CN104458511A - Method for testing autstenitic grain size of steel bainite structure for nuclear pressure vessel - Google Patents
Method for testing autstenitic grain size of steel bainite structure for nuclear pressure vessel Download PDFInfo
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Abstract
The invention relates to a method for testing autstenitic grain size of a steel bainite structure for a nuclear pressure vessel. The method comprises the steps of preparing, grinding and polishing a metallographic phase sample, carrying out chemical etching on a sample and carrying out statistics on the grain size. According to the method, the rational proportions of picric acid, dodecylbenzene sulfonic acid and an additive as well as the etching time are selected, so that the original autstenitic grain size of the low-carbon and low-alloy steel SA508 Gr.3 steel bainite structure for nuclear power can be clearly displayed. After the method is adopted, the problem that the original autstenitic grain boundary is difficult to display in the actual production process of a forge piece of the nuclear pressure vessel can be solved; compared with the traditional method which is used for judging the autstenitic grain size by experience, the method has the advantage that the displayed autstenitic grain boundary is clear and complete; after the method is used for picture processing and statistics, the tested autstenitic grain size is more accurate and the repeatability is good.
Description
Technical field
The present invention relates to metallographic sample preparation and austenite crystal display technique field, especially relate to a kind of method of testing nuclear pressure container steel bainite structure autstenitic grain size.
Background technology
Nuclear power is one of important clean energy resource of modern society, and since Fukushima, Japan nuclear plant safety accident outburst in 2010, Nuclear Safety importance is more and more subject to people's attention.Nuclear pressure container is one of important leverage of Nuclear Safety, the damage of nuclear pressure container means nuclear leakage, therefore people are more and more stricter to the requirement of nuclear pressure container, and intensity, the toughness of design constantly increase, and irradiation fragility susceptibility, tough crisp transition temperature etc. require then constantly to reduce; Meanwhile, nuclear pressure container presents maximization, and the trend of integration, has higher requirement to nuclear pressure container design and manufacture technology and performance guarantee.
The performance of nuclear pressure container is relevant with processing technologys such as metallurgy, castings.From the angle of material science, the performance of material is determined by materials microstructure.So-called tissue comprises autstenitic grain size, and quenching structure is formed, the width of sheet being described as microstructure of more microcosmic and quantification, the crystal boundary length of unit area, the dislocation desity in lath, the diameter of precipitated phase, number and distribution etc.Wherein autstenitic grain size is the principal element determining nuclear power pressure vessel forging performance, fining austenite grains uniquely can improve intensity, also the method for toughness of material can be improved, from mechanism, because refine austenite can increase the austenite grain boundary length of material internal on the one hand, more chief reason is that tiny austenite crystal is when γ-α occurring from quench hot to low temperature and changing, form the substructure in more tiny lath cluster, lath bundle and half bar, add the big angle crystal boundary length of material.
Fining austenite grains is discussed, and is first will have suitable method to measure its austenite grain size.Nuclear pressure container steel is high-purity low-carbon low-alloy steel, and impurity content is low, grain boundary corrosion suffering, and the autstenitic grain size how measuring nuclear power pressure steel is the problem of puzzlement researcher always.201110156636.1) etc. (number of patent application: be studied with regard to the autstenitic grain size of tissue after the distortion of nuclear pressure container steel, result shows to adopt oversaturated picric acid solution+sea-gull board abluent repeatedly to corrode and adds gently to throw the autstenitic grain size that can show nuclear pressure container steel under this condition Hao Luhan.Because this mordant is mainly comparatively effective to martensitic stucture, large forgings is quenched the corrosive effect of austenite grain boundary of the bainite structure obtained not obvious.The people such as Bhadeshia adopt hot corrosion method to have studied Austenite Grain Growth process, from experimental result, adopt heat analysis method really can show austenite grain boundary clearly, due to the singularity of heat analysis method, also can not be used in the prior austenite grain size detection of nuclear power pressure vessel forging.The bright grade of Yang Yun organizes in recrystallizing regulation at research austenite deformation the autstenitic grain size adopting oxidizing process to determine nuclear pressure container steel in addition, adopt method be by distortion after organize polishing after be heated to about 700 DEG C, make its surperficial slight oxidation, then light throwing gets oxygenation level place observation autstenitic grain size.Above method or complicated operation, maybe can not show the autstenitic grain size of bainite structure, invents a kind of suitable high efficiency method and become more and more important to the autstenitic grain size showing nuclear pressure container steel bainite structure.
Summary of the invention
Object of the present invention be exactly provide to overcome defect that above-mentioned prior art exists a kind of can the clear and method of complete display nuclear pressure container steel austenite crystal.
Object of the present invention can be achieved through the following technical solutions:
Test a method for nuclear pressure container steel bainite structure autstenitic grain size, comprise preparation and the polishing of metallographic sample, the chemical etching of sample, statistics three steps of sample observation and grain size, specific as follows:
1) preparation of metallographic sample and polishing:
The cutting and inlay system of a, metallographic sample: the method for the bulk sample Linear cut taken off from actual forging is divided into fritter, and carries out polishing and polishing;
The corase grind of b, sample: by sample successively through aluminium oxide or the grinding of silit water-proof abrasive paper of 180# → 320# → 600#, the speed setting of abrasive disk is 500 ~ 800rpm, change a time sand paper at every turn, need by sample along grinding face 90-degree rotation, to make the polishing scratch of new a time vertical or approximately perpendicular to the polishing scratch of upper a time, till the polishing scratch being ground to new a time covers the polishing scratch of a time, tap water when grinding, is used to do lubricant;
The fine grinding of c, sample: ground on the aluminium oxide water-proof abrasive paper of 1200# by the sample after corase grind, the speed setting of abrasive disk is 300 ~ 500rpm, avoids rotating speed too high and produces darker polishing scratch; Till being ground to invisible upper a time polishing scratch along the direction that upper a time polishing scratch is vertical;
The polishing of d, sample: polishing on woollen polishing cloth will be placed in through the grinded sample of 1200# silit water-proof abrasive paper, use the diamond polishing liquid of 9 μm → 3 μm → 0.5 μm successively, rotating speed is 200 ~ 300rpm, obtain light and do not have pitted polished surface, using water and alcohol rinse successively and use hair-dryer to dry up;
2) chemical etching of sample:
The preparation of a, etching solution: the beaker filling distilled water is put into the water bath that temperature is set to 50 ~ 70 DEG C, picric acid is put into beaker, stir in the process that it is heated, obtain picric acid aqueous solution; Take neopelex afterwards and put into the picric acid aqueous solution prepared, add adjuvant wherein and obtain etching solution after stirring;
B, chemical etching: the water bath etching solution prepared being put into 50 ~ 60 DEG C, after temperature constant, be put in double dish by the sample after polishing, facet upward, the etching solution of a small amount of heat is dipped with absorbent cotton, wipe samples surface gently, back and forth after wiping several times, the etching solution again dipping heat repeats wiping, take out after wiping 3 ~ 5min, use new absorbent cotton wipe surfaces gently under tap water, after the membranaceous product on cleaned samples surface, use hair-dryer to dry up with alcohol rinse;
C, under metaloscope preliminary observation, being placed in polishing gently on woollen polishing cloth by corroding dark sample, not using antiscuffing paste, and light used tap water as lubricant when throwing; If first bite is crossed shallow, repeat b step, until original austenite crystal boundary clear and completely show;
3) sample observation and grain size statistics:
A, at metallography microscope Microscopic observation, take the metallograph of different amplification respectively;
B, employing image analysis software extract austenite grain boundary, adopt the standard method of grain size test, add up its austenite crystal diameter and autstenitic grain size.
Step 1) a step in, split the sample that obtains larger time, directly carry out polishing and polishing, split the sample obtained less time, carry out polishing and polishing after inlaying.
Etching solution is when preparing, and picric acid is dissolved in distilled water, heats therebetween and stirs, the transparent glassy yellow of the solution after heating; After adding neopelex, solution becomes pale yellow translucent, and in etching solution, picric mass percent is 5 ~ 6%, and the mass percent of neopelex is 5 ~ 6%, and the mass percent of adjuvant is 0.1 ~ 0.2%.Using picric acid aqueous solution as mordant, adopt neopelex as wetting agent, after it adds picric acid aqueous solution, in sample etch process, the polar group in metal surface absorption wetting agent, nonpolar group is then formed and aligns, separate sample and picric acid, avoid sample directly to contact with picric, suppress etching solution to the corrosion of matrix, and can not sample grain boundary corrosion be impacted, thus reach the object of selective corrosion crystal boundary.
Described adjuvant is analytically pure HCl solution.
Step 2) when etch is carried out to sample, the etching solution dipping heat with the absorbent cotton soaked spreads upon metallographic sample surface uniformly, wiping is after 3 ~ 5 minutes, dry up with alcohol rinse with after absorbent cotton scrub, preliminary observation under metaloscope, polishing gently on woollen polishing cloth was placed in by corroding dark sample, but can not be deeply polished, the crystal boundary corroding out is prevented to be removed in polishing, the sample inadequate to corrosion, adopt extend the wiping time, until original austenite crystal boundary clear and completely show.
Step 3) in take the metallograph of 200 times, 500 times, 1000 times at metallography microscope Microscopic observation.
Picric acid, as one of the principal ingredient of etching solution, is a kind of organic acid, also known as 2,4,6-trinitrophenol.In picric acid, the oxidisability of nitro is not as good as other inorganic acid such as hydrochloric acid, nitric acid, uses the tissue of its solution corrosion metal material, and corrosion process can be made to slow down, and is conducive to controlling the selectivity of etching time.But easily produce the blunt film of one deck (corrosion product of indissoluble) at sample surfaces during picric acid aqueous corrosion, affect further corrosion and the metallographic observation of sample.Therefore in the present invention, the method for absorbent cotton wiping is adopted, in time the corrosion product on cleaning surface.In addition, picric acid solution is a kind of good universal etchant when adding without other, can show the tissues such as ferrite, pearlite and bainite, and can mix with the solution such as sodium thiosulfate, there is different plated films painted to different tissues, obtain colour metallograpy effect.Do not highlight out the ability of original austenite crystal prevention.Neopelex is anionic surfactant, after it adds saturated picric acid aqueous solution, in sample etch process, its polar group is adsorbed by metal surface, nonpolar group is then formed and aligns, and then separated, avoid sample and directly contact with picric, inhibiting effect is served to matrix etch process.Therefore, as a kind of corrosion inhibiter, its interpolation makes the surface tension of supersaturation picric acid solution reduce, and avoids the excessive corrosion of sample tissue and causes original austenite crystal prevention clearly to manifest.The present invention, through many experiments, determines the etch temperature and time being applicable to the test of examination nuclear pressure container steel bainite structure autstenitic grain size.
Compared with prior art, the present invention is directed to the problem that current nuclear power pressure vessel forging bainite structure original austenite grains is difficult to show, provide a kind of can the clear and method of complete display nuclear pressure container steel austenite crystal, can be used for the method substituting the mensuration grain size relying on ready visual contrast standard diagram at present, have the following advantages:
(1) by the rational proportion of picric acid solution and neopelex, suitable corrosion temperature and etching time is selected to obtain best effect, the best etch temperature (50 ~ 60 DEG C) obtained is groped through many experiments, (3 ~ 5min) clear and complete the manifesting of the original austenite grain of bainite structure can be made in the short period of time, this is because, if thermal creep stress is too low, picric acid is not active to grain boundary corrosion, etching time is long, and efficiency is lower; Temperature is too high, and picric acid has not only corroded crystal boundary and also corroded intergranular structure simultaneously, optionally can not corrode crystal boundary.
(2) etching solution prepares and gets to pour in right amount in small beaker after leaving standstill and implements etch process, avoid on the one hand and do not dissolve completely and the excessive corrosion of supersaturation picric acid particle to sample that precipitate is painted, avoid the large-scale pollution of corrosion product to etching solution on the other hand, remaining etching solution can still be protected fresh.
(3) sample involved in the present invention is the qtenched sample of nuclear pressure container large forgings, it is organized as bainite structure, can be and judges whether it exists mixed crystal, the problem of coarse grains, optimize Technology for Heating Processing, the particularly formulation of follow-up tempering process and theoretical foundation is provided.
Accompanying drawing explanation
Fig. 1 is the nuclear power pressure vessel forging austenitizing temperature of embodiment 1 gained when being 1000 DEG C, the metallograph of bainite structure original austenite grains size and distribution after quenching;
Fig. 2 is the nuclear power pressure vessel forging austenitizing temperature of embodiment 2 gained when being 900 DEG C, the metallograph of bainite structure original austenite grains size and distribution after quenching.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
Test a method for nuclear pressure container steel bainite structure autstenitic grain size, comprise preparation and the polishing of metallographic sample, the chemical etching of sample, statistics three steps of sample observation and grain size, specific as follows:
1) preparation of metallographic sample and polishing:
The cutting and inlay system of a, metallographic sample: from the bulk sample that the austenitizing temperature actual forging that is 1000 DEG C is taken off, intercept the cube of 10mm*10mm*5mm, inlay with phenolic moulding powder by the method for Linear cut, carries out polishing and polishing is prepared for follow-up;
The corase grind of b, sample: sample is ground through the silit water-proof abrasive paper of 180# → 320# → 600# successively, the speed setting of abrasive disk is 600rpm, change a time sand paper at every turn, need by sample along grinding face 90-degree rotation, to make the polishing scratch of new a time vertical or approximately perpendicular to the polishing scratch of upper a time, till the polishing scratch being ground to new a time covers the polishing scratch of a time, tap water when grinding, is used to do lubricant;
The fine grinding of c, sample: ground on the aluminium oxide water-proof abrasive paper of 1200# by the sample after corase grind, the speed setting of abrasive disk is 400rpm, till being ground to invisible upper a time polishing scratch along the direction that upper a time polishing scratch is vertical;
The polishing of d, sample: polishing on woollen polishing cloth will be placed in through the grinded sample of 1200# silit water-proof abrasive paper, use the diamond polishing liquid of 9 μm → 3 μm → 0.5 μm successively, rotating speed is 200rpm, obtain the polished surface of light, use water and alcohol rinse successively and use hair-dryer to dry up.
2) chemical etching of sample:
The preparation of a, etching solution: the beaker filling 100ml distilled water is put into the water bath that temperature is set to 60 DEG C, 5g picric acid is put into beaker, stir in the process that it is heated, prepare picric acid aqueous solution; To weigh afterwards 5g neopelex put into the supersaturation picric acid aqueous solution prepared, add the adjuvant of 0.1% wherein and for subsequent use after stirring;
B, chemical etching: the etching solution prepared is taken out the water bath that 20ml puts into 60 DEG C, after constant temperature, sample is put in double dish, facet upward, the etching solution of a small amount of heat is dipped with absorbent cotton, wipe samples surface, takes out after wiping 3min gently, uses new absorbent cotton wipe surfaces gently under tap water, after the membranaceous product on cleaned samples surface, hair-dryer is used to dry up with alcohol rinse;
C, under metaloscope preliminary observation, after etch, crystal boundary is clear, though there is part room temperature texture to be corroded out simultaneously, extent of corrosion is comparatively light, does not affect the observation of austenite crystal, omits mechanical polishing step.
3) sample observation and grain size statistics:
A, at metallography microscope Microscopic observation, take the metallograph of 200 times, 500 times, 1000 times respectively;
B, adopt suitable image analysis software, extract austenite grain boundary, adopt the standard method of grain size test, add up its austenite crystal diameter and autstenitic grain size.
Fig. 1 is that SA508-3 steel organizes metallograph under these conditions after sample preparation+grinding and polishing+etch under metaloscope under observable 200 times (a), 500 times (b) and 1000 times (c), and what original austenite crystal prevention can be clear and complete manifests.It is 1000 DEG C that austenitizing temperature is worked as in result display, and organizing of original austenite is thick, and adopting image analysis software to record its average crystal grain diameter is 89.7 μm.
Embodiment 2
Test a method for nuclear pressure container steel bainite structure autstenitic grain size, comprise preparation and the polishing of metallographic sample, the chemical etching of sample, statistics three steps of sample observation and grain size, specific as follows:
1) preparation of metallographic sample and polishing:
The cutting and inlay system of a, metallographic sample: the method for the bulk sample Linear cut taken off by the actual forging from austenitizing temperature being 900 DEG C takes off the sample that size is 10mm*10mm*20mm size, because sample is larger, do not need to inlay, the method for hand-held grinding and polishing can be adopted to prepare sample;
The corase grind of b, sample: sample is ground through the silit water-proof abrasive paper of 180# → 320# → 600# successively, the speed setting of abrasive disk is 500rpm, change a time sand paper at every turn, need by sample along grinding face 90-degree rotation, to make the polishing scratch of new a time vertical or approximately perpendicular to the polishing scratch of upper a time, till the polishing scratch being ground to new a time covers the polishing scratch of a time, tap water when grinding, is used to do lubricant;
c, sample fine grinding: by corase grind after sample grind on the aluminium oxide water-proof abrasive paper of 1200#, the speed setting of abrasive disk is 300rpm, till being ground to invisible upper a time polishing scratch along the direction that upper a time polishing scratch is vertical;
The polishing of d, sample: polishing on woollen polishing cloth will be placed in through the grinded sample of 1200# silit water-proof abrasive paper, use the diamond polishing liquid of 9 μm → 3 μm → 0.5 μm successively, rotating speed is 200rpm, obtain the polished surface of light, use water and alcohol rinse successively and use hair-dryer to dry up.
2) chemical etching of sample:
The preparation of a, etching solution: the beaker filling 100ml distilled water is put into the water bath that temperature is set to 60 DEG C, 5g picric acid is put into beaker, stir in the process that it is heated, prepare picric acid aqueous solution; To weigh afterwards 5g neopelex put into the supersaturation picric acid aqueous solution prepared, add the adjuvant of 0.1% wherein and for subsequent use after stirring;
B, chemical etching: the etching solution prepared is taken out the water bath that 20ml puts into 50 DEG C, after constant temperature, sample is put in double dish, facet upward, the etching solution of a small amount of heat is dipped with absorbent cotton, wipe samples surface, takes out after wiping 3min gently, uses new absorbent cotton wipe surfaces gently under tap water, after washing the membranaceous product earning sample surfaces, hair-dryer is used to dry up with alcohol rinse;
C, under metaloscope preliminary observation, find have crystal boundary to manifest after etch, but discontinuous, therefore repeat step 2 (b), examine under a microscope after in this corrosion 3min, now austenite grain boundary is clear, can be used for autstenitic grain size statistics.
3) sample observation and grain size statistics:
A, at metallography microscope Microscopic observation, take the metallograph of 200 times, 500 times, 1000 times respectively;
B, adopt suitable image analysis software, extract austenite grain boundary, adopt the standard method of grain size test, add up its austenite crystal diameter and autstenitic grain size.
Fig. 2 is that SA508-3 steel organizes metallograph after austenitizing temperature is the actual forging sampling+grinding and polishing+etch of 900 DEG C under metaloscope under observable 200 times (a) and 500 times (b), original austenite crystal prevention can be clear and complete the result that manifests show, when austenitizing temperature is 900 DEG C, austenite crystal is tiny, and adopting image analysis software to record its average crystal grain diameter is 27.5 μm.
Claims (5)
1. test a method for nuclear pressure container steel bainite structure autstenitic grain size, it is characterized in that, the method comprises preparation and the polishing of metallographic sample, the chemical etching of sample, statistics three steps of sample observation and grain size, specific as follows:
1) preparation of metallographic sample and polishing:
The cutting and inlay system of a, metallographic sample: the method for the bulk sample Linear cut taken off from actual forging is divided into fritter, and carries out polishing and polishing;
The corase grind of b, sample: by sample successively through aluminium oxide or the grinding of silit water-proof abrasive paper of 180# → 320# → 600#, the speed setting of abrasive disk is 500 ~ 800rpm, change a time sand paper at every turn, need by sample along grinding face 90-degree rotation, to make the polishing scratch of new a time vertical or approximately perpendicular to the polishing scratch of upper a time, till the polishing scratch being ground to new a time covers the polishing scratch of a time, tap water when grinding, is used to do lubricant;
The fine grinding of c, sample: ground on the aluminium oxide water-proof abrasive paper of 1200# by the sample after corase grind, the speed setting of abrasive disk is 300 ~ 500rpm, avoids rotating speed too high and produces darker polishing scratch; Till being ground to invisible upper a time polishing scratch along the direction that upper a time polishing scratch is vertical;
The polishing of d, sample: polishing on woollen polishing cloth will be placed in through the grinded sample of 1200# silit water-proof abrasive paper, use the diamond polishing liquid of 9 μm → 3 μm → 0.5 μm successively, rotating speed is 200 ~ 300rpm, obtain light and do not have pitted polished surface, using water and alcohol rinse successively and use hair-dryer to dry up;
2) chemical etching of sample:
The preparation of a, etching solution: the beaker filling distilled water is put into the water bath that temperature is set to 50 ~ 70 DEG C, picric acid is put into beaker, stir in the process that it is heated, obtain picric acid aqueous solution; Take neopelex afterwards and put into the picric acid aqueous solution prepared, add adjuvant wherein and obtain etching solution after stirring;
B, chemical etching: the water bath etching solution prepared being put into 50 ~ 60 DEG C, after temperature constant, be put in double dish by the sample after polishing, facet upward, the etching solution of a small amount of heat is dipped with absorbent cotton, wipe samples surface gently, back and forth after wiping several times, the etching solution again dipping heat repeats wiping, take out after wiping 3 ~ 5min, use new absorbent cotton wipe surfaces gently under tap water, after the membranaceous product on cleaned samples surface, use hair-dryer to dry up with alcohol rinse;
C, under metaloscope preliminary observation, being placed in polishing gently on woollen polishing cloth by corroding dark sample, not using antiscuffing paste, and light used tap water as lubricant when throwing; If first bite is crossed shallow, repeat b step, until original austenite crystal boundary clear and completely show;
3) sample observation and grain size statistics:
A, at metallography microscope Microscopic observation, take the metallograph of different amplification respectively;
B, employing image analysis software extract austenite grain boundary, adopt the standard method of grain size test, add up its austenite crystal diameter and autstenitic grain size.
2. a kind of method of testing nuclear pressure container steel bainite structure autstenitic grain size according to claim 1, it is characterized in that, step 1) a step in, when the sample that segmentation obtains is larger, directly carry out polishing and polishing, when the sample that segmentation obtains is less, carry out polishing and polishing after inlaying.
3. a kind of method of testing nuclear pressure container steel bainite structure autstenitic grain size according to claim 1, it is characterized in that, etching solution is when preparing, and picric acid is dissolved in distilled water, heat while stir therebetween, the transparent glassy yellow of the solution after heating; After adding neopelex, solution becomes pale yellow translucent, and in etching solution, picric mass percent is 5 ~ 6%, and the mass percent of neopelex is 5 ~ 6%, and the mass percent of adjuvant is 0.1 ~ 0.2%.
4. a kind of method of testing nuclear pressure container steel bainite structure autstenitic grain size according to claim 1 or 3, is characterized in that, described adjuvant is analytically pure HCl solution.5. a kind of method of testing nuclear pressure container steel bainite structure autstenitic grain size according to claim 1, it is characterized in that, step 2) when etch is carried out to sample, the etching solution dipping heat with the absorbent cotton soaked spreads upon metallographic sample surface uniformly, wiping is after 3 ~ 5 minutes, dry up with alcohol rinse with after absorbent cotton scrub, preliminary observation under metaloscope, polishing gently on woollen polishing cloth was placed in by corroding dark sample, but can not be deeply polished, the crystal boundary corroding out is prevented to be removed in polishing, the sample inadequate to corrosion, adopt and extend the wiping time, until original austenite crystal boundary clear and completely show.
5. a kind of method of testing nuclear pressure container steel bainite structure autstenitic grain size according to claim 1, is characterized in that, step 3) at metallography microscope Microscopic observation, take the metallograph of 200 times, 500 times, 1000 times respectively.
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