CN104483179A - Method for displaying original austenite grain boundaries of maraging stainless steel - Google Patents
Method for displaying original austenite grain boundaries of maraging stainless steel Download PDFInfo
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- CN104483179A CN104483179A CN201410706269.1A CN201410706269A CN104483179A CN 104483179 A CN104483179 A CN 104483179A CN 201410706269 A CN201410706269 A CN 201410706269A CN 104483179 A CN104483179 A CN 104483179A
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Abstract
The invention provides a method for displaying original austenite grain boundaries of maraging stainless steel. The displaying of the original austenite grain boundaries is completed by three steps, namely, preparing a sample, carrying out passivation treatment with concentrated nitric acid and carrying out electrolytic etching with concentrated nitric acid. The method comprises the following steps: firstly preparing the sample, grinding and polishing one surface of the sample and grinding the other surfaces of the sample; placing the polished sample in 55-65% (volume fraction) aqueous nitric acid solution and carrying out passivation treatment for 3-5 minutes; carrying out electrolytic etching on the sample at room temperature for 3-5 minutes by adopting stainless steel sheet as a cathode and the passivated sample as an anode at the electrolytic voltage of 5-8V; after the electrolysis, completely rinsing the sample with tap water, rinsing the sample with alcohol and carrying out blow-drying and then observing the clear and complete microstructure-interference-free original austenite grain boundaries under the microscope. The method has the advantages that after the passivation treatment, the grain boundaries are preferentially displayed as compared with microstructures; no residual etching products are caused; the voltage is relatively low and the etching end point is easy to control.
Description
Technical field
The invention belongs to technical field of metallographic detection, be specifically related to a kind of method utilizing the method display 0Cr17Ni4Cu4Nb martensite aged stainless steel original austenite crystal prevention of Passivation Treatment+electro-etching.
Background technology
Crystallite dimension is an important parameter of steel, and grain size directly affects the properties of steel, and therefore Display of Grain Boundary technology is requisite work in the PRODUCTION TRAITS process of steel.Martensite aged stainless steel possesses high strength and corrosion stability, has strict requirement to grain size, and therefore the display technique of martensite aged stainless steel original austenite crystal prevention is particularly important.
At present, the common etchant of martensite aged stainless steel is mainly high iron chloride+aqueous hydrochloric acid solution, nitrate aqueous acid, picric acid+hydrochloric acid+alcoholic solution, chloroazotic acid glycerine and hydrofluorite+aqueous solution of nitric acid totally five kinds, be mainly used to show martensitic stucture, Display of Grain Boundary effect is unsatisfactory.Particularly after tempering and timeliness, Display of Grain Boundary effect is more undesirable.Patent of invention " a kind of etching pit method of martensite martensite aged stainless steel " (application number: introduce 201110382713.5) and use red fuming nitric acid (RFNA)+concentrated hydrochloric acid solution method etch crystal boundary, but organize while Display of Grain Boundary and also can show.Therefore, a kind of Display of Grain Boundary method exploring martensite aged stainless steel is necessary.
Summary of the invention
The object of the present invention is to provide a kind of martensite aged stainless steel original austenite crystal prevention display packing, the method utilizes the method display martensite aged stainless steel original austenite crystal prevention of Passivation Treatment+electro-etching, and the deactivation matter used in invention, electrolytic solution are the aqueous solution of nitric acid that volume fraction is 55% ~ 65%.Adopt the method can solve the difficult problem of martensite aged stainless steel original austenite crystal prevention display, thus when the interference of eliminating tissue, effectively, complete display show crystal boundary.
The present invention specifically provides a kind of display packing of martensite aged stainless steel original austenite crystal prevention, it is characterized in that, complete original austenite crystal prevention display by sample preparation, Passivation Treatment, electro-etching three step, concrete steps are as follows:
(1) sample preparation: first cut aging state sample, sample plane is polished laggard row polishing, dries up after being polished to no marking;
(2) Passivation Treatment: the sample through polishing is placed in aqueous solution of nitric acid Passivation Treatment 3 ~ 5min that volume fraction is 55% ~ 65%;
(3) electro-etching: the sample through Passivation Treatment is carried out normal temperature electro-etching, using stainless steel substrates as negative electrode, passivation sample is as anode, and electrolytic solution is the aqueous solution of nitric acid used in step (2), Control of Voltage is at 5 ~ 8V, and time controling is at 3 ~ 5min; Dry up after sample wash is clean after electrolysis, can complete display be examined under a microscope and the original austenite crystal prevention of inorganization interference.
As preferred embodiment, when prepared by step (1) sample, by sample plane successively on 240#, 600#, 1000#, 2000# abrasive paper for metallograph by thick to smooth poliss, then use the diamond polishing liquid that granularity is W2.5 to carry out polishing, dry up after being polished to no marking; Meanwhile, in order to prevent sample with oxide skin in electro-etching process, pollute electrolytic solution, its lap of sample need polish through 240# abrasive paper for metallograph.
As preferred embodiment, during step (2) Passivation Treatment, sample is placed in the aqueous solution of nitric acid Passivation Treatment 4min that volume fraction is 60%; During step (3) electro-etching by Control of Voltage at 6V, time controling is at 4min.
As preferred embodiment, first with tap water, sample wash is clean after step (3) sample electrolysis, then dry up after specimen surface being rinsed with alcohol.
The display packing of martensite aged stainless steel original austenite crystal prevention of the present invention, is characterized in that: described martensite aged stainless steel is 0Cr17Ni4Cu4Nb martensite aged stainless steel (U.S. trade mark 17-4PH).17-4PH martensite aged stainless steel, not only possesses the high-strength tenacity that Maraging steel is excellent, and has the good decay resistance of stainless steel.
The technology of the present invention is contemplated that:
At present, martensite aged stainless steel original austenite crystal prevention display packing is generally chemical etching, and main etchant is all strong acid, as chloroazotic acid glycerine, hydrofluorite+aqueous solution of nitric acid, nitrate aqueous acid etc.But chemical etching easily forms the residual of etch product, pollutes specimen surface, causes etch face unlimpid.And oxidation rate is fast, and the use as picric acid+hydrochloric acid+alcoholic solution and chloroazotic acid glycerine needs rich experience and skill, not easily grasps fast for most beginner.Therefore, utilize electro-etching can solve the residual problem of etch product, and etch rates can be controlled by control voltage parameter.
Stainless steel electrolytic liquid is generally oxalic acid, chromic acid, aqueous solution of nitric acid etc., preferentially will show martensitic stucture when taking acid solution as electrolytic solution, and crystal boundary is not obvious.Therefore, martensitic stucture passivation can be made by Passivation Treatment, and then make crystal boundary display more preferential than martensitic stucture.
Practice shows: use volume fraction be the aqueous solution of nitric acid of 55%-65% as deactivation matter and electrolytic solution, can effectively, complete display ground show original austenite crystal prevention.The superiority of the method is mainly reflected in: after Passivation Treatment, and crystal boundary ratio organizes preferential display; Remaining without etch product; Voltage is lower, and etch terminal is easy to control.
Accompanying drawing explanation
The photo of Fig. 1 aging state 17-4PH martensite aged stainless steel successively after 60% aqueous solution of nitric acid Passivation Treatment 4min, 6V potential electrolysis etch 4min.
The photo of Fig. 2 aging state 17-4PH martensite aged stainless steel successively after 55% aqueous solution of nitric acid Passivation Treatment 5min, 5V potential electrolysis etch 5min.
The photo of Fig. 3 aging state 17-4PH martensite aged stainless steel successively after 65% aqueous solution of nitric acid Passivation Treatment 3min, 8V potential electrolysis etch 3min.
The photo of Fig. 4 aging state 17-4PH martensite aged stainless steel after 4% hydrofluorite+4% aqueous solution of nitric acid normal temperature chemical etching.
Fig. 5 aging state 17-4PH martensite aged stainless steel through 60% aqueous solution of nitric acid, the photo after 6V potential electrolysis etch 4min.
The photo of Fig. 6 aging state 17-4PH martensite aged stainless steel successively after 60% aqueous solution of nitric acid Passivation Treatment 1min, 6V potential electrolysis etch 4min.
The photo of Fig. 7 aging state 17-4PH martensite aged stainless steel successively after 60% aqueous solution of nitric acid Passivation Treatment 4min, 6V potential electrolysis etch 8min.
Embodiment
The present invention is described in detail by the following examples, wherein all embodiment steel and comparative example steel are through identical Forging Technology, condition of heat treatment is aging state, and chemical composition is: (C:0.015%, Cr:15.67%, Ni:4.56%, Cu:3.39%, Si:0.34%, Mn:0.41%, Nb:0.34%), method of the present invention is finally adopted to carry out etch.
Embodiment 1
The photo of aging state 17-4PH martensite aged stainless steel successively after 60% aqueous solution of nitric acid Passivation Treatment 4min, 6V potential electrolysis etch 4min as shown in Figure 1.
1, sample preparation: first cut aging state sample, by one of them plane of sample successively on 240#, 600#, 1000#, 2000# abrasive paper for metallograph by thick to smooth poliss, then use the diamond polishing liquid that granularity is W2.5 to carry out polishing, dry up after being polished to no marking.Meanwhile, in order to prevent sample with oxide skin in electro-etching process, pollute electrolytic solution, its lap only need polish through 240# abrasive paper for metallograph.
2, Passivation Treatment: the sample through polishing is placed in the aqueous solution of nitric acid Passivation Treatment 4min that volume fraction is 60%;
3, electro-etching: the sample crossed through step 2 Passivation Treatment is carried out normal temperature electro-etching, using stainless steel substrates as negative electrode, passivation sample is as anode.Electrolytic solution is the aqueous solution of nitric acid used in step 2, and Control of Voltage is at 6V, and time controling is at 4min.With tap water, sample wash is clean after electrolysis, then dry up after specimen surface being rinsed with alcohol, can examine under a microscope complete display and the original austenite crystal prevention of inorganization interference, in accompanying drawing 1, larger-size dark structure is ferritic structure.
Embodiment 2
The photo of aging state 17-4PH martensite aged stainless steel successively after 55% aqueous solution of nitric acid Passivation Treatment 5min, 5V potential electrolysis etch 5min as shown in Figure 2.
1, sample preparation: with embodiment 1.
2, Passivation Treatment: passivating dip is the aqueous solution of nitric acid of 55%, the time is 5min
3, electro-etching: electro-etching solution is the aqueous solution of nitric acid of 55%, voltage is 5V, and the time is 5min.Can be observed complete display under the microscope and the original austenite crystal prevention of inorganization interference, larger-size dark structure is ferritic structure.
Embodiment 3
The photo of aging state 17-4PH martensite aged stainless steel successively after 65% aqueous solution of nitric acid Passivation Treatment 3min, 8V potential electrolysis etch 3min as shown in Figure 3.
1, sample preparation: with embodiment 1.
2, Passivation Treatment: passivating dip is the aqueous solution of nitric acid of 65%, the time is 3min
3, electro-etching: electro-etching solution is the aqueous solution of nitric acid of 65%, voltage is 8V, and the time is 3min.Can be observed complete display under the microscope and the original austenite crystal prevention of inorganization interference, larger-size dark structure is ferritic structure.
Comparative example 1
The photo of aging state 17-4PH martensite aged stainless steel after 4% hydrofluorite+4% aqueous solution of nitric acid normal temperature chemical etching as shown in Figure 4
1, sample preparation: with embodiment 1
2, chemical etching: the sample through polishing is carried out normal temperature chemical etching, polished surface should perpendicular to beaker bottom surface.If the parallel beaker bottom surface of polished surface upwards, etch product can remain in surface, is unfavorable for microexamination.Etching solution is 4% hydrofluorite+4% aqueous solution of nitric acid, and the judgement of etch terminal becomes silver gray with sample polished surface and is as the criterion.With tap water, sample wash is clean after etch, then dry up after specimen surface being rinsed with alcohol, examine under a microscope.As seen from the figure: after adopting 4% hydrofluorite+4% aqueous solution of nitric acid chemical etching, examine under a microscope the vestige that can recognize crystal boundary, but be almost all tissue, effectively can not grade to grain size, in accompanying drawing 4, larger-size white tissues is ferritic structure.
Comparative example 2
Aging state 17-4PH martensite aged stainless steel is through 60% aqueous solution of nitric acid, and the photo after 6V potential electrolysis etch 4min as shown in Figure 5.1, sample preparation: with embodiment 1
2, electro-etching:
Electro-etching solution is the aqueous solution of nitric acid of 60%, and voltage is 6V, and the time is 4min.As seen from the figure: examining under a microscope is all typical martensite lath tissue, can recognize the vestige of crystal boundary.Compare with embodiment, after having lacked red fuming nitric acid (RFNA) Passivation Treatment, organize comparatively crystal boundary preferentially to show, cannot grain size grading be carried out.
Comparative example 3
The photo of aging state 17-4PH martensite aged stainless steel successively after 60% aqueous solution of nitric acid Passivation Treatment 1min, 6V potential electrolysis etch 4min as shown in Figure 6.
1, sample preparation: with embodiment 1.
2, Passivation Treatment: passivating dip is the aqueous solution of nitric acid of 60%, the time is 1min
3, electro-etching: electro-etching solution is the aqueous solution of nitric acid of 60%, voltage is 6V, and the time is 4min.
As seen from the figure: examine under a microscope original austenite crystal prevention that is clear and inorganization interference, but crystal boundary is imperfect, much tiny crystal grain does not show, and stain is more.Compare with embodiment 1, in red fuming nitric acid (RFNA), the Passivation Treatment time is relatively short, and Display of Grain Boundary is imperfect, cannot carry out grain size grading.
Comparative example 4
The photo of aging state 17-4PH martensite aged stainless steel successively after 60% aqueous solution of nitric acid Passivation Treatment 4min, 6V potential electrolysis etch 8min as shown in Figure 7.
1, sample preparation: with embodiment 1.
2, Passivation Treatment: passivating dip is the aqueous solution of nitric acid of 60%, the time is 4min
3, electro-etching: electro-etching solution is the aqueous solution of nitric acid of 60%, voltage is 6V, and the time is 8min.As seen from the figure: the original austenite crystal prevention examining under a microscope complete display, but there is martensitic stucture to disturb, be unfavorable for that grain size is graded.
Above-described embodiment, only for technical conceive of the present invention and feature are described, its object is to person skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences done according to Spirit Essence of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (6)
1. a display packing for martensite aged stainless steel original austenite crystal prevention, is characterized in that, complete original austenite crystal prevention display by sample preparation, Passivation Treatment, electro-etching three step, concrete steps are as follows:
(1) sample preparation: first cut aging state sample, sample plane is polished laggard row polishing, dries up after being polished to no marking;
(2) Passivation Treatment: the sample through polishing is placed in aqueous solution of nitric acid Passivation Treatment 3 ~ 5min that volume fraction is 55% ~ 65%;
(3) electro-etching: the sample through Passivation Treatment is carried out normal temperature electro-etching, using stainless steel substrates as negative electrode, passivation sample is as anode, and electrolytic solution is the aqueous solution of nitric acid used in step (2), Control of Voltage is at 5 ~ 8V, and time controling is at 3 ~ 5min; Dry up after sample wash is clean after electrolysis, can complete display be examined under a microscope and the original austenite crystal prevention of inorganization interference.
2. according to the display packing of martensitic stain less steel original austenite crystal prevention described in claim 1, it is characterized in that: when prepared by step (1) sample, by sample plane successively on 240#, 600#, 1000#, 2000# abrasive paper for metallograph by thick to smooth poliss, then use the diamond polishing liquid that granularity is W2.5 to carry out polishing, dry up after being polished to no marking; Its lap of sample polishes through 240# abrasive paper for metallograph.
3. according to the display packing of martensite aged stainless steel original austenite crystal prevention described in claim 1, it is characterized in that: during step (2) Passivation Treatment, sample is placed in the aqueous solution of nitric acid Passivation Treatment 4min that volume fraction is 60%.
4., according to the display packing of martensite aged stainless steel original austenite crystal prevention described in claim 1, it is characterized in that: during step (3) electro-etching by Control of Voltage at 6V, time controling is at 4min.
5. according to the display packing of martensite aged stainless steel original austenite crystal prevention described in claim 1, it is characterized in that: first with tap water, sample wash is clean after step (3) sample electrolysis, then dry up after specimen surface being rinsed with alcohol.
6. according to the display packing of the arbitrary described martensite aged stainless steel original austenite crystal prevention of Claims 1 to 5, it is characterized in that: described martensite aged stainless steel is 0Cr17Ni4Cu4Nb martensite aged stainless steel.
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| CN104977299A (en) * | 2015-06-19 | 2015-10-14 | 东方电气集团东方锅炉股份有限公司 | Method for displaying P91 and P92 ferrite heat-resistant steel original austenite crystal boundary |
| CN105606426A (en) * | 2015-12-18 | 2016-05-25 | 北京有色金属研究总院 | Metallurgical analysis etching method of layered metal composite material |
| CN105908249A (en) * | 2016-05-19 | 2016-08-31 | 河北工业大学 | Electrolytic corrosion method of stainless steel/carbon steel composite plate metallographic structure |
| CN107741452A (en) * | 2017-09-14 | 2018-02-27 | 浙江大学 | The method of testing of Martensite Volume Fraction in a kind of austenitic stainless steel |
| CN107741449A (en) * | 2017-09-14 | 2018-02-27 | 浙江大学 | The test device of Martensite Volume Fraction in austenitic stainless steel |
| CN109490302A (en) * | 2018-11-11 | 2019-03-19 | 上海电气上重铸锻有限公司 | A kind of test method of the austenite grain of midium-carbon steel martensitic structure |
| CN109632436A (en) * | 2018-12-14 | 2019-04-16 | 河钢股份有限公司 | A kind of EBSD test sample surface treatment method of high nitrogen stainless steel |
| CN110749718A (en) * | 2019-10-25 | 2020-02-04 | 成都先进金属材料产业技术研究院有限公司 | Dendritic crystal corrosive agent and corrosion method for maraging stainless steel |
| CN112213171A (en) * | 2020-10-22 | 2021-01-12 | 昆明理工大学 | Corrosion display method for original austenite grain boundary of S34MnV steel |
| CN112730003A (en) * | 2020-12-21 | 2021-04-30 | 安徽工业大学 | Metallographic corrosion method for delta-ferrite in 2Cr13 martensitic stainless steel continuous casting billet |
| CN112730004A (en) * | 2020-12-21 | 2021-04-30 | 安徽工业大学 | Metallographic corrosion method for delta-ferrite in 1Cr13 martensitic stainless steel |
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| CN113670698A (en) * | 2021-07-12 | 2021-11-19 | 包头钢铁（集团）有限责任公司 | Austenite steel metallographic etchant and display method |
| CN113862767A (en) * | 2021-08-30 | 2021-12-31 | 东方电气(广州)重型机器有限公司 | Electrolytic corrosion method of austenitic stainless steel and application thereof |
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