CN104532242A - Austenitic stainless steel metallography corrosion agent and austenitic stainless steel metallography display method - Google Patents
Austenitic stainless steel metallography corrosion agent and austenitic stainless steel metallography display method Download PDFInfo
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Abstract
The invention provides an austenitic stainless steel metallography corrosion agent with good erosion effect, and an austenitic stainless steel metallography display method. The corrosion agent has the advantages of simple preparation, convenient operation and small pollution, and the display method had the advantages of good stability and reappearance, and rapid, uniform and clear display of the microstructure. The display method comprises the following steps: mixing 1 part by volume of nitric acid with the mass concentration of 65-68% with 3 parts by volume of hydrochloric acid with the mass concentration of 36-38%, 1.5-3 parts by volume of acetic acid with the mass concentration of 36% and 1 part by volume of hydrofluoric acid with the mass concentration of 40% or more, slightly stirring by using a stirring bar for 20s, standing for 30min to prepare the corrosion agent; immersing a polished austenitic stainless steel sample in the corrosion agent, making the corrosion surface of the sample vertical to the surface of the corrosion agent during immersion, slightly stirring the sample, and allowing the sample to be immersed for 35-60s until the corrosion surface is argenteous; and taking out the immersed sample, flushing by using clear water, carrying out spray washing by using anhydrous ethanol, and carrying out blow drying to obtain the austenitic stainless steel structure to be observed.
Description
Technical field
The present invention relates to a kind of etching reagent and display packing of austenitic stainless steel metallographic, be specially adapted to 316,316L austenitic stainless steel.
Background technology
Austenitic stainless steel is a most important class in stainless steel family, because it is anti-corrosion, and good normal temperature and low temperature plasticity and toughness, formability and good weldability and be widely used in each industrial circle and current consumption field.The output of austenitic stainless steel accounts for 70% of stainless steel output, the metallurgic product type that its product culvert cover plate, pipe, silk, band, excellent silk, forging etc. are nearly all.
In the research of austenitic stainless steel, its composition and processing and heat treatment technique determine its organization type, and then determine its performance.For obtaining required austenitic stainless steel, need to analyze austenitic stainless steel structure and properties, in time adjustment its composition, processing and heat treatment technique, prerequisite is exactly adopt suitable etching reagent to show its metallographic structure.
Consult disclosed documents and materials and patent at present, more or less there is the problem of some following aspects in usual 316L austenitic stainless steel etching reagent: 1, reaction is violent, the bad grasp of etching time, and tissue corrosion is uneven; 2, etching reagent less stable, circulation ratio is bad; 3, prepare or operate more complicated; 4, twin interference grain fineness number grading in tissue is during especially for resection grading and metallographic software grading, larger to Influence on test result.The such as publication number etching reagent that to be the patent of invention of CN102517585A be is component with hydrochloric acid, glycerol, nitric acid and hydrogen peroxide, though it meets the object of display organization, but come with some shortcomings: its component hydrogen peroxide is strong oxidizer, now with the current, etching reagent less stable, can not long-term storage; Etching time is longer, from several minutes to dozens of minutes; After corrosion, in metallographic structure, contraction crystalline substance is more, the grading of interference grain fineness number.The invention solves the problem of more above-mentioned display austenitic stainless steel etching reagent, have important improved action and realistic meaning to materials microstructure analysis.
Summary of the invention
The object of the invention is to overcome above shortcomings in prior art, and the etching reagent of the austenitic stainless steel metallographic providing a kind of erosion effect good and display packing, and prepare simple, easy to operate, pollute little, stability and favorable reproducibility, and can quick, even, clear display metallographic structure.
The present invention's adopted technical scheme that solves the problem is:
A kind of etching reagent of austenitic stainless steel metallographic, it is characterized in that: by volume number consists of: mass concentration is 1 part, the nitric acid of 65% ~ 68%, mass concentration is the hydrochloric acid 3 parts of 36% ~ 38%, and mass concentration is the acetic acid 1.5 ~ 3 parts of 36%, mass concentration be not less than 40% 1 part, hydrofluoric acid.
The number of acetic acid of the present invention is the one in 1.6 parts, 1.7 parts, 1.8 parts, 1.9 parts, 2.0 parts, 2.1 parts, 2.2 parts, 2.3 parts, 2.4 parts, 2.5 parts, 2.6 parts, 2.7 parts, 2.8 parts and 2.9 parts.
The mass concentration of nitric acid of the present invention is the one in 65%, 65.5%, 66%, 66.5%, 67%, 67.5% and 68%.
The mass concentration of hydrochloric acid of the present invention is the one in 36.2%, 36.4%, 36.6%, 36.8%, 37%, 37.2%, 37.4%, 37.6%, 37.8% and 38%.
The mass concentration of hydrofluoric acid of the present invention is the one in 40%, 42%, 44%, 46%, 48%, 50%, 52%, 54%, 56%, 58% and 60%.
A metallographic phase display method for austenitic stainless steel, is characterized in that: comprise the steps:
Acetic acid, hydrochloric acid, nitric acid, hydrofluoric acid are mixed successively, stirs gently by stirring rod and leave standstill 30 minutes afterwards in 20 seconds, be configured to above-mentioned etching reagent;
Immersed by polished austenite stainless steel sample in the etching reagent configured, during immersion, sample erosional surface is vertical with corrosion liquid level, and stirs sample gently, and the etch time is 35 ~ 60 seconds, becomes silver gray to be advisable with erosional surface; The complete taking-up of etch, rinse with clear water, dehydrated alcohol hydro-peening dries up, and namely obtains the austenite stainless structure of steel that will observe.
During polishing austenite stainless steel sample of the present invention, carried out grinding successively in austenitic stainless steel sample survey face and be polished to no marking minute surface with 180#, 600#, 800#, 1000#, 1200# waterproof abrasive paper, then rinsing with clear water, then dehydrated alcohol hydro-peening dries up.
The etch time of the present invention is the one in 40 seconds, 45 seconds and 50 seconds.
The present invention compared with prior art, has the following advantages and effect: 1, simple to operate, and corrosion inhibitor component is easy to obtain, with low cost, and preparation is convenient; 2, consuming time few, stability and favorable reproducibility; 3, normal temperature can carry out; 4, crystal boundary is clear, and etching reagent is less to tissue interference, and corrosive effect is good.
Accompanying drawing explanation
Fig. 1 is the micro-organization chart of 316L austenitic stainless steel after the embodiment of the present invention 1 is corroded.
Fig. 2 is the micro-organization chart of 316L austenitic stainless steel after the embodiment of the present invention 2 is corroded.
Fig. 3 is the micro-organization chart of 316L austenitic stainless steel after the embodiment of the present invention 3 is corroded.
Fig. 4 is the micro-organization chart of 316L austenitic stainless steel after the embodiment of the present invention 4 is corroded.
Embodiment
Below in conjunction with accompanying drawing, also by embodiment, the present invention is described in further detail, and following examples are explanation of the invention and the present invention is not limited to following examples.
I, see Fig. 1 ~ Fig. 4, the purity level of the nitric acid in following examples, hydrochloric acid, acetic acid, hydrofluoric acid is analytical pure, and the mass concentration of nitric acid is 65% ~ 68%, the mass concentration of hydrochloric acid is 36% ~ 38%, the mass concentration of acetic acid is 36%, the mass concentration of hydrofluoric acid is for being not less than 40%.
One, embodiment 1:
Preparation: under normal temperature, successively 46.5ml acetic acid, 93ml hydrochloric acid, 31ml nitric acid and 31ml hydrofluoric acid are poured in plastic cup, stir 20 seconds by stirring rod, and leave standstill 30 minutes, be mixed with etching reagent.Namely etching reagent by volume number consist of: 1 part, nitric acid, hydrochloric acid 3 parts, acetic acid 1.5 parts, 1 part, hydrofluoric acid.
Sample preparation: be polished to minute surface after being ground with 180#, 600#, 800#, 1000#, 1200# waterproof abrasive paper successively in 316L austenitic stainless steel sample survey face, then rinse with clear water, dehydrated alcohol hydro-peening dries up.
Corrosion display: with the clamping of bamboo tweezer, austenite stainless steel sample after polishing is immersed in the metallographic etching agent configured, during immersion, sample erosional surface is vertical with corrosion liquid level, and stir sample gently, the etch time is 40 seconds, becomes silver gray to be advisable with erosional surface, the complete taking-up sample of etch, rinse with clear water, dehydrated alcohol hydro-peening dries up, and namely obtains the austenite stainless structure of steel that will observe.
Two, embodiment 2:
Preparation: under normal temperature, successively 57ml acetic acid, 87ml hydrochloric acid, 29ml nitric acid and 29ml hydrofluoric acid are poured in plastic cup, stir 20 seconds by stirring rod, and leave standstill 30 minutes, be mixed with etching reagent.Namely etching reagent by volume number consist of: 1 part, nitric acid, hydrochloric acid 3 parts, acetic acid about 1.97 parts, 1 part, hydrofluoric acid.
Sample preparation: be polished to minute surface after being ground with 180#, 600#, 800#, 1000#, 1200# waterproof abrasive paper successively in 316L austenitic stainless steel sample survey face, then rinse with clear water, dehydrated alcohol hydro-peening dries up.
Corrosion display: with the clamping of bamboo tweezer, austenite stainless steel sample after polishing is immersed in the metallographic etching agent configured, during immersion, sample erosional surface is vertical with corrosion liquid level, and stir sample gently, the etch time is 45 seconds, becomes silver gray to be advisable with erosional surface, the complete taking-up sample of etch, rinse with clear water, dehydrated alcohol hydro-peening dries up, and namely obtains the austenite stainless structure of steel that will observe.
Three, embodiment 3:
Preparation: under normal temperature, successively 67ml acetic acid, 81ml hydrochloric acid, 27ml nitric acid and 27ml hydrofluoric acid are poured in plastic cup, stir 20 seconds by stirring rod, and leave standstill 30 minutes, be mixed with etching reagent.Namely etching reagent by volume number consist of: 1 part, nitric acid, hydrochloric acid 3 parts, acetic acid about 2.48 parts, 1 part, hydrofluoric acid.
Sample preparation: be polished to minute surface after being ground with 180#, 600#, 800#, 1000#, 1200# waterproof abrasive paper successively in 316L austenitic stainless steel sample survey face, then rinse with clear water, dehydrated alcohol hydro-peening dries up.
Corrosion display: with the clamping of bamboo tweezer, austenite stainless steel sample after polishing is immersed in the metallographic etching agent configured, during immersion, sample erosional surface is vertical with corrosion liquid level, and stir sample gently, the etch time is 50 seconds, becomes silver gray to be advisable with erosional surface, the complete taking-up sample of etch, rinse with clear water, dehydrated alcohol hydro-peening dries up, and namely obtains the austenite stainless structure of steel that will observe.
Four, embodiment 4:
Preparation: under normal temperature, successively 75ml acetic acid, 75ml hydrochloric acid, 25ml nitric acid and 25ml hydrofluoric acid are poured in plastic cup, stir 20 seconds by stirring rod, and leave standstill 30 minutes, be mixed with etching reagent.Namely etching reagent by volume number consist of: 1 part, nitric acid, hydrochloric acid 3 parts, acetic acid about 3 parts, 1 part, hydrofluoric acid.
Sample preparation: be polished to minute surface after being ground with 180#, 600#, 800#, 1000#, 1200# waterproof abrasive paper successively in 316L austenitic stainless steel sample survey face, then rinse with clear water, dehydrated alcohol hydro-peening dries up.
Corrosion display: with the clamping of bamboo tweezer, austenite stainless steel sample after polishing is immersed in the metallographic etching agent configured, during immersion, sample erosional surface is vertical with corrosion liquid level, and stir sample gently, the etch time is 60 seconds, becomes silver gray to be advisable with erosional surface, the complete taking-up sample of etch, rinse with clear water, dehydrated alcohol hydro-peening dries up, and namely obtains the austenite stainless structure of steel that will observe.
Five, all the other embodiments:
Etching reagent by volume number composition can also be: nitric acid is 1 part, hydrochloric acid is 3 parts, hydrofluoric acid is 1 part, and acetic acid is then the one in 1.6 parts, 1.7 parts, 1.8 parts, 1.9 parts, 2.0 parts, 2.1 parts, 2.2 parts, 2.3 parts, 2.4 parts, 2.5 parts, 2.6 parts, 2.7 parts, 2.8 parts and 2.9 parts.
The mass concentration of II, nitric acid is the one in 65%, 65.5%, 66%, 66.5%, 67%, 67.5% and 68%.
The mass concentration of hydrochloric acid is the one in 36.2%, 36.4%, 36.6%, 36.8%, 37%, 37.2%, 37.4%, 37.6%, 37.8% and 38%.
The mass concentration of hydrofluoric acid is the one in 40%, 42%, 44%, 46%, 48%, 50%, 52%, 54%, 56%, 58% and 60%.
In addition, it should be noted that, the above-mentioned embodiment of the present invention is only for clearly illustrating that example of the present invention illustrates, and is not the restriction to embodiments of the present invention, specific embodiment described in this specification sheets, the shape, institute's title of being named etc. of its parts and components can be different.For those of ordinary skill in the field, other multi-form change and variations can also be made on the basis of the above description.Here cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.
Claims (8)
1. the etching reagent of an austenitic stainless steel metallographic, it is characterized in that: by volume number consists of: mass concentration is 1 part, the nitric acid of 65% ~ 68%, mass concentration is the hydrochloric acid 3 parts of 36% ~ 38%, and mass concentration is the acetic acid 1.5 ~ 3 parts of 36%, mass concentration be not less than 40% 1 part, hydrofluoric acid.
2. the etching reagent of austenitic stainless steel metallographic according to claim 1, is characterized in that: the number of described acetic acid is the one in 1.6 parts, 1.7 parts, 1.8 parts, 1.9 parts, 2.0 parts, 2.1 parts, 2.2 parts, 2.3 parts, 2.4 parts, 2.5 parts, 2.6 parts, 2.7 parts, 2.8 parts and 2.9 parts.
3. the etching reagent of austenitic stainless steel metallographic according to claim 1 and 2, is characterized in that: the mass concentration of described nitric acid is the one in 65%, 65.5%, 66%, 66.5%, 67%, 67.5% and 68%.
4. the etching reagent of austenitic stainless steel metallographic according to claim 1 and 2, is characterized in that: the mass concentration of described hydrochloric acid is the one in 36.2%, 36.4%, 36.6%, 36.8%, 37%, 37.2%, 37.4%, 37.6%, 37.8% and 38%.
5. the etching reagent of austenitic stainless steel metallographic according to claim 1 and 2, is characterized in that: the mass concentration of described hydrofluoric acid is the one in 40%, 42%, 44%, 46%, 48%, 50%, 52%, 54%, 56%, 58% and 60%.
6. a metallographic phase display method for austenitic stainless steel, is characterized in that: comprise the steps:
Acetic acid, hydrochloric acid, nitric acid, hydrofluoric acid are mixed successively, stirs gently by stirring rod and leave standstill 30 minutes afterwards in 20 seconds, be configured to the etching reagent described in the arbitrary claim of Claims 1 to 5;
Immersed by polished austenite stainless steel sample in the etching reagent configured, during immersion, sample erosional surface is vertical with corrosion liquid level, and stirs sample gently, and the etch time is 35 ~ 60 seconds, becomes silver gray to be advisable with erosional surface; The complete taking-up of etch, rinse with clear water, dehydrated alcohol hydro-peening dries up, and namely obtains the austenite stainless structure of steel that will observe.
7. the metallographic phase display method of austenitic stainless steel according to claim 6, it is characterized in that: during polishing austenite stainless steel sample, austenitic stainless steel sample survey face is carried out grinding with 180#, 600#, 800#, 1000#, 1200# waterproof abrasive paper successively and is polished to no marking minute surface, rinse with clear water, then dehydrated alcohol hydro-peening dries up again.
8. the metallographic phase display method of the austenitic stainless steel according to claim 6 or 7, is characterized in that: the described etch time is the one in 40 seconds, 45 seconds and 50 seconds.
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Cited By (8)
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| CN106245029A (en) * | 2016-07-08 | 2016-12-21 | 西安热工研究院有限公司 | Aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel shows, preparation method and application method |
| CN108036991A (en) * | 2017-11-29 | 2018-05-15 | 西部金属材料股份有限公司 | A kind of sample treatment of observing nuclear level silver-indium-cadmium control rod macrostructure |
| CN110453222A (en) * | 2019-08-08 | 2019-11-15 | 重庆科技学院 | Show the corrosive liquid and preparation method and application of super-high strength steel austenite grain boundary |
| CN110846664A (en) * | 2019-11-20 | 2020-02-28 | 哈尔滨哈锅锅炉工程技术有限公司 | Etching agent for austenitic stainless steel metallographic phase and display method |
| CN112695323A (en) * | 2020-12-10 | 2021-04-23 | 广西北部湾新材料有限公司 | Metallographic etchant for austenitic stainless steel cold-rolled sheet and sample corrosion method |
| CN113106465A (en) * | 2021-04-21 | 2021-07-13 | 西安瑞鑫科金属材料有限责任公司 | high-Cr corrosion-resistant stainless steel surface oxide film remover and film removing method |
| CN113295503A (en) * | 2021-05-28 | 2021-08-24 | 金川镍钴研究设计院有限责任公司 | Chemical polishing etching solution for MBA-2 copper alloy |
| CN113984473A (en) * | 2021-10-29 | 2022-01-28 | 唐山瑞丰钢铁（集团）有限公司 | Ultra-low carbon steel metallographic corrosive and display method of metallographic structure |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106245029A (en) * | 2016-07-08 | 2016-12-21 | 西安热工研究院有限公司 | Aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel shows, preparation method and application method |
| CN106245029B (en) * | 2016-07-08 | 2018-12-04 | 西安热工研究院有限公司 | Aggressive agent that the lasting sample tissue of Super304H austenitic stainless steel is shown, preparation method and application method |
| CN108036991A (en) * | 2017-11-29 | 2018-05-15 | 西部金属材料股份有限公司 | A kind of sample treatment of observing nuclear level silver-indium-cadmium control rod macrostructure |
| CN110453222A (en) * | 2019-08-08 | 2019-11-15 | 重庆科技学院 | Show the corrosive liquid and preparation method and application of super-high strength steel austenite grain boundary |
| CN110453222B (en) * | 2019-08-08 | 2021-07-13 | 重庆科技学院 | Corrosive liquid for displaying austenite grain boundary of ultrahigh-strength steel, and preparation method and application thereof |
| CN110846664A (en) * | 2019-11-20 | 2020-02-28 | 哈尔滨哈锅锅炉工程技术有限公司 | Etching agent for austenitic stainless steel metallographic phase and display method |
| CN112695323A (en) * | 2020-12-10 | 2021-04-23 | 广西北部湾新材料有限公司 | Metallographic etchant for austenitic stainless steel cold-rolled sheet and sample corrosion method |
| CN113106465A (en) * | 2021-04-21 | 2021-07-13 | 西安瑞鑫科金属材料有限责任公司 | high-Cr corrosion-resistant stainless steel surface oxide film remover and film removing method |
| CN113295503A (en) * | 2021-05-28 | 2021-08-24 | 金川镍钴研究设计院有限责任公司 | Chemical polishing etching solution for MBA-2 copper alloy |
| CN113984473A (en) * | 2021-10-29 | 2022-01-28 | 唐山瑞丰钢铁（集团）有限公司 | Ultra-low carbon steel metallographic corrosive and display method of metallographic structure |
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Application publication date: 20150422 |