CN101353794A - Austenitic stainless steel metallographic etchant, preparing method and use thereof - Google Patents
Austenitic stainless steel metallographic etchant, preparing method and use thereof Download PDFInfo
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- CN101353794A CN101353794A CNA2008100424342A CN200810042434A CN101353794A CN 101353794 A CN101353794 A CN 101353794A CN A2008100424342 A CNA2008100424342 A CN A2008100424342A CN 200810042434 A CN200810042434 A CN 200810042434A CN 101353794 A CN101353794 A CN 101353794A
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Abstract
The invention discloses a metallographic-phase aggressive agent of an austenitic stainless steel, a preparation method thereof and application thereof. The metallographic-phase aggressive agent comprises the mixed solution of hydrofluoric acid and nitric acid, calculated by volume ratio, the proportion of each component of the agent is that hydrofluoric acid : nitric acid : water is equal to 2 : 1 : 7. The preparation method thereof is carried out according to the following steps of: taking 70ml of water first, then taking 10ml of analytically pure nitric acid and finally taking 20ml of analytically pure hydrofluoric acid, which are then evenly mixed. The application method thereof comprises the following steps of: putting a simple of the austenitic stainless steel in the metallographic-phase aggressive agent of the austenitic stainless steel and observing the color change of the surface of the sample by time, taking out the sample of the austenitic stainless steel when metallographic-phase surface of the sample is corroded to darker silver gray, washing the sample with water which is then neutralized with alkaline solution and finally washing with water and absolute ethyl alcohol. The technical effects thereof are represented by good corrosion effect, clear austenite grain boundary, slow corrosion speed, easy control, no pollution and other aspects.
Description
Technical field
The present invention relates to a kind of austenitic stainless steel metallographic etchant, also relate to the compound method and the application of this austenitic stainless steel metallographic etchant simultaneously.
Background technology
Graphite phase in some non-metallic inclusion, cast iron, the particular tissues such as hole in the mmaterial, the sample flour milling after polishing must corrode with etchant, could observe at microscopically after the visual contrast of acquisition (or reinforcement).The method that obtains contrast is a lot, whether changes specimen surface according to obtaining the contrast process, can be divided into not changing surface method (as optical method) and changing specimen surface method (as electrochemical etching method, physics etch method) two big classes.
In the past, it is several that austenitic stainless steel metallographic etchant mainly contains chloroazotic acid, chloroazotic acid diluent, the FeCl3+HCl aqueous solution, the HNO3+HCl aqueous solution, the CuCl+HCl aqueous solution and picric acid+aqueous hydrochloric acid etc., and these etchants have following shortcoming:
1. for the austenitic stainless steel of solid solution weak effect, crystal boundary can not clearly show, only can make the part crystal boundary obtain to show;
2. the easy residual dirt of metallographic examination face after corroding makes examination face unclean, influences interpretation of result;
3. more shallow cut can not be removed, the impact analysis result;
4. the erosion operations complexity needs abundant working experience, need observe bubble and color as the chloroazotic acid wipe method, does not have the difficult grasp of certain experience.
The work experience of more than ten years also shows, it is the thing that vast metallographic worker generally shakes the head that the metallographic specimen of austenitic stainless steel is made, exactly because this work too difficulty do, many metallographic workers do not set foot in this project all one's life yet, are so difficult because the metallographic specimen of austenitic stainless steel is made exactly!
Summary of the invention
One of technical problem to be solved by this invention is, have at existing austenitic stainless steel metallographic etchant that crystal boundary is unintelligible, erosive velocity is too fast, the shortcoming that is not easy to control, a kind of new austenitic stainless steel metallographic etchant is provided, crystal boundary clearly can be accessed, and the grasp erosive velocity can well be controlled.
Two of technical problem to be solved by this invention is that a kind of compound method of preparing above-mentioned austenitic stainless steel metallographic etchant is provided.
Three of technical problem to be solved by this invention is that the application method of above-mentioned austenitic stainless steel metallographic etchant is provided.
A kind of austenitic stainless steel metallographic etchant, by the mixing solutions of hydrofluoric acid and nitric acid, metering by volume, the ratio of each component is respectively: hydrofluoric acid: nitric acid: water=2: 1: 7.
A kind of compound method at austenitic stainless steel metallographic etchant follows these steps to carry out: 1) measure 70 ml waters with glass measure, pour in the plastics liquid storage bottle; 2) measure 10 milliliters in analytical pure nitric acid with plastic measuring glass, pour in the described plastics liquid storage bottle, and shake up; 3) measure 20 milliliters of analytical pure hydrofluoric acid with plastic measuring glass again, pour mixing in the described plastics liquid storage bottle into.
A kind of application of austenitic stainless steel metallographic etchant, operate by following method: 1) clamp the qualified austenitic stainless steel metallographic specimen of polishing and put into austenitic stainless steel metallographic etchant with bamboo tweezers, make metallographic examination face immerse in the liquid fully, examination is towards last or side direction, and the variation of examination face look is observed in timing; When 2) treating that metallographic examination face is etched to darker silver gray, take out the austenitic stainless steel metallographic specimen, fully clean with the mobile tap water earlier at once with bamboo tweezers; 3) again the austenitic stainless steel metallographic specimen is immersed the neutralization of carrying out remaining acid in the alkaline solution; 4) in the alkali lye and after again water fully wash; 5) clean with dehydrated alcohol at last.
Above-mentioned alkaline solution is Carbon Dioxide saturated aqueous solution of sodium or aqueous sodium hydroxide solution.Also can be other alkaline solution.
Technique effect of the present invention is significantly outstanding:
1. austenite grain boundary can obtain the utmost point and shows clearly, makes erosion effect splendid, especially also can farthest obtain to show to relatively poor its crystal boundary of austenitic stainless steel of solid solution effect;
2. erosive velocity is slow, makes erosion effect be easy to control.The erosion time of this etchant can be distributed in 0 to 60min scope, and when the austenitic stainless steel solid solution was effective, erosion time was in 20 to 40min scopes; When the solid solution effect after the relatively poor or solution treatment through tempering and other mode heat treated, erosion time is at least more than several minutes;
3. do not have the pollution that corrosion products is brought through this etchant erosive metallographic examination face, the soluble in water and rapid diffusion of the corrosion products of formation can not residue on the metallographic examination face in water, makes erosion effect the best;
4. this etchant also has certain chemical rightenning effect, when more shallow cut is arranged on the examination face, can cut is etched by slowly corroding for a long time, thereby reach the effect of chemical rightenning;
5. can arbitrarily adjust erosion effect, when carrying out that the degree of depth corrodes and when obtaining the crystal boundary of broad, to austenite grain boundary as long as prolong erosion time; Otherwise,, then only need to shorten erosion time if need carry out shallow erosion and be convenient to observe residual ferrite or other phase to crystal boundary;
6. pass through to use alkali lye neutral purging method, but the murder by poisoning of hydrofluoric acid avoided to human body, although allow the operator use relievedly.
Embodiment
A kind of austenitic stainless steel metallographic etchant, by the mixing solutions of hydrofluoric acid and nitric acid, metering by volume, the ratio of each component is respectively: hydrofluoric acid: nitric acid: water=2: 1: 7.
A kind of compound method at austenitic stainless steel metallographic etchant follows these steps to carry out: 1) measure 70 ml waters with glass measure, pour in the plastics liquid storage bottle; 2) measure 10 milliliters in analytical pure nitric acid with plastic measuring glass, pour in the described plastics liquid storage bottle, and shake up; 3) measure 20 milliliters of analytical pure hydrofluoric acid with plastic measuring glass again, pour mixing in the described plastics liquid storage bottle into.
A kind of application of austenitic stainless steel metallographic etchant, operate by following method: 1) clamp the qualified austenitic stainless steel metallographic specimen of polishing and put into austenitic stainless steel metallographic etchant with bamboo tweezers, make metallographic examination face immerse in the liquid fully, examination is towards last or side direction, and the variation of examination face look is observed in timing; When 2) treating that metallographic examination face is etched to darker silver gray, take out the austenitic stainless steel metallographic specimen, fully clean with the mobile tap water earlier at once with bamboo tweezers; 3) again the austenitic stainless steel metallographic specimen is immersed the neutralization of carrying out remaining acid in the alkaline solution; 4) in the alkali lye and after again water fully wash; 5) clean with dehydrated alcohol at last.
Claims (4)
1. an austenitic stainless steel metallographic etchant by the mixing solutions of hydrofluoric acid and nitric acid, measures by volume, and the ratio of each component is respectively: hydrofluoric acid: nitric acid: water=2: 1: 7.
2. the compound method at the described austenitic stainless steel metallographic etchant of claim 1 follows these steps to carry out: 1) measure 70 ml waters with glass measure, pour in the plastics liquid storage bottle; 2) measure 10 milliliters in analytical pure nitric acid with plastic measuring glass, pour in the described plastics liquid storage bottle, and shake up; 3) measure 20 milliliters of analytical pure hydrofluoric acid with plastic measuring glass again, pour mixing in the described plastics liquid storage bottle into.
3. the application of an austenitic stainless steel metallographic etchant, operate by following method: 1) clamp the qualified austenitic stainless steel metallographic specimen of polishing and put into austenitic stainless steel metallographic etchant with bamboo tweezers, make metallographic examination face immerse in the liquid fully, examination is towards last or side direction, and the variation of examination face look is observed in timing; When 2) treating that metallographic examination face is etched to darker silver gray, take out the austenitic stainless steel metallographic specimen, fully clean with the mobile tap water earlier at once with bamboo tweezers; 3) again the austenitic stainless steel metallographic specimen is immersed the neutralization of carrying out remaining acid in the alkaline solution; 4) in the alkali lye and after again water fully wash; 5) clean with dehydrated alcohol at last.
4. the application of austenitic stainless steel metallographic etchant according to claim 3 is characterized in that: described alkaline solution is Carbon Dioxide saturated aqueous solution of sodium or aqueous sodium hydroxide solution.
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CNA2008100424342A CN101353794A (en) | 2008-09-03 | 2008-09-03 | Austenitic stainless steel metallographic etchant, preparing method and use thereof |
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CN101603894B (en) * | 2009-07-16 | 2012-01-04 | 厦门大学 | Etching agent for titanium carbonitride coating on surface of hard alloy cutter and method for using same |
CN102383131A (en) * | 2011-11-03 | 2012-03-21 | 模德模具(东莞)有限公司 | Formula for corrosive medicinal liquid used for high hardness die steel and preparation method for same |
CN102443803A (en) * | 2012-02-23 | 2012-05-09 | 中国船舶重工集团公司第七二五研究所 | Metallographic corrosion method for martensitic precipitation hardening stainless steel crystal boundary |
CN102507292A (en) * | 2011-09-21 | 2012-06-20 | 内蒙古包钢钢联股份有限公司 | Method for displaying austenite grain boundary of low-carbon micro-alloy steel |
CN102517585A (en) * | 2011-12-16 | 2012-06-27 | 振石集团东方特钢股份有限公司 | Metallographic etchant and erosion method of austenitic stainless steel |
CN102928282A (en) * | 2012-11-02 | 2013-02-13 | 上海锅炉厂有限公司 | Method for solving problem of acid returning permeation of metal cracks subjected to corrosion of corrosives |
CN103234801A (en) * | 2013-04-25 | 2013-08-07 | 北京科技大学 | Method for displaying and treating Cr12 type martensitic heat-resistant steel primary austenite grain boundary |
CN103323309A (en) * | 2013-06-26 | 2013-09-25 | 广西师范大学 | Characterization method capable of acquiring high-definition metal titanium surface boride layer morphology |
CN103487309A (en) * | 2013-08-27 | 2014-01-01 | 中国船舶重工集团公司第七二五研究所 | Method for displaying grain size of metal material |
CN103805999A (en) * | 2014-03-06 | 2014-05-21 | 国家电网公司 | Type 18-8 chromium-nickel austenite stainless steel metallographic phase etching liquid for power station boiler and etching method |
CN103926132A (en) * | 2014-04-30 | 2014-07-16 | 厦门大学 | Hard alloy cutter surface coating etchant and application method thereof |
CN104233304A (en) * | 2014-09-22 | 2014-12-24 | 无锡贺邦金属制品有限公司 | Chemical polishing solution for stainless steel and preparation method thereof |
CN106124392A (en) * | 2016-07-29 | 2016-11-16 | 张家港清研检测技术有限公司 | The metallographic etchant of a kind of austenitic ferrochrome and caustic solution |
CN106350820A (en) * | 2016-08-30 | 2017-01-25 | 东方电气集团东方锅炉股份有限公司 | Etching agent for displaying shot-blasted layer of inner wall of austenitic heat-resistant steel pipe, and use method of etching agent |
CN108396321A (en) * | 2018-03-07 | 2018-08-14 | 济南大学 | A kind of metallographic etchant for austenitic stainless steel and its prepare caustic solution |
CN110672397A (en) * | 2019-09-16 | 2020-01-10 | 唐山钢铁集团有限责任公司 | Metallographic sample preparation and display method for aluminum-silicon coated steel plate |
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 |
CN113325020A (en) * | 2021-06-24 | 2021-08-31 | 北京科技大学 | Metallographic erosion method for observing duplex stainless steel welded joint under SEM |
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2008
- 2008-09-03 CN CNA2008100424342A patent/CN101353794A/en active Pending
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CN101603894B (en) * | 2009-07-16 | 2012-01-04 | 厦门大学 | Etching agent for titanium carbonitride coating on surface of hard alloy cutter and method for using same |
CN102507292A (en) * | 2011-09-21 | 2012-06-20 | 内蒙古包钢钢联股份有限公司 | Method for displaying austenite grain boundary of low-carbon micro-alloy steel |
CN102383131A (en) * | 2011-11-03 | 2012-03-21 | 模德模具(东莞)有限公司 | Formula for corrosive medicinal liquid used for high hardness die steel and preparation method for same |
CN102517585B (en) * | 2011-12-16 | 2013-08-07 | 振石集团东方特钢股份有限公司 | Metallographic etchant and erosion method of austenitic stainless steel |
CN102517585A (en) * | 2011-12-16 | 2012-06-27 | 振石集团东方特钢股份有限公司 | Metallographic etchant and erosion method of austenitic stainless steel |
CN102443803A (en) * | 2012-02-23 | 2012-05-09 | 中国船舶重工集团公司第七二五研究所 | Metallographic corrosion method for martensitic precipitation hardening stainless steel crystal boundary |
CN102928282A (en) * | 2012-11-02 | 2013-02-13 | 上海锅炉厂有限公司 | Method for solving problem of acid returning permeation of metal cracks subjected to corrosion of corrosives |
CN103234801A (en) * | 2013-04-25 | 2013-08-07 | 北京科技大学 | Method for displaying and treating Cr12 type martensitic heat-resistant steel primary austenite grain boundary |
CN103323309B (en) * | 2013-06-26 | 2015-08-19 | 广西师范大学 | A kind of characterizing method obtaining the metal titanium surface boride layer morphology of high-resolution |
CN103323309A (en) * | 2013-06-26 | 2013-09-25 | 广西师范大学 | Characterization method capable of acquiring high-definition metal titanium surface boride layer morphology |
CN103487309A (en) * | 2013-08-27 | 2014-01-01 | 中国船舶重工集团公司第七二五研究所 | Method for displaying grain size of metal material |
CN103805999A (en) * | 2014-03-06 | 2014-05-21 | 国家电网公司 | Type 18-8 chromium-nickel austenite stainless steel metallographic phase etching liquid for power station boiler and etching method |
CN103926132A (en) * | 2014-04-30 | 2014-07-16 | 厦门大学 | Hard alloy cutter surface coating etchant and application method thereof |
CN104233304A (en) * | 2014-09-22 | 2014-12-24 | 无锡贺邦金属制品有限公司 | Chemical polishing solution for stainless steel and preparation method thereof |
CN104233304B (en) * | 2014-09-22 | 2017-02-08 | 李璇捷 | Chemical polishing solution for stainless steel and preparation method thereof |
CN106124392A (en) * | 2016-07-29 | 2016-11-16 | 张家港清研检测技术有限公司 | The metallographic etchant of a kind of austenitic ferrochrome and caustic solution |
CN106350820A (en) * | 2016-08-30 | 2017-01-25 | 东方电气集团东方锅炉股份有限公司 | Etching agent for displaying shot-blasted layer of inner wall of austenitic heat-resistant steel pipe, and use method of etching agent |
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CN108396321A (en) * | 2018-03-07 | 2018-08-14 | 济南大学 | A kind of metallographic etchant for austenitic stainless steel and its prepare caustic solution |
CN108396321B (en) * | 2018-03-07 | 2020-01-21 | 济南大学 | Metallographic corrosive liquid for austenitic stainless steel and preparation corrosion method thereof |
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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 |
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CN113588363B (en) * | 2021-07-23 | 2023-10-31 | 唐山钢铁集团有限责任公司 | Metallographic sample preparation and display method for iron-aluminum-silicon layer of aluminum-silicon coated steel plate |
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