CN103389304B - The area fraction assessment method of M/A island tissue in a kind of pipe line steel - Google Patents
The area fraction assessment method of M/A island tissue in a kind of pipe line steel Download PDFInfo
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Abstract
The invention discloses the area fraction assessment method of M/A island tissue in a kind of pipe line steel, belong to metallographic structure quantitative technique field.Described method comprises: area fraction series standard judge picture is organized on the M/A island setting up pipe line steel; M/A island is carried out to institute's test tube line steel curved beam and organizes Graphics Processing; By the M/A island tissue of metallography microscope sem observation sample, and area fraction series standard judge picture is organized to compare with set up M/A island; Determine to organize the immediate standard judge picture of area fraction with Zhong M/A island, visual field, area fraction is organized on the M/A island obtaining surveyed pipe line steel.The inventive method is simple to operate, require relatively low to the recognition capability of personnel and the display gray scale on M/A island, operator by with the comparison of series standard judge picture, the area fraction on M/A island in tissue can be assessed rapidly, easily, result is accurate, reliable, for pipeline steel organizational structure design and quality control provide technical support.
Description
Technical field
The present invention relates to metallographic structure quantitative technique field, more particularly, relate to the area fraction assessment method of M/A island tissue in a kind of pipe line steel.
Background technology
The toughness and tenacity of steel and its heterogeneous microstructure closely related.Hi-grade steel pipe line steel adopts thermomechanical Controlling Technology (TMCP) or burning optimization on line technology (HOP) to obtain granular bainite (GB) tissue usually.The distinguishing feature of granular bainite microstructure is on high density dislocation iron-based body, be dispersed with martensite and retained austenite (M/A) constituent element.This constituent element in island, is therefore called M/A island usually.M/A island is the important composition of granular bainite microstructure, is mainly distributed in intracrystalline or grain boundaries.As second-phase hard in tissue, there is appreciable impact on M/A island on the mechanical property of pipe line steel especially break resistance.Therefore, the quantitative assessment of the characteristic parameter such as M/A island area fraction, size has become pipe line steel and has checked indispensable project.
At present, the area fraction assessment method that laboratory is commonly used is metallographic software quantitative analysis method, and the method is generally divided into manual extraction and automatically extracts.
Manual extraction uses metallographic software or image processing software that all M/A islands are extracted by manual operations, then the M/A island total area obtained area fraction compared with the area of metallograph.Manual extraction method, owing to adopting manual identification, wastes time and energy, and identifies that the Capability Requirement on M/A island is very high to operating personnel.
Automatic extraction is the gray scale difference that software utilizes in tissue, automatically extracts M/A island tissue and carries out quantitative test.Although the method is simply rapid, the requirement of Dan Dui M/A island display packing is very high.If M/A island and matrix gray scale difference not obvious.Software often extracts crystal boundary or carbonide and analyzes, and causes the inaccurate of quantitatively calculating.
Chinese patent CN102175191A provides the quantivative approach of a kind of M/A island area percentage.First the method have employed Lapara mordant and carries out painted to M/A island.Then use laser confocal microscope scanned sample under zlasing mode, and carry out suitably regulating obtaining the obvious macrograph of gray scale difference to light intensity.Although the content on M/A island in the method energy accurate analysis pipe line steel tissue.But its complicated operation, need coordinate the use of laser confocal microscope, and this microscope costly, belong to high-end, unconventional equipment.
Therefore, said method is when evaluating M/A island area fraction, and existence is wasted time and energy, complicated operation, and requires high deficiency to the recognition capability of operating personnel and the display gray scale on M/A island.
Summary of the invention
The object of the invention is to waste time and energy for existing method, complicated operation, and high deficiency is required to the recognition capability of operating personnel and the display gray scale on M/A island, provide the area fraction assessment method of M/A island tissue in a kind of pipe line steel, the method can evaluate the area fraction that pipe line steel organizes Zhong M/A island quickly and accurately.
To achieve these goals, the technical solution adopted in the present invention is as follows:
An area fraction assessment method for M/A island tissue in pipe line steel, described assessment method comprises:
Area fraction series standard judge picture is organized on the M/A island setting up pipe line steel; M/A island is carried out to institute's test tube line steel curved beam and organizes Graphics Processing; By the M/A island tissue of microscopic examination sample, and area fraction series standard judge picture is organized to compare with set up M/A island; Determine to organize the immediate standard judge picture of area fraction with Zhong M/A island, visual field, area fraction is organized on the M/A island obtaining surveyed pipe line steel.
Area fraction series standard judge picture is organized on described M/A island, it is characterized in that: according to Hi-grade steel pipe line steel tissue characteristic, the M/A island area fraction of the series standard judge picture set up is 0 ~ 6%, is spaced apart 0.5%.
Carry out the tissue display of M/A island to institute's test tube line steel curved beam, its concrete grammar is as follows:
1) sample preparation: carried out polishing and polishing in the inspection face of pipe line steel sample, the inspection face prepared should become minute surface and no marking;
2) the corrosion display on M/A island: add 0.95-1.05g Sodium Metabisulfite in every 100ml distilled water; 3.6-3.7g picric acid and 0.6-0.7g NaOH is added in every 100ml absolute ethyl alcohol.Mixed by two kinds of solution and be heated to 50 ° of C ~ 60 ° C, insulation 2-4min, make it dissolve completely and fully react rear gained solution to be staining reagent, described distilled water solution and ethanol solution volume ratio are 1:1-3:2; Volume ratio is adopted by the pipe line steel sample prepared to be clean with alcohol after the nital corrosion 5 ~ 10s of 2 ~ 4% to dry up again; The staining reagent prepared is heated to 40 ° of C ~ 60 ° C, pipe line steel sample is put into and to adopt alcohol to clean after wherein soaking 120 ~ 240s to dry up, obtain brilliant white M/A island.
Sample also can adopt other solution corrosions, being as the criterion by clear display M/A island tissue.
Preferably, 1g Sodium Metabisulfite is added in every 100ml distilled water in the corrosion step display on described M/A island; 3.65g picric acid and 0.65g NaOH is added in every 100ml absolute ethyl alcohol.Mixed by two kinds of solution and be heated to 55 DEG C, insulation 3min, make it dissolve completely and fully react rear gained solution to be staining reagent, described distilled water solution and ethanol solution volume ratio are 3:2.
Preferably, visual field quantity on institute's test tube line steel curved beam inspection face is at least two, and determine that area fraction is organized on Zhong M/A island, each visual field with set up series standard judge picture, the M/A island area fraction evaluation result of institute's test tube line steel curved beam is obtained by averaging.
If observe Zhong M/A island, visual field organize area fraction to be between two judge picture content, its survey Zhong M/A island, visual field and organize area fraction to get area fraction between two judge picture.
Preferably, described microscopical enlargement factor is 500 times, and being close with tested visual field Zhong M/A island tissue size and standard judge picture Zhong M/A island tissue size is as the criterion.When M/A island size and the size in standard series figure in tested visual field differ greatly be difficult to compare time, the suitably microscopical enlargement ratio of adjustment, makes Zhong M/A island, tested visual field size be near the mark series of drawing as far as possible.
Beneficial effect of the present invention:
Simple to operate, require relatively low to the recognition capability of personnel and the display gray scale on M/A island, compensate for the deficiencies in the prior art.Operator by with standard series figure comparison, rapidly, the area fraction on M/A island in evaluation tissue easily, result accurately, reliable.The method provides technical support to pipeline steel organizational structure design and quality control.
Accompanying drawing explanation
Fig. 1 is assessment method procedure Procedure figure provided by the present invention.
Tu2Shi M/A organize on island area fraction be 0.5% standard judge picture;
Tu3Shi M/A organize on island area fraction be 1.0% standard judge picture;
Tu4Shi M/A organize on island area fraction be 1.5% standard judge picture;
Tu5Shi M/A organize on island area fraction be 2.0% standard judge picture;
Tu6Shi M/A organize on island area fraction be 2.5% standard judge picture;
Tu7Shi M/A organize on island area fraction be 3.0% standard judge picture;
Tu8Shi M/A organize on island area fraction be 3.5% standard judge picture;
Tu9Shi M/A organize on island area fraction be 4.0% standard judge picture;
Figure 10 be M/A island organize area fraction be 4.5% standard judge picture;
Figure 11 be M/A island organize area fraction be 5.0% standard judge picture;
Figure 12 be M/A island organize area fraction be 5.5% standard judge picture;
Figure 13 be M/A island organize area fraction be 6.0% standard judge picture.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described further.
The invention provides the area fraction assessment method of M/A island tissue in a kind of pipe line steel, as shown in Figure 1, described assessment method comprises:
One, area fraction series standard judge picture is organized on the M/A island setting up pipe line steel; As shown in Fig. 2-13.According to Hi-grade steel pipe line steel tissue characteristic, described M/A island organizes the M/A island content of area fraction series standard judge picture to be 0 ~ 6%, is spaced apart 0.5%.
Two, M/A island is carried out to institute's test tube line steel curved beam and organize Graphics Processing; Concrete grammar step is as follows:
1) sample preparation: carried out polishing and polishing in the inspection face of pipe line steel sample, the inspection face prepared should become minute surface and no marking;
2) the corrosion display on M/A island: add 0.95-1.05g Sodium Metabisulfite in every 100ml distilled water; 3.6-3.7g picric acid and 0.6-0.7g NaOH is added in every 100ml absolute ethyl alcohol.Mixed by two kinds of solution and be heated to 50 ° of C ~ 60 ° C, insulation 2-4min, make it dissolve completely and fully react rear gained solution to be staining reagent, described distilled water solution and ethanol solution volume ratio are 1:1-3:2; Volume ratio is adopted by the pipe line steel sample prepared to be clean with alcohol after the nital corrosion 5 ~ 10s of 2 ~ 4% to dry up again; The staining reagent prepared is heated to 40 ° of C ~ 60 ° C, pipe line steel sample is put into and to adopt alcohol to clean after wherein soaking 120 ~ 240s to dry up, obtain brilliant white M/A island.
Sample also can adopt volume ratio be 2 ~ 4% nital or other solution corrosions, can clear display M/A island tissue be as the criterion.
Preferably, 1g Sodium Metabisulfite is added in every 100ml distilled water in the corrosion step display on described M/A island; 3.65g picric acid and 0.65g NaOH is added in every 100ml absolute ethyl alcohol.Mixed by two kinds of solution and be heated to 50 ° of C ~ 60 ° C, insulation 2-4min, make it dissolve completely and fully react rear gained solution to be staining reagent, described distilled water solution and ethanol solution volume ratio are 3:2.
Three, observed the M/A island tissue of pipeline steel curved beam by metaloscope, and organize area fraction series standard judge picture to compare with set up M/A island;
Four, determine to organize the immediate standard judge picture of area fraction with Zhong M/A island, surveyed visual field, area fraction is organized on the M/A island obtaining surveyed pipe line steel.
Visual field quantity on institute's test tube line steel curved beam inspection face is at least two, and determines that area fraction is organized on Zhong M/A island, each visual field with set up series standard judge picture, obtains the M/A island area fraction evaluation result of institute's test tube line steel curved beam by averaging.
If observe Zhong M/A island, visual field organize area fraction to be between two judge picture content, its survey Zhong M/A island, visual field and organize area fraction to get area fraction between two judge picture.
The enlargement factor of described metaloscope is 500 times, and being close with tested visual field Zhong M/A island tissue size and standard judge picture Zhong M/A island tissue size is as the criterion.When the size in M/A island size in tested visual field and standard series figure differ greatly be difficult to comparative measurements time, the suitably microscopical enlargement ratio of adjustment, makes Zhong M/A island, tested visual field size be near the mark series of drawing as far as possible.
Embodiment:
1) sample preparation: X70 sample is used respectively to 120#, 360#, 600#, 800#, 1000# metallographic waterproof abrasive paper is roughly ground, fine grinding, uses the adamas of 2.5 μm, 1.5 μm to spray each polishing 3min of brilliant polish to sample afterwards respectively.Now the inspection face of sample becomes minute surface and no marking.
2) display on M/A island: clean with alcohol after sample being adopted the nital of 2% corrosion about 6s and dry up; By Sodium Metabisulfite 0.75g, picric acid 1.825g, NaOH 0.32g, distilled water 75ml, ethanol 50ml mix, and are heated to 50 ° of C, are put into by sample after wherein soaking 120s and dry up with alcohol is clean.
3) observe under sample being placed in metaloscope visual field, first with the low whole inspection face of enlargement ratio complete observation, choose 3 typical viewing field that inspection Mian Shang M/A island area fraction is moderate.
4) 3 typical viewing field are compared with standard series figure respectively, to determine that area fraction is organized on M/A island with the immediate grading picture in observation visual field, record assessed value respectively and be respectively 2.0%, 1.75% and 2.0%, calculate the M/A island that its mean value obtains this sample and organize area fraction evaluation result to be 1.92%.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. the area fraction assessment method of M/A island tissue in pipe line steel, it is characterized in that, described assessment method comprises:
Area fraction series standard judge picture is organized on the M/A island setting up pipe line steel; M/A island is carried out to institute's test tube line steel curved beam and organizes Graphics Processing; By the M/A island tissue of microscopic examination institute test tube line steel curved beam, and area fraction series standard judge picture is organized to compare with set up M/A island; Determine to organize the immediate standard judge picture of area fraction with Zhong M/A island, visual field, area fraction is organized on the M/A island obtaining surveyed pipe line steel;
The M/A island of described pipe line steel organizes area fraction series standard judge picture to comprise M/A island to organize area fraction to be respectively the standard judge picture of 0.5%, 1.0%, 1.5%, 2.0%, 2.5%, 3.0%, 3.5%, 4.0%, 4.5%, 5.0%, 5.5%, 6.0%;
Carry out the tissue display of M/A island to institute's test tube line steel curved beam, its concrete grammar is as follows:
1) sample preparation: carried out polishing and polishing in the inspection face of institute's test tube line steel curved beam, makes it check face to become minute surface;
2) the corrosion display on M/A island: add 0.95-1.05g Sodium Metabisulfite in every 100ml distilled water; 3.6-3.7g picric acid and 0.6-0.7g NaOH is added in every 100ml absolute ethyl alcohol, two kinds of solution are mixed and is heated to 50 DEG C ~ 60 DEG C, insulation 2-4min, make it dissolve completely and fully react rear gained solution to be staining reagent, described distilled water and absolute ethyl alcohol volume ratio are 1:1-3:2; Volume ratio is adopted by the institute's test tube line steel curved beam prepared to be clean with alcohol after the nital corrosion 5 ~ 10s of 2 ~ 4% to dry up again; The staining reagent prepared is heated to 40 DEG C ~ 60 DEG C, institute's test tube line steel curved beam is put into and to adopt alcohol to clean after wherein soaking 120 ~ 240s to dry up, obtain brilliant white M/A island.
2. the area fraction assessment method of M/A island tissue in pipe line steel according to claim 1, is characterized in that,
Visual field quantity on institute's test tube line steel curved beam inspection face is at least two, and compares with series standard judge picture and determine that area fraction is organized on Zhong M/A island, each visual field, obtains the M/A island area fraction evaluation result of institute's test tube line steel curved beam by averaging.
3. the area fraction assessment method of M/A island tissue in pipe line steel according to claim 2, is characterized in that,
If observe Zhong M/A island, visual field organize area fraction to be between two judge picture content, its survey Zhong M/A island, visual field and organize area fraction to get the mean value of the area fraction of two judge picture.
4., according to the area fraction assessment method of M/A island tissue in the arbitrary described pipe line steel of claim 1-3, it is characterized in that,
Described microscopical enlargement factor is 500 times.
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| CN104374789A (en) * | 2014-10-24 | 2015-02-25 | 中国石油天然气集团公司 | Quantitative analysis method for content of martensite-austenite island structures in high-strength microalloy pipeline steel |
| CN106442522A (en) * | 2016-06-29 | 2017-02-22 | 内蒙古第机械集团有限公司 | Method for inspecting quality rating of 60Si2CrVAT steel heat treatment |
| CN109142010B (en) * | 2018-09-10 | 2020-12-01 | 中国石油天然气集团有限公司 | Method for detecting distribution and content of residual austenite in low-alloy structural steel |
| CN109490300B (en) * | 2018-10-16 | 2021-02-26 | 包头钢铁（集团）有限责任公司 | Reagent preparation method and reagent use method |
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| US6841788B1 (en) * | 2000-08-03 | 2005-01-11 | Ascend Instruments, Inc. | Transmission electron microscope sample preparation |
| JP2002195921A (en) * | 2000-12-25 | 2002-07-10 | Fuji Electric Co Ltd | Thin film specimen and method for producing the same |
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