tissue after light corrosion can produce different oxidation products, thereby under metaloscope, present different color and lusters in follow-up oxidizing process.
After light corrosion, need to use ultrasound wave that the corrosion product that is attached to specimen surface after corrosion is removed, avoid follow-up oxidizing process to have a negative impact.
Sample after gently corroding is placed on to the fundamental purpose being oxidized in 150~300 DEG C of stoves without atmosphere protection is: the microstructure after gently corroding is carried out to heat-tinting; be organized in because different and in light corrosion process, produce different corrosion products; and different corrosion products presents different color and lusters after oxidation, thereby reach the object of differentiating different tissues.The temperature of oxidation can not be too high, to avoid causing retained austenite in M-A island to decompose, affects measuring accuracy.According to the decomposition temperature of low-alloy nodular bainite steel retained austenite, determine that highest oxidation temperature is 300 DEG C.
Advantage of the present invention and beneficial effect are:
1, the sample that uses common etching pit method to prepare can only be seen ferrite clearly, and martensite/austenite island profile not obvious on picture.Although adopt LePera reagent etching pit technology ferrite HeM-A island well can be made a distinction, can not well distinguish the nuance in M-A island.The technology that the present invention proposes, not only can well distinguish ferrite in granular bainite, M-A island, and can be good at martensite in BaM-A island and austenite separately difference come, thereby quantitative test has the martensite of crucial impact and content and the distribution situation of retained austenite to material property effectively respectively.
2, the present invention is applied widely, low-alloy nodular bainite steel can be no more than for alloying element content the low-alloy bainite steel such as CrMo system, NiCr system, MnMoNi system, SiMn system, SiMnMo system, CrMnSi system, CrMnMo system or CrNiMo system of 5wt.%, and 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.
3, the present invention applies simply, experimental repeatability is good, it is reliable to analyze data, with respect to using modern advanced technology resource, no matter the not only good economy of tool and avoid the loaded down with trivial details of sample preparation, still have good economic and social benefit in the time of scientific research or product development.
Brief description of the drawings
Fig. 1 is the metallograph of embodiment 1 material (2.25Cr-1Mo-0.25V steel is through the processing of normalizing+air cooling) after general corrosion.
Fig. 2 is that embodiment 1 material (2.25Cr-1Mo-0.25V steel is through the processing of normalizing+air cooling) adopts the metallograph after the corrosion of Lepara reagent.
Fig. 3 is that embodiment 1 material (2.25Cr-1Mo-0.25V steel is through the processing of normalizing+air cooling) adopts the metallograph after the inventive method oxidation corrosion.
Fig. 4 utilizes XRD to survey the spectrum of residual austenite content before and after embodiment 1 metallographic specimen hot corrosion insulation.
Fig. 5 is the metallographs of embodiment 2 materials (G18CrMo2-6 steel is through the processing of normalizing+sand cooling) after general corrosion.
Fig. 6 is the metallographs of embodiment 2 materials (G18CrMo2-6 steel is through the processing of normalizing+sand cooling) after the corrosion of LePera reagent.
Fig. 7 is that embodiment 2 materials (G18CrMo2-6 steel is through the processing of normalizing+sand cooling) use the metallograph after caustic solution of the present invention.
Fig. 8 is the metallographs of embodiment 3 materials (SA508-3 steel is through the processing of normalizing+air cooling) after general corrosion.
Fig. 9 is the metallographs of embodiment 3 materials (SA508-3 steel is through the processing of normalizing+air cooling) after the corrosion of LePera reagent.
Figure 10 is that embodiment 3 materials (SA508-3 steel is through the processing of normalizing+air cooling) use the metallograph after caustic solution of the present invention.
Embodiment
In embodiment, the martensite in low-alloy nodular bainite steel of the present invention in martensite/austenite island and classification demonstration and the quantitative detecting method of retained austenite, its step is as follows:
(1) press sampling standard by after low-alloy nodular bainite steel steel sample intercepting to be measured, be prepared into a certain size metallographic specimen;
(2) described metallographic specimen, through grinding, after mechanical buffing and electropolishing, is first used the light etch of nital of 2~6wt%, and the etch time is 5~15 seconds, and recycling ultrasound wave cleans sample.
(3) metallographic specimen after Ultrasonic Cleaning is placed in 150~300 DEG C of stoves without atmosphere protection, is incubated 2~6 hours, come out of the stove and be placed on exsiccator hollow cold to room temperature;
(4) at the tissue of metallography microscope Microscopic observation low-alloy nodular bainite steel: polygonal ferrite and bainite ferrite are bluish violet, and it is brown that martensite is, and retained austenite is ecru;
(5) to respectively carrying out mutually quantitative test in tissue.
In order well to embody reliable, simple, the economic comprehensive information that also can obtain metallographic structure of the inventive method.In follow-up specific embodiment, other two kinds of method of contrast that the present invention enumerates, are used for illustrating that the present invention has other the two kinds superiority that characterize metallographic structure methods, but two kinds of method of contrast that adopt do not mean that and be subject to the present invention to protect restriction.
For proved invention has wider range of application, and consider the feasibility of practical operation, the present invention is chosen in three kinds of typical low-alloy nodular bainite steels as case study on implementation, is respectively 2.25Cr-1Mo-0.25V steel, G18CrMo2-6 steel and SA508-3 steel.
Embodiment 1
1, sample preparation
(a) the present embodiment adopts 2.25Cr-1Mo-0.25V steel normalizing state to prepare metallographic specimen, sample be generally 10 × 10 × 10mm or 8 × 8 × 8mm square or
right cylinder.There is no specific requirement for sample size, but select this sample should be representative.
(b) grind sample and roughly grind on metallographic specimen Plane surface grinding machine, on Automatic Grinding Prototype, respectively with refining on 150#, 400#, 800#, 1200#, 2000# abrasive paper for metallograph, obvious cut is not seen in visual inspection, for follow-up mechanical buffing is prepared.
(c) mechanical buffing.Polishing rotating speed is advisable at 250~350r/min, and adopting polishing abrasive pastes is W2.5 (m) the diamond polishing cream of granularity of 1.5 μ m~2.5 μ, the smooth minute surface of having no time of specimen surface examining under a microscope without tiny cut after polishing.
(d) electropolishing.For the reliability of testing, prevent from decomposing because stress causes retained austenite in grind away process, all ground samples of the present invention all increase electropolishing operation one.Electrolytic polishing process is: voltage 50V, electric current 5mA, electrolysis temperature-20 DEG C~-30 DEG C; The absolute ethyl alcohol of perchloric acid alcoholic solution, 12wt% distilled water and the 80wt% of polishing fluid: 8wt%, polishing time is advisable at 30s~60s.
2, the pre-etching of sample
Nital pre-etching time 8~15s that sample is 4wt% by concentration, clean with absolute ethyl alcohol immediately and dry up with hot hair dryer, pre-etching is too not dark, otherwise after heated oxide, organize too dark, the sample after pre-etching to metallography microscope Microscopic observation can more clearly see clearly be organized as suitable.
3, constant temperature oven heated oxide corrosion
The good sample of pre-etching is placed in to the constant temperature oven without atmosphere protection with quartzy double dish, Thermostat Temperature Control, 180~240 DEG C of left and right, temperature retention time decides according to the change color situation of specimen surface after oxidation.With the prolongation of temperature retention time, specimen surface is generally changed by greyish white-orange-bluish violet, in the time that sample is bluish violet, can from constant temperature oven, takes out and be placed in exsiccator hollow cold to room temperature.According to the film forming thickness principle that can produce good interference effect, film forming thickness general control is in 300~600 dust scopes, and the present embodiment temperature retention time under this condition is 2~4 hours corrosive effect the bests.
4, the observation of microstructure and image acquisition
(a) because granular bainite microstructure ZhongM-A island in the embodiment of the present invention is all more tiny, for martensite and retained austenite in better quantitative test M-A island, metaloscope adopts laser co-focusing (display effect is consistent with simple microscope) observation, when observation, use 20 ×, 50 ×, 100 ×, 200 × objective lens;
(b) switch on power, select white light source, regulate suitable aperture and field stop, select at random 5~10 different visual fields, one 1000, the clear metallograph of 2000 enlargement factors are clapped respectively in each visual field, and typical metallograph as shown in Figure 3.In order to contrast the feature of the present invention that shows, the metallograph of same sample after use general corrosion method and the corrosion of LePera reagent respectively as depicted in figs. 1 and 2.
5, metallograph is organized the identification of phases and quantitative test
Utilize Analy SIS quantitative analysis software to respectively carrying out mutually quantitative test in tissue; Extract phase character: granular bainite matrix or polygonal ferrite show that it is ecru that bluish violet, martensite are brown, retained austenite, image is carried out to quantitative test, recording M-A island mean intercept is 2.4 μ m, wherein in M-A island, martensite content is that 7.5wt%, residual austenite content are that 4.8wt% is (because the density difference of each phase is less, the approximate volume fraction of thinking equates with massfraction, be convenient to and the contrast of XRD measured value), 0.12/μ of the density m on M-A island
2.The metallographic statistics that adopts the present invention corrosion with adopt LePera reagent corrosion metallographic statistics, that XRD surveys remained austenite content contrast is as shown in table 1, identical fine of the result of test and other method of testings.
Table 1 uses the Statistical Comparison of different method of testings to martensite and retained austenite in the 2.25Cr-1Mo-0.25V nodular bainite steel M-A island of embodiment 1.
Measure in the forward and backward tissue of oxidation corrosion remained austenite content with XRD substantially constant, measurement data is as shown in table 1 and Fig. 4, the better heat stability of low-alloy nodular bainite steel below 260 DEG C is described, oxidation processes can not cause the decomposition of the retained austenite in material.
Embodiment 2
It is G18CrMo2-6 steel that the present embodiment uses material, and sample is after normalizing+sand cooling is processed, and microstructure is mainly made up of granular bainite and a small amount of acicular ferrite.The sample making course of the present embodiment is the same with the method for embodiment 1, but because the present embodiment material corrosion resistance is poor, in the time of pre-etching, adopt 2wt% nital etching time 5~10s, to be simultaneously adjusted into 160~180 DEG C, temperature retention time be 4~6 hours to constant temperature oxidizing temperature.
Fig. 5 is the metallograph of the present embodiment material after general corrosion, and Fig. 6 is the metallograph of the present embodiment material after the corrosion of LePera reagent, and Fig. 7 is the metallograph after the present embodiment materials'use caustic solution of the present invention.
From above-mentioned three figure, can find out, general corrosion can only partly be differentiated the micro-structural feature of the present embodiment material, cannot differentiate M-A; After the corrosion of LePera mordant, the present embodiment material Zhong M-A island can be gone out respectively, but cannot distinguish martensite and the retained austenite in ChuM-A island; Martensite in Neng Jiang M-A of the present invention island and austenite are different color and show, and can realize quantitative test and statistics to above-mentioned two kinds of tissues.
Embodiment 3
It is SA508-3 steel that the present embodiment uses material, and sample is after normalizing+air cooling is processed, and microstructure is mainly made up of granular bainite.The sample making course of the present embodiment is the same with embodiment 1 method, adopts 5wt% nital etching time 5~8s when pre-etching, and constant temperature oxidation filming temperature is adjusted into 240~280 DEG C, and temperature retention time is 2~4 hours.
Fig. 8 is the metallograph of the present embodiment material after general corrosion, and Fig. 9 is the metallograph of the present embodiment material after the corrosion of LePera reagent, and Figure 10 is the metallograph after the present embodiment materials'use caustic solution of the present invention.
From above-mentioned three figure, can find out, general corrosion can only partly be differentiated the micro-structural feature of the present embodiment material, cannot differentiate M-A; After the corrosion of LePera mordant, the present embodiment material Zhong M-A island can be gone out respectively, but cannot distinguish martensite and the retained austenite in ChuM-A island; Martensite in Neng Jiang M-A of the present invention island and austenite are different color and show, and can realize quantitative test and statistics to above-mentioned two kinds of tissues.
Embodiment result shows, the method of microstructure classification demonstration and quantitative measurment in ferrous materials of the present invention, adopt better simply means as far as possible comprehensively to characterize Microstructure characteristics as far as possible, only by commonly using etching pit technology in conjunction with low-temperature oxidation developing technology, for identification and quantitative detection of the microstructure in such steel provide guarantee, also promote research and development of products exploitation, obtained significant economic benefit and social benefit.
Claims (10)
1. classification demonstration and the quantitative detecting method of martensite and retained austenite in Yi Zhong M-A island, is characterized in that, its step is as follows:
(1) intercept low-alloy nodular bainite steel test block to be detected by sampling standard, use grinds, mechanical buffing mode is prepared metallographic specimen;
(2) remove metallographic specimen Surface stress layer with electrolytic polishing method, then use the nital pre-etching 5~15 seconds of 2wt%~6wt%, finally the sample after pre-etching is put into absolute ethyl alcohol and use Ultrasonic Cleaning;
(3) metallographic specimen after Ultrasonic Cleaning is placed in to 150~300 DEG C without in atmosphere protection stove, is incubated 2~6 hours, come out of the stove and be placed on exsiccator hollow cold to room temperature;
(4) at the tissue of metallography microscope Microscopic observation low-alloy nodular bainite steel: polygonal ferrite and bainite ferrite are bluish violet, and it is brown that martensite is, and retained austenite is ecru;
(5) utilize quantitative analysis software to respectively observing mutually and quantitative test in tissue.
2. according to classification demonstration and the quantitative detecting method of martensite and retained austenite in M-A claimed in claim 1 island, it is characterized in that, use grinds, mechanical buffing mode is prepared after metallographic specimen, need to use absolute ethyl alcohol-perchloric acid-distilled water solution to carry out electropolishing to sample, cause the decomposition of retained austenite to eliminate stress in sample making course; Electrolytic polishing process is: voltage 40~60V, electric current 4~6mA, electrolysis temperature-20 DEG C~-30 DEG C; The absolute ethyl alcohol of perchloric acid alcoholic solution, 10~15wt% distilled water and the 75~85wt% of polishing fluid: 5~10wt%, polishing time is at 30s~60s.
3. according to classification demonstration and the quantitative detecting method of martensite and retained austenite in M-A claimed in claim 1 island, it is characterized in that, the nital pre-etching of use 2wt%~6wt% 5~15 seconds, under metaloscope, can slightly see tissue clearly, then the sample after pre-etching is put into absolute ethyl alcohol and used Ultrasonic Cleaning 10~20 minutes, remove corrosion product.
4. according to classification demonstration and the quantitative detecting method of martensite and retained austenite in M-A claimed in claim 1 island; it is characterized in that; metallographic specimen after Ultrasonic Cleaning is placed in to 150~260 DEG C without being incubated 2~6 hours in atmosphere protection stove, makes to observe surface blueing look under visual inspection and be advisable.
5. according to classification demonstration and the quantitative detecting method of martensite and retained austenite in M-A claimed in claim 1 island, it is characterized in that, at metallography microscope Microscopic observation, differentiate various phases in tissue by color contrast, polygonal ferrite and bainite ferrite are bluish violet, it is brown that martensite is, and retained austenite is ecru, differentiated each phase and carried out quantitative test by color distinction.
6. according to classification demonstration and the quantitative detecting method of martensite and retained austenite in M-A claimed in claim 1 island, it is characterized in that, in low alloy steel, main alloying element content is no more than 5wt.%, and material microstructure is taking granular bainite as main.
7. according to classification demonstration and the quantitative detecting method of martensite and retained austenite in M-A claimed in claim 1 island, it is characterized in that, low-alloy nodular bainite steel is CrMo system, NiCr system, MnMoNi system, SiMn system, SiMnMo system, CrMnSi system, CrMnMo system or the CrNiMo system that alloying element content is no more than 5wt.%.
8. according to classification demonstration and the quantitative detecting method of martensite and retained austenite in M-A claimed in claim 1 island, it is characterized in that, grind sample roughly grinds on metallographic specimen Plane surface grinding machine, on Automatic Grinding Prototype respectively with refining on 150#, 400#, 800#, 1200#, 2000# abrasive paper for metallograph, obvious cut is not seen in visual inspection, for follow-up mechanical buffing is prepared.
9. according to classification demonstration and the quantitative detecting method of martensite and retained austenite in M-A claimed in claim 1 island, it is characterized in that, mechanical buffing rotating speed is at 250~350r/min, adopting polishing abrasive pastes is the diamond polishing cream of W2.5 granularity, the smooth minute surface of having no time of specimen surface examining under a microscope without tiny cut after polishing.
10. according to classification demonstration and the quantitative detecting method of martensite and retained austenite in M-A claimed in claim 1 island, it is characterized in that, with the prolongation of temperature retention time, specimen surface is changed by greyish white-orange-bluish violet, in the time that sample is bluish violet, can from constant temperature oven, takes out and be placed in exsiccator hollow cold to room temperature; According to the film forming thickness principle that can produce good interference effect, film forming thickness is controlled at 300~600 dust scopes.
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CN114855167A (en) * | 2022-04-15 | 2022-08-05 | 包头钢铁(集团)有限责任公司 | Corrosive agent for displaying microstructure of low-carbon copper-containing steel quenching sample and corrosion display method thereof |
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-
2014
- 2014-06-19 CN CN201410284069.1A patent/CN104111230B/en active Active
Non-Patent Citations (6)
Title |
---|
B.V.KOVACS: "On the Terminology and Structure of ADI", 《AFS TRANSACTIONS》 * |
On the Terminology and Structure of ADI;B.V.Kovacs;《AFS Transactions》;19941231;417-420 * |
下贝氏体一马氏体耐磨钢的研制;司鹏程;《金属热处理》;19941231(第8期);全文 * |
司鹏程: "下贝氏体一马氏体耐磨钢的研制", 《金属热处理》 * |
热轧TRIP钢残余奥氏体及其稳定性研究;高绪涛等;《材料工程》;20111231(第11期);参见第40页左栏第2段 * |
高绪涛等: "热轧TRIP钢残余奥氏体及其稳定性研究", 《材料工程》 * |
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