CN103389050A - Method for displaying M/A island structures inside pipeline steel - Google Patents
Method for displaying M/A island structures inside pipeline steel Download PDFInfo
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Abstract
The invention discloses a method for displaying M/A island structures inside pipeline steel, and belongs to the technical field of metallographic phase structure displaying and quantifying. Specifically, A sample is grinded and polished into a mirror face to be used later; 1g sodium metabisulfite is added into 100ml distilled water inside a beaker; 3.65g picric acid and 0.65g sodium hydroxide are added into 100ml absolute ethyl alcohol; the two kinds of solutions are mixed according to the proportion of 3: 2 and are heated and stirred to obtain the improved staining reagent; 2-4% of nitric acid ethyl alcohol solution is used for slightly corroding the prepared sample, and the sample is placed into the staining reagent to be immersed for 120-240 seconds and then is washed clean through the ethyl alcohol and is blown to be dried; an M/A island presents bright white and is very different from the surrounding structures in the gray level. The method is easy to operate, the corrosion time is short, and the area content, the size, the shape and other characteristic parameters of the M/A island in the structures can be fast, accurately and quantificationally analyzed through metallographic phase software.
Description
Technical field
The present invention relates to metallographic structure demonstration and quantitative technique field, the display packing of M/A island tissue in a kind of pipe line steel specifically is provided.
Background technology
The toughness and tenacity of steel and its heterogeneous microstructure are closely related.Along with the raising of toughness and tenacity, the pipe line steel tissue develops into granular bainite (GB) type gradually by initial ferrite-pearlite (PF-P) type.The distinguishing feature of granular bainite microstructure is distributing on high density dislocation iron-based body martensite and retained austenite (M/A) island.The M/A island is the important composition of granular bainite microstructure.As hard second-phase in tissue, the characteristic parameters such as the area content on M/A island, size, form have considerable influence to the pipe line steel toughness and tenacity.Therefore, the quantitative test on M/A island, to the pipeline steel organizational structure design, improves material property significant, has become the indispensable project of pipe line steel check.
At present, laboratory analytical approach commonly used has manual imitation method and metallographic software quantitative analysis method etc.The imitation method is to cover after sample is organized the tissue of copying the M/A island on photo and carry out quantitative test with paraffin paper.The method, owing to adopting manual imitation, wastes time and energy, and it is very high that operating personnel are identified the Capability Requirement on M/A island, progressively is eliminated.Metallographic software quantitative analysis method is the gray scale difference in software utilization tissue, automatically extracts M/A island tissue and carries out quantitative test.Although the method is rapidly simple, and is very high to the requirement of M/A island display packing.As adopt traditional nitric acid alcohol corrosion (Fig. 1), software to tend to a crystal boundary or carbonide to extract and analyze, what cause quantitatively calculating is inaccurate.
(petroleum industry is published in " microscopic examination of high-strength micro-alloy pipe line steel and discriminating collection of illustrative plates " that the people such as Li Helin, Guo Shengwu, Feng Yaorong show, 2001) mentioned a kind of Lapara mordant in, this mordant can carry out painted to the M/A island, after painted, in tissue, the M/A island is white, all the other are grey black, and metallographic software can extract and quantitative test the M/A island more accurately.But this Lapara reagent etching time is longer, often near 10min, and the M/A island after painted and the remaining tissue gray scale difference often not obvious, the precision that causes the quantitative test of M/A island is not very desirable.
Chinese patent CN 102175191 A disclose " quantivative approach of the area percentage of a kind of MA island tissue ", and it adopts the Lapara mordant to carry out painted to the M/A island.After painted, must use laser confocal microscope scanned sample under zlasing mode, and light intensity is carried out suitably regulating obtain gray scale difference and significantly organize photo.The content on M/A island in the method energy accurate analysis pipe line steel tissue.But its complicated operation, need to coordinate the use of laser confocal microscope, and this microscope is more expensive, belongs to high-end, unconventional equipment.
Summary of the invention
In order to realize fast, the M/A island in the display pipeline structure of steel clearly, thereby can accurately to the M/A island in the pipe line steel tissue, carry out quantitative test, the invention provides the display packing of M/A island tissue in a kind of pipe line steel.
Described technical scheme is as follows:
The display packing of M/A island tissue in a kind of pipe line steel, described step is as follows:
Step 1, make minute surface with the check face of pipe line steel sample;
Step 2, the preparation of staining reagent
Add the 0.95-1.05g Sodium Metabisulfite in every 100ml distilled water;
Add 3.6-3.7g picric acid and 0.6-0.7g NaOH in every 100ml absolute ethyl alcohol;
Two kinds of solution are mixed and be heated to 50 ℃～60 ℃, insulation 2-4min, dissolve it fully and fully namely obtain staining reagent after reaction;
Wherein distilled water solution and ethanol solution volume ratio are 1:1-3:2;
Step 3, carry out corrosion treatment with pipe line steel sample prepared in step 1, and it is positioned over the corrosion demonstration of entering the M/A island in the prepared staining reagent of step 2.
Preferably, in described step 2, the preparation of staining reagent specifically comprises the following steps:
Add the 1g Sodium Metabisulfite in every 100ml distilled water;
Add 3.65g picric acid and 0.65g NaOH in every 100ml absolute ethyl alcohol;
Two kinds of solution are mixed and be heated to 50 ℃, insulation 3min, dissolve it fully and fully namely obtain staining reagent after reaction, and wherein said distilled water solution and ethanol solution volume ratio are 3:2.
Further, the concrete grammar that in described step 3, the pipe line steel sample is carried out corrosion treatment is:
It is to clean and dry up with alcohol again after nital corrosion 5 ~ 10s of 2 ~ 4% that the pipe line steel sample is adopted volume ratio, and this moment, metallographic observation should be slight etch.
Further, after the metallographic of pipe line steel sample was carried out slight etch, concrete grammar that its corrosion shows was:
The staining reagent for preparing is heated to 40 ℃～60 ℃;
Pipe line steel sample after slight etch is put into and wherein soaked 120～240s;
Clean and dry up by alcohol, obtain brilliant white M/A island.
The check face with the pipe line steel sample described in step 1 is made minute surface, and its concrete grammar comprises: polishing is processed and polishing:
Described polishing is processed and is polished by the check face of metallographic waterproof abrasive paper to the pipe line steel sample;
Described polishing comprises rough polishing and fine polishing, by using the test check face of adamas spraying brilliant polish after polishing disk is to fine grinding, carries out polishing.
The paper trade mark that the metallographic waterproof abrasive paper that uses is processed in described polishing sequentially is followed successively by 120#, 360#, 600#, 800#, 1000#, and by the ascending metallographic fine sandpaper trade mark that uses in order, the polishing direction of the metallographic fine sandpaper of adjacent two trades mark becomes 90 °.
Described rough polishing is processed the adamas spraying brilliant polish that adopts 2.5 μ m, and polishing time is 2～5min;
Described essence is thrown and is processed the adamas spraying brilliant polish that adopts 1.5 μ m, and polishing time is 2～5min.
Beneficial effect of the present invention is:
By preparing staining reagent, the pipe line steel test check face after polishing, polishing is corroded demonstration, it is simple to operate, the not enough 5min of etching time.Comparing etching time with Lapara reagent shortens greatly.M/A island and remaining tissue gray scale difference in tissue are obvious, can adopt the metallographic software characteristic parameter such as the M/A island area content in the quantitative test tissue, size, form quickly and accurately.
Description of drawings
Fig. 1 adopts the X80 pipe line steel after traditional nitric acid alcohol corrodes to organize photo;
Fig. 2 adopts the X70 pipe line steel of the embodiment of the present invention 1 to organize photo;
Fig. 3 adopts the X80 pipe line steel of the embodiment of the present invention 2 to organize photo;
Fig. 4 adopts the X80 pipe line steel of the embodiment of the present invention 3 to organize photo.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described further.
The invention provides the display packing of M/A island tissue in a kind of pipe line steel, described step is as follows:
Step 1, make minute surface with the check face of pipe line steel sample;
Its concrete disposal route comprises: polishing is processed and polishing:
It is by using different trade mark metallographic waterproof abrasive papers to carry out grinding process to test check face that described polishing is processed, and the polishing direction after the replacing fine sandpaper becomes 90 ° with upper track polishing direction, until the upper track polishing scratch is ground off.Above process need uninterruptedly keeps the water of certain flow as liquid coolant.Grinding process uses the paper trade mark of metallographic waterproof abrasive paper sequentially to be followed successively by 120#, 360#, 600#, 800#, 1000#.
Polishing is carried out polishing by the test check face after adopting adamas spraying brilliant polish to fine grinding.
Polishing wherein comprises that rough polishing is processed and essence is thrown processing;
Described rough polishing is processed the adamas spraying brilliant polish that adopts 2.5 μ m, and polishing time is 2～5min;
Described essence is thrown and is processed the adamas spraying brilliant polish that adopts 1.5 μ m, and polishing time is 2～5min.
Step 2, the preparation of staining reagent
Add the 0.95-1.05g Sodium Metabisulfite in every 100ml distilled water; Add 3.6-3.7g picric acid and 0.6-0.7g NaOH in every 100ml absolute ethyl alcohol.Two kinds of solution are mixed and be heated to 50 ℃～60 ℃, insulation 2-4min, dissolve it and fully react rear gained solution to be staining reagent fully, and described distilled water solution and ethanol solution volume ratio are 1:1-3:2;
Step 3, the corrosion on M/A island shows
It is to clean and dry up with alcohol again after nital corrosion 5 ~ 10s of 2 ~ 4% that pipe line steel sample polished in step 1 is adopted volume ratio; This moment, metallographic observation should be slight etch, otherwise appropriateness is adjusted etching time.
The staining reagent for preparing in step 2 is heated to 40 ℃～60 ℃, the pipe line steel sample is put into wherein to soak after 120～240s adopt alcohol to clean to dry up, obtain brilliant white M/A island.
Embodiment 1
Step 1, the preparation of pipe line steel sample
The X70 sample is used respectively 120#, 360#, 600#, 800#, 1000# metallographic waterproof abrasive paper are roughly ground, fine grinding.Polishing direction after the replacing fine sandpaper will become 90 ° with the upper track direction, until the upper track polishing scratch grinds off.Afterwards sample is used respectively each polishing of adamas spraying brilliant polish 3min of 2.5 μ m, 1.5 μ m.This moment, the check face of sample became minute surface and no marking.
Step 2, the preparation of staining reagent
The 0.95g Sodium Metabisulfite will be added in 100ml distilled water in beaker; Add 3.6g picric acid and 0.6g NaOH in the 100ml absolute ethyl alcohol.Two kinds of solution 3:2 are mixed and be heated to 50 ℃, insulation 2min.Stir and it is dissolved fully and fully reaction with glass bar in heating process, gained solution is staining reagent.
Step 3, the corrosion on M/A island shows
To clean and dry up with alcohol behind the nital corrosion 5s left and right of sample employing 2%.This moment, metallographic observation should be mild corrosion.Staining reagent prepared in step 2 is heated to 50 ℃, sample is put into wherein to soak after 200s with alcohol, clean and dry up.
Through above-mentioned the pipe line steel sample is processed after, it is placed under metaloscope and observes, as shown in Figure 2, the M/A island presents brilliant white M/A island, and is obvious with the surrounding tissue gray scale difference.
Embodiment 2
Step 1, the preparation of pipe line steel sample
The X80 sample is used respectively 120#, 360#, 600#, 800#, 1000# metallographic waterproof abrasive paper are roughly ground, fine grinding.Polishing direction after the replacing fine sandpaper will become 90 ° with the upper track direction, until the upper track polishing scratch grinds off.Afterwards sample is used respectively each polishing of adamas spraying brilliant polish 5min of 2.5 μ m, 1.5 μ m.This moment, the check face of sample became minute surface and no marking.
Step 2, the preparation of staining reagent
The 1g Sodium Metabisulfite will be added in 100ml distilled water in beaker; Add 3.65g picric acid and 0.65g NaOH in the 100ml absolute ethyl alcohol.Two kinds of solution 3:2 are mixed and be heated to 50 ℃, insulation 3min.Stir and it is dissolved fully and fully reaction with glass bar in heating process, gained solution is staining reagent.
Step 3, the corrosion on M/A island shows
To clean and dry up with alcohol behind the nital corrosion 5s left and right of sample employing 2%.This moment, metallographic observation should be slight etch.Staining reagent prepared in step 2 is heated to 50 ℃, sample is put into wherein to soak after 180s with alcohol, clean and dry up.
Through above-mentioned the pipe line steel sample is processed after, it is placed under metaloscope and observes, as shown in Figure 3, the M/A island presents brilliant white M/A island, and is obvious with the surrounding tissue gray scale difference.
Embodiment 3
Step 1, the preparation of pipe line steel sample
The X80 sample is used respectively 120#, 360#, 600#, 800#, 1000# metallographic waterproof abrasive paper are roughly ground, fine grinding.Polishing direction after the replacing fine sandpaper will become 90 ° with the upper track direction, until the upper track polishing scratch grinds off.Afterwards sample is used respectively each polishing of adamas spraying brilliant polish 5min of 2.5 μ m, 1.5 μ m.This moment, the check face of sample became minute surface and no marking.
Step 2, the preparation of staining reagent
The 1.05g Sodium Metabisulfite will be added in 100ml distilled water in beaker; Add 3.7g picric acid and 0.7g NaOH in the 100ml absolute ethyl alcohol.Two kinds of solution 3:2 are mixed and be heated to 50 ℃, insulation 3min.Stir and it is dissolved fully and fully reaction with glass bar in heating process, gained solution is staining reagent.
Step 3, the corrosion on M/A island shows
To clean and dry up with alcohol behind the nital corrosion 5s left and right of sample employing 4%.This moment, metallographic observation should be slight etch.Staining reagent prepared in step 2 is heated to 55 ℃, sample is put into wherein to soak after 240s with alcohol, clean and dry up.
Through above-mentioned the pipe line steel sample is processed after, it is placed under metaloscope and observes, as shown in Figure 4, the M/A island presents brilliant white M/A island, and is obvious with the surrounding tissue gray scale difference.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (7)
1. the display packing of M/A island tissue in a pipe line steel, is characterized in that, described step is as follows:
Step 1, make minute surface with the check face of pipe line steel sample;
Step 2, the preparation of staining reagent
Add the 0.95-1.05g Sodium Metabisulfite in every 100ml distilled water;
Add 3.6-3.7g picric acid and 0.6-0.7g NaOH in every 100ml absolute ethyl alcohol;
Two kinds of solution are mixed and be heated to 50 ℃～60 ℃, insulation 2-4min, dissolve it fully and fully namely obtain staining reagent after reaction;
Wherein distilled water solution and ethanol solution volume ratio are 1:1-3:2;
Step 3, carry out corrosion treatment with pipe line steel sample prepared in step 1, and it is positioned over the corrosion demonstration of entering the M/A island in the prepared staining reagent of step 2.
2. the display packing of M/A island tissue in pipe line steel according to claim 1, is characterized in that,
In described step 2, the preparation of staining reagent specifically comprises the following steps:
Add the 1g Sodium Metabisulfite in every 100ml distilled water;
Add 3.65g picric acid and 0.65g NaOH in every 100ml absolute ethyl alcohol;
Two kinds of solution are mixed and be heated to 50 ℃, insulation 3min, dissolve it fully and fully namely obtain staining reagent after reaction, and wherein said distilled water solution and ethanol solution volume ratio are 3:2.
3. the display packing of M/A island tissue in pipe line steel according to claim 1 and 2, is characterized in that,
The concrete grammar that in described step 3, the pipe line steel sample is carried out corrosion treatment is:
It is to clean and dry up with alcohol again after nital corrosion 5 ~ 10s of 2 ~ 4% that the pipe line steel sample is adopted volume ratio, and this moment, metallographic observation should be slight etch.
4. the display packing of M/A island tissue in pipe line steel according to claim 3, is characterized in that,
After the metallographic of pipe line steel sample was carried out slight etch, concrete grammar that its corrosion shows was:
The staining reagent for preparing is heated to 40 ℃～60 ℃;
Pipe line steel sample after slight etch is put into and wherein soaked 120～240s;
Clean and dry up by alcohol, obtain brilliant white M/A island.
5. the display packing of M/A island tissue in pipe line steel according to claim 1, is characterized in that,
The check face with the pipe line steel sample described in step 1 is made minute surface, and its concrete grammar comprises: polishing is processed and polishing:
Described polishing is processed and is polished by the check face of metallographic waterproof abrasive paper to the pipe line steel sample;
Described polishing comprises rough polishing and fine polishing, by using the test check face of adamas spraying brilliant polish after polishing disk is to fine grinding, carries out polishing.
6. the display packing of M/A island tissue in pipe line steel according to claim 5, is characterized in that,
The paper trade mark that the metallographic waterproof abrasive paper that uses is processed in described polishing sequentially is followed successively by 120#, 360#, 600#, 800#, 1000#, and by the ascending metallographic fine sandpaper trade mark that uses in order, the polishing direction of the metallographic fine sandpaper of adjacent two trades mark becomes 90 °.
7. the display packing of M/A island tissue in pipe line steel according to claim 5, is characterized in that,
Described rough polishing is processed the adamas spraying brilliant polish that adopts 2.5 μ m, and polishing time is 2～5min;
Described essence is thrown and is processed the adamas spraying brilliant polish that adopts 1.5 μ m, and polishing time is 2～5min.
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Cited By (7)
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| CN104236980A (en) * | 2014-09-30 | 2014-12-24 | 钢铁研究总院 | Retained austenite contained dual phase steel color metallography coloring agent and coloring display method |
| 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 |
| CN106191864A (en) * | 2016-08-19 | 2016-12-07 | 山东钢铁股份有限公司 | Heterogeneous structure high-grade pipe line steel original austenite grain boundary corrosion agent and using method |
| CN109142010A (en) * | 2018-09-10 | 2019-01-04 | 中国石油天然气集团有限公司 | A kind of method of retained austenite distribution and content in detection low-alloy structural steel |
| CN109490300A (en) * | 2018-10-16 | 2019-03-19 | 包头钢铁（集团）有限责任公司 | The configuration method of reagent and the application method of reagent |
| CN111103183A (en) * | 2020-01-03 | 2020-05-05 | 中国石油天然气集团有限公司 | Method for displaying macroscopic morphology of high-steel-grade pipeline circumferential weld in multiple ways |
| CN111141577A (en) * | 2019-12-31 | 2020-05-12 | 江苏共昌轧辊股份有限公司 | Coating method of colored gold interference film |
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| CN104236980A (en) * | 2014-09-30 | 2014-12-24 | 钢铁研究总院 | Retained austenite contained dual phase steel color metallography coloring agent and coloring display method |
| 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 |
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| CN109142010A (en) * | 2018-09-10 | 2019-01-04 | 中国石油天然气集团有限公司 | A kind of method of retained austenite distribution and content in detection low-alloy structural steel |
| 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 |
| CN109490300A (en) * | 2018-10-16 | 2019-03-19 | 包头钢铁（集团）有限责任公司 | The configuration method of reagent and the application method of reagent |
| 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 |
| CN111141577A (en) * | 2019-12-31 | 2020-05-12 | 江苏共昌轧辊股份有限公司 | Coating method of colored gold interference film |
| CN111103183A (en) * | 2020-01-03 | 2020-05-05 | 中国石油天然气集团有限公司 | Method for displaying macroscopic morphology of high-steel-grade pipeline circumferential weld in multiple ways |
| CN111103183B (en) * | 2020-01-03 | 2022-06-03 | 中国石油天然气集团有限公司 | Method for displaying macroscopic morphology of high-steel-grade pipeline circumferential weld in multiple ways |
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