CN101984334B - Method for displaying metallurgical structure of interstitial-free steel by ultralow-carbon cold roll annealing - Google Patents
Method for displaying metallurgical structure of interstitial-free steel by ultralow-carbon cold roll annealing Download PDFInfo
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Abstract
The invention relates to a method for displaying the metallurgical structure of ultralow-carbon cold roll annealed interstitial-free steel, which belongs to the technical field of physical detection. The invention is used for realizing the aims of clear display and easy operation of the metallurgical structure of ultralow-carbon cold roll annealed interstitial-free steel. The method comprises the following steps: a. coarse grinding; b. polishing; c. erosion by a first reagent: eroding the polished sample in the first reagent for 10-20 seconds, wherein the first reagent is 5.5-6.5% nitric acidalcohol; d. erosion by a second reagent: eroding the sample in the second reagent immediately after taking out the sample from the first reagent, until the sample surface is evenly black, wherein the second reagent is prepared from 3-7g of sodium pyrosulfite, 9-12g of anhydrous sodium thiosulfate and 70-100ml of distilled water; and e. sample detection: wiping the sample with the first reagent tore move black on the surface, rinsing with alcohol, and blow-drying so that people can observe the sample. The method has the advantages of simpleness, simplified steps, easy master, resource conservation and high efficiency; the obtained structure has the advantages of clear grain boundary and no double grain boundary, and can properly reflect the annealing situation; and thus, the method is very suitable for field usage, and performs important functions on reasonably controlling technological parameters and ensuring product performance in the production field.
Description
Technical field
Type of the present invention relates to a kind of metallographic structure explicit representation, and method that particularly can the metallographic structure of clear demonstration ultra-low carbon cold-rolling annealed gapless atomic steel belongs to the physical detection technical field.
Technical background
The metallographic structure of ultra-low carbon cold-rolling annealed gapless atomic steel directly influences the performance of steel; Especially the form of ferrite crystal grain can reflect directly that with size the performance of steel is fine or not; And can directly reflect the situation that Zhao Shi anneals; Situation is organized in metallographic structure through analyzing the ultra-low carbon cold-rolling annealed gapless atomic steel, and rationally the CONTROL PROCESS parameter makes the performance of steel reach best.But; The metallographic structure of ultra-low carbon cold-rolling annealed gapless atomic steel shows it is a difficult problem in actual production all the time; Present many enterprises also adopt traditional with 4% nital as etchant, to the method that test specimen corrodes, this conventional method is if erosion time is short; The metallographic structure that obtains is as shown in Figure 1, organizes crystal grain not show fully; If the erosion time lengthening, crystal boundary can not show clear fully, also the twin boundary phenomenon can occur sometimes, and its metallographic structure is referring to Fig. 2.Because this method can not correctly reflect the form and the size of ferrite crystal grain, influence observation, thereby can not reliable information be provided for production to annealed structure.
Also have several method to show the metallographic structure of ultra-low carbon cold-rolling annealed gapless atomic steel at present, one Chinese patent application 97100731.4 discloses a kind of " method for displaying metallographic structure of cold rolled annealed gapless atomic steel ", and the method adopts two kinds of reagent that sample is corroded; But, second kind of reagent needs earlier sample to be carried out 3-6 time polishing repeatedly before corroding; Operating process is loaded down with trivial details consuming time, and operating personnel are not easy to grasp, even so; Can not guarantee sample preparation success, poor operability.One Chinese patent application 97119946.9 discloses a kind of " method for displaying metallographic structure of cold rolled annealed gapless atomic steel "; The method also is to adopt two kinds of reagent that sample is corroded, but before erosion earlier preparation hydrogen peroxide 30-45%, oxalic acid 1.5-10%, hydrofluorite 0.1-1%, all the other carry out wiping for the reagent of water to sample, with the removal interfere with layer; And then advance to corrode; This kind method needs the preparation plurality of reagents, has complex operation equally; Expense is high, the problem of poor operability.Therefore seek the method for displaying metallographic structure of a kind of simple, economical and practical ultra-low carbon cold-rolling annealed gapless atomic steel, very necessary for instructing produced on-site.
Summary of the invention
Problem to be solved by this invention be overcome the defective of prior art and provide a kind of simple to operate, organize crystal boundary ultra-low carbon cold-rolling annealed gapless atomic steel method for displaying metallographic structure clearly.
The alleged problem of the present invention is that following technical scheme solves:
A kind of ultra-low carbon cold-rolling annealed gapless atomic steel method for displaying metallographic structure, its special feature is: it carries out according to following steps:
A. corase grind: sample roughly ground to the surface polisher polish;
B. polishing: sample successively at 280#-320#-400#-600#-800# coated abrasive working, is polished through buffing machine again;
C. reagent one corrodes: will polish sample and insert erosion 10-20 second in the reagent one, said reagent one is that volumn concentration (down together) is the nitric acid alcohol of 5.5-6.5%;
D. reagent two corrodes: sample is put into reagent two erosions immediately by taking out in the reagent one; Be uniform black to specimen surface, said reagent two proportionings are following: the distilled water of 3-7 gram Sodium Metabisulfite, 9-12 gram Sodium Thio Sulphate(Anhydrous), 70-100 milliliter;
E. sample detects: the sample that will pass through reagent two erosions is extremely clean with reagent one wipe surfaces, rinses well with alcohol again, then dries up, and can observe grain structure.
Above-mentioned ultra-low carbon cold-rolling annealed gapless atomic steel method for displaying metallographic structure, erosion time is 30-80 second in the said d step, said reagent two is promptly joined promptly and is used.
The present invention is directed to the metallographic structure of present ultra-low carbon cold-rolling annealed gapless atomic steel does not still have the method problem of clear display and easy operating and improves.Said method adopts two kinds of reagent that sample is carried out etchant, and wherein, reagent one is high concentration nitric acid alcohol; Reagent two is the solution that is mixed of Sodium Metabisulfite, Sodium Thio Sulphate(Anhydrous) and distilled water; Sample does not need steps such as wiping, polishing to get into reagent two erosions immediately after one short time of reagent corrodes, and to the uniform black of sample, uses reagent one wipe surfaces again; Remove black, clean back with the alcohol flushing dry up make can clear display organization crystal boundary sample.Method of operating of the present invention is simple, and operation steps is simplified, and is easy to grasp; Avoid repeatedly specimen erodes or polishing process are economized on resources, efficient is high; What obtain organizes crystal boundary clear, and does not have the twin boundary phenomenon, can the correct response annealing case; Be fit to very much on-the-spot the use, can play an important role for reasonable CONTROL PROCESS parameter in production scene and assurance properties of product.
Description of drawings
Fig. 1 corrodes as etchant for the nitric acid alcohol of employing 4%, and the short time is corroded resulting metallographic structure photo;
Fig. 2 corrodes resulting metallographic structure photo for a long time for the nitric acid alcohol of employing 4% corrodes as etchant;
The metallographic structure photo of Fig. 3 for obtaining according to the inventive method.
Embodiment
The inventive method is to grope to draw through experimental study repeatedly; This method is abandoned the step of sample being polished or needs the removal of obtain solution wiping in advance interfere with layer repeatedly; After employing is the erosion of 5.5-6.5% nitric acid alcohol short time by concentration; Directly insert in the reagent two that the distilled water by 3-7 gram Sodium Metabisulfite, 9-12 gram Sodium Thio Sulphate(Anhydrous), 70-100 milliliter is mixed and corrode, use reagent one again, dry up observation with the alcohol flushing with surperficial wiped clean.The sample that corrodes through reagent one directly immerses in the reagent two, and the nitric acid of remained on surface impels Sodium Metabisulfite WS decomposition in the reagent two, emits SO
2, H
2S and H
2SO
2Can eliminate the passivation on surface, sodium thiosulfate is catalyzer, impels reaction to accelerate.The first step corrodes the Fe that generates
++Can directly participate in following reaction, Fe
+++ H
2S → FeS ↓, further reaction takes place in crystal boundary, and it is recessed to form ditch, and iron protosulfide forms black thin film at specimen surface simultaneously.The sample that the surface occurs black thin film is directly used reagent one wiping, and reaction: FeS+2HNO as follows takes place
3→ Fe (NO
3)
2+ H
2S ↑, black iron protosulfide film is removed fully, make specimen surface totally noiseless, be convenient to observe.
For making sample can show grain structure clearly, sample corrodes to need to become to polished surface in reagent two and is even black and exceeds, usually this process need 30-80 second.It is extremely clean with reagent one wipe surfaces to corrode good sample, rinses well with alcohol again, then dries up, and the grain structure that promptly can be observed cleaning is as shown in Figure 3.Be guaranteeing that erosion effect, reagent two need promptly be joined promptly uses.
Below provide several specific embodiments
Embodiment 1: with the ultra-low carbon cold-rolling annealed gapless atomic steel (weight percentage is C0.004, Mn:017, S:0.0016, P:0.012, Si:0.012, Als:0.028, O:0.0050, N:0.0012 Ti0.008) processes metallographic specimen; Sample roughly ground to the surface polisher polish, then successively at 280#-320#-400#-600#-800# coated abrasive working, the buffing machine polishing; To polish sample and insert in the reagent one and to corrode 10 seconds, reagent one is 6% nitric acid alcohol; To pass through sample that reagent one corrodes and insert to corrode in the reagent two to specimen surface and be even black, the time is 30 seconds, and said reagent two proportionings are following: 7 gram Sodium Metabisulfites, 11 gram Sodium Thio Sulphate(Anhydrous)s, 100 milliliters distilled water; To pass through reagent two and corrode the sample taking-up, to clean, rinse well with alcohol again, then dry up, can observe grain structure with 6% nitric acid alcohol wipe surface.
Embodiment 2: ultra-low carbon cold-rolling annealed gapless atomic steel (weight percentage is C 0.004, Mn 0.18, S 0.017, P 0.012, Si0.012, Als 0.028, O 0.0050, N 0.0012, Ti 0.008) is processed metallographic specimen; Sample roughly ground to the surface polisher polish, then successively at 280#-320#-400#-600#-800# coated abrasive working, the buffing machine polishing; To polish sample and insert in the reagent one and to corrode 15 seconds, reagent one is 5.5% nitric acid alcohol; To pass through sample that reagent one corrodes and insert to corrode in the reagent two to specimen surface and be even black, the time is 30 seconds, and said reagent two proportionings are following: 3 gram Sodium Metabisulfites, 9 gram Sodium Thio Sulphate(Anhydrous)s, 70 milliliters distilled water; To pass through reagent two and corrode the sample taking-up, to clean, rinse well with alcohol again, then dry up, can observe grain structure with 5.5% nitric acid alcohol wipe surface.
Embodiment 3: ultra-low carbon cold-rolling annealed gapless atomic steel (weight percentage is C 0.004, Mn 017, S 0.016, P 0.012, Si 0.016, Als 0.021, O 0.0020, N 0.0012, Ti 0.008) is processed metallographic specimen; Sample roughly ground to the surface polisher polish, then successively at 280#-320#-400#-600#-800# coated abrasive working, the buffing machine polishing; To polish sample and insert in the reagent one and to corrode 20 seconds, reagent one is 6.5% nitric acid alcohol; To pass through sample that reagent one corrodes and insert to corrode in the reagent two to specimen surface and be even black, the time is 80 seconds, and said reagent two proportionings are following: 6 gram Sodium Metabisulfites, 12 gram Sodium Thio Sulphate(Anhydrous)s, 90 milliliters distilled water; To pass through reagent two and corrode the sample taking-up, to clean, rinse well with alcohol again, then dry up, can observe grain structure with 6.5% nitric acid alcohol wipe surface.
Claims (2)
1. ultra-low carbon cold-rolling annealed gapless atomic steel method for displaying metallographic structure, it is characterized in that: it carries out according to following steps: a. corase grind: sample is roughly ground to the surface polisher polished; B. polishing: sample successively at 280#-320#-400#-600#-800# coated abrasive working, is polished through buffing machine again; C. reagent one corrodes: will polish sample and insert erosion 10-20 second in the reagent one, said reagent one is the nitric acid alcohol of volumn concentration 5.5-6.5%; D. reagent two corrodes: sample is put into reagent two erosions immediately by taking out in the reagent one; Be uniform black to specimen surface, said reagent two proportionings are following: the distilled water of 3-7 gram Sodium Metabisulfite, 9-12 gram Sodium Thio Sulphate(Anhydrous), 70-100 milliliter; E. sample detects: the sample that will pass through reagent two erosions is extremely clean with reagent one wipe surfaces, rinses well with alcohol again, then dries up, and can observe grain structure.
2. ultra-low carbon cold-rolling annealed gapless atomic steel method for displaying metallographic structure according to claim 1 is characterized in that: erosion time is 30-80 second in the said d step, and said reagent two is promptly joined promptly and used.
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| CN103852358B (en) * | 2014-03-02 | 2015-12-02 | 首钢总公司 | The display packing of a kind of ultra low carbon IF thin plate metallographic structure |
| CN105823671B (en) * | 2016-06-12 | 2019-01-08 | 东北大学 | A kind of display methods of middle manganese automobile steel original austenite crystal prevention |
| CN107421797A (en) * | 2017-08-08 | 2017-12-01 | 宝钢集团新疆八钢铁有限公司 | The metallographic rapid detection method of ultra-low carbon cold-rolling plate |
| CN112461618B (en) * | 2019-09-09 | 2022-05-10 | 上海梅山钢铁股份有限公司 | Method for displaying metallographic structure of ultralow-carbon cold-rolled annealed interstitial-free steel plate |
| CN111458208A (en) * | 2020-03-25 | 2020-07-28 | 唐山钢铁集团有限责任公司 | Display method for distinguishing cold-rolled annealed multiphase steel structure |
| CN112504798A (en) * | 2020-11-02 | 2021-03-16 | 抚顺特殊钢股份有限公司 | Metallographic corrosive agent and corrosion method for high-alloy ultra-pure ultra-high strength steel |
| CN113358645B (en) * | 2021-05-12 | 2023-01-31 | 东南大学 | Etching agent suitable for displaying austenite grains of low-carbon low-alloy steel and display method thereof |
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| CN1054433C (en) * | 1997-10-30 | 2000-07-12 | 宝山钢铁(集团)公司 | Method for displaying metallographic structure of cold rolled annealed gapless atomic steel |
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Address after: 063016 Binhe Road, Hebei, Tangshan City, No. 9 Patentee after: River steel Limited by Share Ltd Tangshan branch Address before: 063016 Binhe Road, Hebei, Tangshan City, No. 9 Patentee before: Hebei Steel Co., Ltd., Tangshan Branch |